HANDBOOK OF PHARMACY EMBRACING THE THEORY AND PRACTICE OF PHARMACY AND THE ART OF DISPENSING. FOR STUDENTS OF PHARMACY AND MEDICINE, PRACTICAL PHARMACISTS, AND PHYSICIANS. BY VIRGIL COBLENTZ, Ph.G., A.M., Phil.D., PROFESSOR OF THEORY AND PRACTICE OF PHARMACY AND DIRECTOR OF THE PHARMACEUTICAL LABORATORY IN THE COLLEGE OF PHARMACY OF THE CITY OF NEW YORK. WITH THREE HUNDRED AND NINETY-FIVE ILLUSTRATIONS. PHILADELPHIA: P. BLAKISTON, SON & CO., IOI2 WALNUT STREET. 1894. Copybight, 1894, by P. Blakiston, Son & Co. Wm. F. Fell & Co., ELECTROTYPERS AND PRINTERS, 1220-1224 SANSOM STREET, PHILADELPHIA. PREFACE. In preparing this Handbook, the author’s aim was to supply to the student of pharmacy a compendious and yet sufficiently detailed text-book for systematic study, and to those exercising the art a trustworthy guide to be consulted in daily practice. In accordance with this general plan, particular care has been bestowed upon the explanation of all operations and methods usually occurring in dispensing establishments and laboratories designed on a small scale. To give anything like a full account of modern apparatus, appliances, and methods pursued in large manufacturing establishments would have enlarged the work unnecessarily, without practical benefit to the dispensing apothe- cary. The present work is divided into four parts, viz.: Physical and Mechanical Operations; Galenical Pharmacy; the Art of Dispensing; and Volumetric Analysis. Part I, which treats of the general principles, and physical or chemical operations in their general application, presents what may be called the theory of pharmacy. A thorough knowledge of the subjects embraced in this section is of vital importance to the apothecary, in order to enable him to control the quality of the medicinal substances which he purchases or dispenses. He who is unable to apply the proper tests or make the necessary determinations himself, is compelled to rely upon statements at second hand, and is thus handicapped not only in the manage- ment of his own business, but will be unable to secure the confi- dence of the public or of the medical profession, either of whom will, sooner or later, find out the shallowness of his knowledge. This portion of the work, and such of the succeeding portions as appeared to require it, have been profusely illustrated with drawings, diagrams, and cuts of apparatus and appliances, care- fully selected from the best sources, both domestic and foreign. Processes which have become antiquated have been either entirely omitted, or are only briefly described. Some processes, as for instance that of grinding and powdering drugs on a large scale, have practically ceased to come within the province of the dis- pensing pharmacist, and demand machinery which is beyond the requirements of the latter; it has, therefore, received only a very brief mention. But the processes of grinding and powdering drugs on a small scale, and the most suitable apparatus for this purpose, have been treated of in detail. Such subjects as the III IV PREFA CE. determination of melting and boiling points, evaporation, subli- mation, desiccation, solution and solubility, crystallization, decan- tation, filtration, etc., have also been discussed at length, particu- larly for the benefit of students and beginners. Especial care has been bestowed on the subjects of maceration, percolation and expression. Part II treats of the various classes of galenical preparations. Each class is described and explained as fully as its importance warrants, and in connection with each class are given descriptions and explanations of the processes of those preparations which require a commentary. Particular attention has been given to the explanation of the several steps of the processes involving chemical reactions by means of equations or diagrams, and the method of testing, as well as the application of volumetric methods of assay, are fully explained. Working processes are, as a rule, only given in the case of those preparations which require a com- mentary. For all others, the reader or student is referred to the U. S. Pharmacopoeia, which he is expected to consult, and which this work is not designed to replace. In connection with many of the more important preparations, examples or exercises are given which will assist in acquiring a thorough understanding of the reactions and calculations involved in the explained process. Whenever necessary, syllabi or tables of the various prepara- tions have been given under the several classes. Part III embraces the Art of Dispensing. In the section treating on Prescriptions, the aim of the author has been to make it as practical as possible. Foreign methods of prescrip- tion writing and dispensing have been treated of, wherever thought necessary, alongside of those prevailing in this country, and a chapter added on homoeopathic pharmacy, which is found to be a necessary occupation of the regular apothecary in some sections of the country. Much care has been devoted to the chapters on explosive or dangerous prescriptions, and on incom- patibilities. The series of characteristic prescriptions, to which explanatory comments are added, will also, it is hoped, be found generally useful. Owing to the prominence which the new Pharmacopoeia gives to the volumetric methods of assay, it has been thought not only useful, but quite necessary to present this subject somewhat more at length in Part IV, so as to make the student and general user of the book thoroughly familiar with it. It is an old experience of teachers that students approach this subject frequently with reluctance, as it appears to many of them at first difficult; but that they nearly all quickly master it, as soon as they under- stand the simple basis upon which the whole rests. The author desires to acknowledge his indebtedness for valu- able advice and assistance received from Charles Rice, Phil. D., PREFACE. V of New York City. Likewise, acknowledgments are due to Prof. J. U. Lloyd, of Cincinnati, Ohio; also, Mr. A. Zimmerman, Ph.G., and Mr. W. H. Madison, Ph. G., for assistance rendered. Many of the illustrations in this book were selected from vari- ous text-books and works of reference, which necessarily demand proper acknowledgment. It was found impracticable to mention the source in each separate instance, hence the author deemed it best and proper that a list of these be given in detail here, viz.:— Arbeitsmethoden fiir Organisch-Chemische Laboratorien; Lassar-Cohn. Leipzig: Leopold Voss. Arzneiverordnungslehre ; R. Kobert. Stuttgart: F. Enke. Atlas zu deu fliichtigen Oelen ; K. L. Vetters. Weimar : F. Voigt. Atlas zu den fetten Oelen ; G. Bornemann. Weimar : F. Voigt. Die Neueren Arzneimittel; B. Fischer. Berlin : J. Springer. Ganot’s Physics ; E. Atkinson. New York : Wm. Wood & Co. Kommentar zum Arzneibuch fiir das Deutsche Reich ; H. Hager, B. Fischer and C. Hartwich. Berlin : J. Springer. Commentar zur siebenten Ausgabe der oesterreichischen Pharmacopoe ; F. Schneider und A. Vogl. Wien : C. Gerald. Lehrbuchder Organischen Chemie ; V. Meyer und P. Jacobson. Leipzig : Veit & Co. Lehrbuch der Anorganischen Chemie; (Graham-Otto), A. Michaelis. Braunschweig : F. Vieweg und Sohn. Mohr’s Lehrbuch der Titrirmethode; A. Classen. Braunschweig : Vieweg. Manual of Analytical Chemistry ; J. Muter. Philadelphia : Blakiston & Co. Ostwald’s Outlines of General Chemistry ; J. Walker : Macmillan & Co. Proceedings of the American Pharmaceutical Association. Physikalisch-Chemische Methoden ; J. Traube. Leipzig : L. Voss. Pharmaceutisches Manual ; E. Dieterich. Berlin : J. Springer. Real Encyclopaedic der Pharmacie; E. Geissler, J. Miller. Leipzig: Urban & Co Redwood’s Pharmacy, Proctor. Treatise on Chemistry ; Roscoe and Schorlemmer. Macmillan & Co. : London. Schule der Pharmacie, I; E. Mylius. Berlin : J. Springer. Lehrbuch der Pharmaceutischen Chemie ; E. Schmidt. Braunschweig : Vieweg und Sohn. Technik der Experimental Chemie ; R. Arendt. Leipzig : Leopold Voss. The Art of Dispensing, Chemist and Druggist. London. Chemiker-Zeitung; G. Krause, Cothen. Pharmaceutische Centralhalle ; H. Hager und E. Geissler, Dresden. New York City, September, 1894. TABLE OF CONTENTS. INTRODUCTION. PAGE Terms and Definitions, 1 Pharmacopoeias, History of, 1 Pharmacopoeias, Table of, 2 Pharmacopoeia Nomenclature, 3 PART I. CHAPTER I. Weights and Measures, 7 Units of Length, Time, Mass, 7 Ancient Standards, 8 Modern Standards, 8 Tables of Various Systems of Weight and Measure 20 Balances, Various Systems, 21 Weights, 30 Measuring Vessels, 32 CHAPTER II. Specific Gravity ; Density, Standards, 34 Specific Gravity of Solids, 35 “ “ by Displacement in Graduated Cylinder, 36 “ of Insoluble Bodies Heavier than Water, 36 “ “ “ “ “ Lighter “ “ 37 “ “ “ Soluble Bodies, 38 “ “ “ Liquids, 38 “ “ “ “ by means of Pycnometer, 38 “ “ “ “ ‘‘ “ “ Hydrometer, 40 “ “ “ “ “ “ “ Specific Gravity, Balance, ... 45 “ “ “ “ “ “ “ Jolly’s Spiral Balance, 46 “ “ “ “ “ “ “ Sprengel Sp. Gr. Tube, 47 “ “ “ “ “ “ “ Given Weight of Di f. Volumes, . 48 “ “ “ “ “ “ “ Lovis’ Sp. Gr. Beads, 48 “ “ “ Fats, 49 Specific Volume, 49 Exercises in Specific Gravity and Specific Volume, 50 Tables of Specific Gravity, 51 CHAPTER III. Heat : Various Applications in Pharmacy, 52 Valuation of Heat, 52 Apparatus for Generation of Heat, 53 Measuring of Heat, 57 Testing Thermometers, 61 Boiling Point, 62 Melting Point, 63 Melting and Congealing Point of Fats and Waxes, 65 vii VIII TABLE OF CONTENTS. CHAPTER IV. page Heat : Operations Requiring a High Degree of Heat, 67 Blowpipe, 67 Crucibles, 68 Ignition, Fusion, Calcination, Deflagration, Torrefaction, Carbonization, . 69 CHAPTER V. Heat : Operations Requiring a Lower Degree of Heat, 71 Evaporation, 71 Evaporating Vessels, 72 Vacuum Apparatus, 76 Baths, 81 CHAPTER VI. Distillation, 85 Fractional Distillation, 95 Destructive Distillation, 97 Pharmaceutical Stills, 98 CHAPTER VII. Sublimation, 105 CHAPTER VIII. Desiccation, 108 Desiccators, Ill Drying Gases and Liquids, 113 CHAPTER IX. Comminution, 115 Drug Mills, 116 Pulverization, 119 Sifting, 120 Trituration (Mortars, Spatulas), 121 Levigation, 125 Elutriation, 126 Trochiscation, 127 CHAPTER X. Solution, 128 Solubility, Conditions Governing, 128 Solvents used in Pharmacy, 129 Solutions, Various Kinds, 130 Solution of Gases, 131 Density of Solutions, 133 Changes of Volume and Temperature by Solution, 133 Determination of Solubility, 134 Percentage Solutions, 137 Rules and Examples for Dilution and Fortification, 138 CHAPTER XL Diffusion—Dialysis, 141 CHAPTER XII. Crystallization, 143 Systems of Crystallography, 143 Methods of Crystallization, 147 Growing of Crystals, 149 Draining Crystals, Crystallizing Vessel, 150 Effect of Solvents on Crystallization, 151 IX CHAPTER XIII. page Granulation, 152 CHAPTER XIV. Exsiccation, 153 CHAPTER XV. Deliquescence and Efflorescence, 154 Deliquescent and Efflorescent Bodies, 154 Effects of the Exposure of Chemicals to Light and Air, 154 CHAPTER XVI. Precipitation, 156 Various Causes of Precipitation, 156 Objects of Precipitation, 157 Different Classes of Precipitates, 157 Fractional Precipitation, 159 CHAPTER XVII. Decantation, 161 Siphons, 162 Pipettes, • . . 164 Wash Flask, 165 Collection and Washing of Precipitates, 165 CHAPTER XVIII. COLATION, 168 CHAPTER XIX. Filtration, 170 Filter Paper, 170 Methods of Folding Filter Paper, 171 Maxims to be observed in Filtering, 174 Funnels, 176 Upward Filtration, 178 Special Filtering Apparatus, 178 Hot Filtration, 179 Rapid Filtration, 180 CHAPTER XX. Clarification, 184 By Application of Heat, 184 By Mechanical Appliances, 184 Use of Gelatin, 184 Use of Insoluble Bodies, 184 Use of Alcohol 185 CHAPTER XXI. Decoloration, 186 CHAPTER XXII. Separation of Immiscible Liquids, 187 CHAPTER XXIII. Extraction, 189 Maceration, 189 TABLE OF CONTENTS. X TABLE OF CONTENTS. CHAPTER XXIV. page Percolation, 191 History, 191 Theory, 192 Percolators, 193 Moistening and Packing, 197 Various Steps of Operation, 197 Various Forms of Percolating Apparatus, 199 Pressure Percolation, • 204 Vacuum “ • 206 Hot Percolation or Extraction, 207 CHAPTER XXV. Expression, 210 Screw Presses, 210 Hydraulic Press, 212 Centrifugal Machines for Laboratory Use, 213 PART II. GALENICAL PHARMACY.—SOLUTIONS. CHAPTER XXVI. Aqueous Solutions. Aqu.e Medicate, 217 Medicated Waters prepared by Direct Solution, 217 “ “ “ “ Intermediate Solution, 218 “ “ “ “ Distillation, 218 Explanatory Text, 221 Table of Official Medicated Waters, 225 Injectiones 226 Liquores, 227 Explanatory Text, 227 Table of Official Liquors, 243 Infusa, . • 244 Various Methods of Preparation, 245 Table of Official Infusions, . 246 Decocta 247 Table of Decoctions, 247 Mucilagines, 248 Table of Official Mucilages, 248 CHAPTER XXVII. Acetous Solutions. Aceta 249 Table of Official Vinegars 249 CHAPTER XXVIII. Alcoholic or Hydroalcoholic Solutions. Spiritus, 250 Spirits prepared by Direct Solution, 250 Spirits “ “ Chemical Reaction, 251 Spirits “ “ Distillation, 251 Explanatory Text, 251 Table of Official Spirits, 250 Vina Medicata, 256 Table of Official Wines, • 257 TABLE OF CONTENTS. XI PAGE Tincture, 258 Menstruum, 258 Strength, 258 Preparation, 259 Preservation, . 261 Tincture Herbarum Recentium, .... 261 Succi, 262 Explanatory Text—Assays of Tinctures, 262 Syllabus of Tinctures, 267 Extracta Fluida, 269 Menstruum, 269 Percolation, 270 Repercolation, 270 Percolation and Maceration with Expression, 272 Maceration and Percolation in Vacuo, 273 Preservation, 273 CHAPTER XXIX. Saccharine Solutions. Syrupi, 275 Various Methods of Preparation, 275 Clarification, 277 Preservation, 277 Explanatory Text, 278 Table of Official Syrups 283 Mellita and Oxymellita, 284 Elixiria 285 CHAPTER XXX. Glycerine Solutions. Glycerita 286 Table of Official Glycerites, 286 CHAPTER XXXI. Oleic Acid Solutions. Ole ata, 287 Preparation by Solution, 287 Preparation by Chemical Reaction, 288 Explanatory Text, 289 CHAPTER XXXII. Ethereal Solutions. OleoresiNz®, 290 Various Methods of Preparing, 290 Table of Official Oleoresins, 291 Collodia, 292 Table of Official Collodions, 292 MIXTURES. CHAPTER XXXIII. Linimenta, 293 Table of Official Liniments, 293 Mistura?, 294 Table of Official Mixtures, 294 XII TABLE OF CONTENTS. PAGE Emulsiones, 295 Theory of Emulsification, t 295 Continental, English and other Methods, 296 Various Emulsifying Agents, 297 Emulsification of Special Drugs, 300 Notes, 301 Table of Official Emulsions, 302 SOLIDS. I. FOR INTERNAL USE. CHAPTER XXXIV. PULVERES, 303 Preparation, 303 Dividing, 304 Cachets, 305 Gelatin Capsules, Hard and Elastic, 307 Filling Capsules, 307 Table of Official Powders, 310 Triturationes, 310 Oleosacchara, 311 Confectioner, 312 Massas, 312 Explanatory Text, 313 Trochisci, 314 Various Forms, Pastilles, Ovoids, Bacilli, 316 Table of Official Troches, 317 Pilulas, 318 Massing, 318 Excipients, Liquid, 322 Excipients, Solid, 323 Classification of Various Substances to be Massed, 324 Coating, Varnishing, Silvering, Sugar, Gelatin, Keratin and Salol, . . . 326 Tablettas, 331 Tablet Triturates, 331 Compressed Tablets, 335 Extracta, • 341 Methods of Preparation, 341 Physical Character and Preservation, 343 Table of Official Extracts 343 Explanatory Text, Assays, 344 Abstracta 349 Resinas, 350 Table of Official Resins, 350 Resinoids (Eclectic) 350 II. FOR EXTERNAL USE. CHAPTER XXXV. Unguenta, 352 Bases, 352 Made by Fusion, 352 “ “ Mechanical Admixture, 352 “ “ Chemical Reaction, 354 Preservation and Dispensing, 354 Table of Official Ointments, 354 Explanatory Text, . , 355 Cerata, 357 Table of Official Cerates, 357 TABLE OF CONTENTS. XIII PAGE Emplastra, 358 Plasters Proper, 358 Resinous Plasters, 358 Spreading and Perforation, 358 Explanatory Text, 361 Table of Official Plasters, 361 Charts, 362 Suppositoria, 363 Bases, 363 Hand Rolled, 365 Moulded, 365 Compressed, 368 Various Moulds 370 Suppository Capsules and Hollow Cacao-Butter Suppositories, 371 General Remarks, 372 PART III. CHAPTER XXXVI. The Art of Dispensing. The Prescription, 375 Parts of the Prescription, Analysis, 375 Grammatical Construction, 376 Doses, 379 Abbreviations, 379 Abbreviation of Latin Terms and Phrases, 380 Foreign Prescriptions 383 Cabalistic Signs and Abbreviations, 384 Metric Prescriptions, 385 Table of Terms occurring in French and German Prescriptions, .... 385 Homoeopathic Dispensing, • 388 “ Prescriptions, ... • 388 Table of Solubilities, 390 Explosive Mixtures, 390 Incompatibles ; Pharmaceutical, Therapeutical and Chemical, 394 Examples of Incompatibles, classified, 394 Typical Prescriptions explained, 399 PART IV. CHAPTER XXXVII. Volumetric Analysis, 413 Definitions, 413 Various Standard Solutions, 413 Indicators, 414 Apparatus Employed, 415 Measuring Flasks and Cylinders, .415 Pipettes, 415 Burettes, 415 Preparation of Standard Solutions, with Exercises, 419 Alkalimetry, Exercises in estimation of various alkalies, 422 Acidimetry, “ “ “ “ “ acids, 427 Standard Solution of Silver Nitrate. —Estimations of Halogens.—Volhard’s Method.—Estimation of HCN, KCN, etc., . . 429 Standard Solution of Iodine.—Estimation of Arsenous Oxide, Sulphurous Acid and Sulphites.—Hyposulphites, etc., . . 432 Standard Solution of Sodium Hyposulphite.—Estimation of Iodine, Chlor ine, Bromine, Iron in Ferric Salts, 434 XIV TABLE OF CONTENTS. PAGE Standard Solution of Potassium Dichromate.—Estimation of Metallic Iron and various Ferrous Salts, 436 Standard Solution of Potassium Permanganate.—Estimation of Hydrogen Dioxide, Barium Dioxide, Iron, Ferrous Salts, Hypophosphorous Acid and Hypophosphites, 439 Standard Solution of Bromine.—Estimation of Phenol, 443 APPENDIX. Table of Atomic Weights, 447 Table of Solubilities, 448 List of Pharmacopceial Chemicals and Reagents, 455 Table of Thermometric Equivalents, 461 Table of Equivalents of Weights and Measures, 466 Table of Equivalents of Measures of Length, 472 LIST OF ILLUSTRATIONS. FIG. PAGE 1. The Pound Weight—Ancient and Modern Standards, 9 2. Position of Stopper for Dropping, 13 3-5. Vials for producing Drops, • • 14 6. Metric Diagram, 18 7. Balance, 21 8. Beam with Movable Fulcrum, 22 9. Analytical Balance, 23 10. Prescription Balance, 23 11. Hand Scales, .... 24 12. Proper way of Holding Hand Scales, 24 13. Army Prescription Scales, 25 14. Counter-Balance, 25 15. Counter-Balance (Laboratory), 26 16. Counter-Balance (Dispensing), 26 17. Gorham Dispensing Balance, 26 18. Fairbank’s Druggists’ Scale, 27 19. Balance for Weighing Solutions, 27 20. Physician’s Vest-pocket Scale, 27 21. Counter Scale, 28 22. Box Prescription Scale, 28 23. Torsion Counter Scale, 29 24. Torsion Counter Scale, 29 25. Torsion Prescription Scale, 29 26. Triple Graduated Beam, 29 27. Avoirdupois Iron Weights, 30 28. Metric Iron Weights, 30 29. Cup Weights (Troy), 30 30. Block Weights, 30 31. Prescription Weights (Metric), 30 32. Analytical Weights, 30 33. Aluminum Wire Weights, 31 34. Aluminum Grain Weights, . 31 35. Apothecaries’ Coin Weights, 31 36. Apothecaries’ Brass-foil Weights, 31 37. Brass Metric Weights, *. . . 31 38. Aluminum Wire and Foil Weights (Metric), 31 39. Porcelain Measuring Cup, 32 40-2. Graduates, 32 43-5. Cubic-Centimeter and Minim Measures, 33 46. Hydrostatic Balance, 35 47. Immersion of Solid (Specific Gravity), 35 48. Pycnometer, 38 49. Pycnometer with Thermometer, 39 50. Squibb’s Pycnometer, 40 51. Weighing Hydrometer, 41 52. Scale Hydrometer, 41 53. Nicholson’s Hydrometer, 41 54. Rousseau’s Densimeter, 42 55. Baume’s Hydrometer (Heavy Liquids), 43 56. Baume’s Hydrometer (Light Liquids), 43 57. Squibb’s Urinometer with Cylinder, 44 58. Westphal Specific Gravity Balance, . . 45 59. Beam of Westphal Balance, showing Position of Weights, 46 XV XVI LIST OF ILLUSTRATIONS. FIG. PAGE 60. Mohr’s Specific Gravity Balance, 47 61. Jolly’s Spiral Balance, 47 62. Sprengel Specific Gravity Tube, 48 63. Specific Gravity of Solid Fats (Westphal Balance), 48 64. Specific Gravity of Solid Fats (Areometer), 48 65. Alcohol Lamp, 52 66. Berzelius’ Alcohol Lamp, 52 67. Barthel Spirit Lamp, 53 68. Bunsen Burner, 54 69. Bunsen Burner, in Sections 54 70. Bunsen Flames, 55 71. Bunsen Burner (Seven-tubed), 55 72. Erlenmeyer’s Burner, 55 73. Fletcher’s Solid Flame Heating Burner, 56 74. Fletcher’s Gas Stove 56 75. Gas Stove, 56 76. Instantaneous Water Heater, 56 77-8. Blast Lamp with Cross Section, 57 79. Thermometer (Milk-glass Scale), 58 80. Thermometer (Graduated on Tube), 58 81. Fahrenheit, Centigrade, Reaumur Thermometers, 58 82. Boiling-point Determination, 61 83. Fractionating Flask (Measurements) 62 84. Apparatus for Fractional Distillation, 63 85. Drawing Out Tubing, 64 86. Capillary Tubes for Melting Point Determinations, 64 87. Melting Point Tubes in Position, 65 88. Taking Melting Point in Bath of Sulphuric Acid, . 65 89. Long-neck Flask for Melting Point Determinations, 66 90. Air Bath for Melting Point Determinations, 66 91. Tubes for Fusing Point Determination, 66 92. Sectional View of Bunsen Flame, 67 93. Blowpipe, 67 94. Blowpipe Flame, 68 95. Crucibles, Hessian, Graphite, Platinum, Porcelain, Clay, Copper, ... 68 96. Ignition with Blast Lamp, 69 97. Mechanical Stirring Apparatus for Evaporating Fluids 72 98. Mechanical Stirring Apparatus, 72 99. Cascade Evaporator (Siebert), 73 100-1. Evaporation, 74 102. Evaporating and Crystallizing Dishes, 75 103. Evaporating over Direct Flame, 76 104. Evaporating with Properly Regulated Flame, 76 105. Evaporating with Flame Unnecessarily High, 76 106. Pharmaceutical Vacuum Apparatus, 77 107. Vacuum Apparatus (Sectional View), 78 108. Hempel’s Evaporator, 79 109. Bath for Evaporating Inflammable Liquids, 79 110-11. Draught Chambers, 80 112. Copper Water-Bath, 81 113. Iron Water-Bath, 81 114. Iron Water Bath with Constant Level, 81 115. Water-Bath with Constant Level (Kekule), 81 116. Water-Bath with Constant Level, 81 117. Water-Bath (Landolt), 82 118. Steam Evaporating Kettle, 82 119. Iron Sand-Baths, 82 120. Filling Sand-Bath, 82 121. Tripods, 83 122. Fleck’s Air-Bath, 84 123. Simplest Form of Distillation, 85 124. Distillation (Improvised Condenser), ... 85 125. Distillation, 86 126. Fractionating Flask with Thermometer, 86 LIST OF ILLUSTRATIONS. XVII FIG. PAGE 127. Flask with T-Tube for Fractionating, 86 128. Glass Retorts, 87 129. Filling Retort, 87 130. Earthenware Retorts, 87 131. Lead Retort, 87 132. Liebig Condenser (Improvised), 88 133-5. Liebig Condensers (Various Forms), 88 136. Distilling Apparatus with Worm Condenser, 89 137. Distilling with Air Condenser, 89 138. Pinch-cocks, 90 139. Adj ustable Pinch-cocks, 90 140. Retort Stand, 91 141. Receivers, 91 142. Adapters (Various Forms), 91 143. Retorts with Adapters, . . . . • 92 144. Position for Breaking a Tube, 92 145. Bending Tubing, 92 146. Properly and Poorly Bent Tubing, 92 147. Mohr’s Cork Borer, 93 148. Cork File, 93 149. Lever Cork Press, . . 94 150. Rotary Cork Press, 94 151. Flask with Upright or Reflux Condenser, 94 152. Soxhlet’s Spherical Condenser, 94 153. Apparatus for Distillation in Current of Steam, 95 154. French Column Apparatus, 96 155. Retorts for Destructive Distillation, 97 156. Laboratory Copper Still, 98 157. Curtman Still (Sectional View), 98 158. Beck’s Pharmaceutical Still, 99 159. Edel’s-Hood Still, 100 160. Prentiss Still, 100 161. Remington Still (Sectional View), 100 162. Automatic Water Still, 101 163. Curran Water Still, 101 164. Mitscherlich Condenser, 102 165. Rice’s Pharmaceutical Still, 103 166. Experimental Sublimation of Sulphur, 105 167. Oddo’s Sublimation Apparatus, 105 168. Bruehl’s Sublimation Apparatus, 106 169. Sublimation of Benzoic Acid (Small Scale), 106 170. Sublimation of Benzoic Acid (Hager’s Apparatus), 106 171. Apparatus for the Preparation of Calomel, 107 172. Drying Closet (Sectional View), 109 173. Copper Drying Oven, 110 174. Copper Drying Oven (Double Wall), Ill 175. Iron Drying Oven, Ill 176. Watch-glasses for Weighing Powders, Ill 177. Bell-glass Desiccator, Ill 178. Hempel’s Desiccator, 112 179. Vacuum Desiccator, 112 180. Gas Wash Bottles, 113 181. Drying Tube (Chloride of Calcium), 113 182. Drying Jar (Chloride of Calcium), 113 183. Poulain’s Pulverizing Works, 115 184. Enterprise Drug-Mill, 117 185. Hance Drug-Mill (Cross Section), 117 186. Hance Drug-Mill (Showing Parts), . 118 187. Pulverization of Corrosive or Poisonous Substances, 119 188. Hunter’s Sifter and Mixer, 12o 189. Trituration, 121 190. Motion Described by Pestle in Trituration, 121 191. Iron Mortars, 122 192. Wedgwood Mortar, 123 XVIII LIST OF ILLUSTRATIONS. FIG. PAGE 193. Porcelain Mortar (Shallow), 123 194. Porcelain Mortar (Deep), 123 195. Glass Mortar, .... 123 196. Agate Mortar, 123 197. Ointment Spatula, 124 198. Pill Spatula, 124 199. Horn Spatulas, 124 200. Powder Spatula, 124 201. Porphyry Slab and Muller, 125 202. Levigating Mortar, 125 203. Elutriation 126 204. Mould for Levigated Chalk, 127 205. Table of Curves of Solubility for Nitrates, .... 130 206. Apparatus for Generation, Washing, and Solution of Gases, 131 207. Preparation of Chlorine Water, 132 208. Weighing Bottle, 134 209. The Lysimeter, 136 210-11. Dialysers, 142 212-17. Crystals, Regular or Isometric System, 144 218-25. “ Tetragonal and Hexagonal Systems, 145 226-29. “ Rhombic or Ortho rhombic System 145 230-32. “ Monoclinic System, 146 233-34. ‘ ‘ Triclinic System, 146 235-36. Growing Crystals, 149 237. Draining Crystals, 150 238. Crystallizing Vessel, 150 239. Beaker Glasses, 159 240. Precipitating Jar, 159 241. Decantation with Guiding rod, 161 242. Careless Decantation, 162 243. Decanting over Greased Rim, 162 244-5. Decanting with Siphon, 163 246. Siphon Apparatus, 163 247. Siphons with Suction Tubes, 163 248. Rinsing out Precipitates, . . 164 249. Pipettes, 164 250. Suction Arrangement for Pipettes, 165 251. Wash or Spritz Flask, 165 252. 3, 4. Automatic Filtering and Washing Apparatus, 166 255. Automatic Filtration of Volatile Liquids 167 256. Straining Bag 168 257. Strainer Frame, 168 258-9. Forcible Straining, 169 260-3 Folding Filters, .... 172 264. Folding Filter, 172 265-71. Folding Filters, 173 272. Plaited Filter 174 273-4. Decanting Fluids on Filter, 175 275-6 Filtering Stands . . 175 277. Filtering into Bottle, . .’ 176 278. Chemist’s Cover, 176 279. Properly Shaped Funnel, 176 280. Proper and Faulty Shaped Funnels, 177 281. Ribbed or Fluted Funnel, 177 282. Filter for “ Upward Filtration,” 178 283. Apparatus for “ Upward ” Filtration of Oils, 179 284. Perforated Filtering Cone, 179 285. Jacketed Funnel, 180 286. Dieterich’s Jacketed Funnel, 180 287. Liebreich’s Steam Coil Jacket for Hot Filtration, 180 288. Water Pump, .181 289. Rapid Filtration, 181 290. Suction Flask for Rapid Filtration, 182 291. Funnel with Perforated Disc, 182 LIST OF ILLUSTRATIONS. XIX FIG. PAGE 292. Perforated Porcelain Disc (Kaehler and Martini’s), 182 293. Rapid Filtration (Improvised Apparatus), 183 294. Separating Funnel (Stoppered), 187 295. Separating Funnel (Currier), 187 296. Separating Flask (Pear shape), 187 297. Separation of Fluids by Capillary Pipette, 188 298-9. Separation of Immiscible Fluids by Siphon, 188 300. Real’s Press (Percolator), 191 301. Cylindrical Glass Percolator, 193 302. Conical, “ “ 193 303. Metal Percolator, 193 304. Apparatus for Percolation, 196 305. Graduated Receiving Jar, 196 306. Christ-Dieterich Percolator, 200 307. Percolator (Warmbrunn-Quilitz), 200 308. Siphon Percolator (Squibb’s), . . . 201 309. “ “ ( “ ' ) 203 310-11. Lentz’s Pressure Percolator, 205 312. Percolator with Air Pump, 206 313. Lewin’s Extraction Apparatus, 207 314. Currier’s Extraction Apparatus, 208 315. Tincture Press, • 211 316. Differential-Arm Screw-Press, 211 317. Witt’s Pharmaceutical Press, 211 318. Enterprise Screw Press, 212 319. Knee Lever Press, 212 320. Hydraulic Press, 213 321-22. Centrifugal Machines, 214 323. Laboratory Centrifugal Machine, 214 324. Apparatus for the Distillation of Volatile Oils, 219 325. Squire’s Infusion Mug, • . . . . 245 326. Infusion Mug, with Bath, 245 327. Alien’s Nitrometer (Curtmann), 253 328. Percolation with Volatile Solvent, 290 329. Soxhlet’s Extraction Apparatus, 291 330. Seidlitz Powder Measure, 304 331. Diamond Powder Divider, 304 332-34. Powder Folders, 305 335. Apparatus for Sealing Cachets (Chapereau), 306 336. Apparatus for Sealing Cachets (The Konseal), 306 337. Capsule Moulds, 307 338. Globular and Ovoid Capsules, 308 339. Elastic Gelatin Capsules, . . 308 340. Hard Gelatin Capsules, 308 341. Davenport Capsule Filler, 308 342. Raymond Capsule Filler, 309 343. Acme Capsule Filler, 309 344. Troches (Various Forms), 314 345. Rolling Out Mass for Troches, 315 346. Troche Cutting Machine, 316 347. Ovoids, 316 348. Mouth Pastilles, 316 349. Pill Mortar, 320 350. Pill Tile, 320 351. Pill Pestle, 320 352. Pill Roller (Sectional View), 320 353. Pill Spatula, 320 354. Pill Machine, 321 355. Pill or Plaster Press, 321 356. Pill Finisher, 322 357. Pill Finisher (Adjustable), 322 358. Pill Silverer, . . 327 359. Gelatin Pill Coating Machine (Maynard), 329 360. Gelatin Pill Coating Machine (Patch), 329 XX LIST OF ILLUSTRATIONS. FIG. PAGE 361. Tablet Triturate Mould, 331 362. Compressed Tablet Mould, 339 363. Compressed Tablet Machine, 339 364. Ointment Spatula, 353 365. Plaster Spatula, 358 366. Forms for Spreading Cerates or Plasters, 359 367-68. Plaster Block and Iron, 359 369. Plaster Perforating Machine (Lentz), . 360 370. Suppositories (Rectal), 363 371. Wellcome’s Improved-shaped Suppository, 363 372 Wellcome’s Improved-shaped Bougie, 363 373. Suppository Moulds, 367 374. See’s Suppository Mould, 367 375. Blackmann’s Suppository Mould, 367 376-77. The Perfection Suppository Machine, 369 378. Suppository Machine (W., T. & Co.), 369 379. Bougie Press, 370 380. Gelatin Suppository Capsules, ... 371 381-82. Hollow Cacoa-Butter Suppositories, 372 383. Cabalistic Prescription Signs, 384 384. Measuring Flasks, 415 385. Measuring Cylinder, 415 386. Burette operated with Pinch-cock, . 416 387. Device for Dropping from Burettes, . . . 416 388. Burettes with Glass Stop cocks, 416 389. Meniscus, . . 417 390. Reading of Meniscus, 417 391. Burette with Enameled Sides, 418 392. Effects produced by Meniscus, 418 393. Erdmann Float, 418 394. Burette Stand, 419 395. Burette in Position, 419 HANDBOOK OF PHARMACY. INTRODUCTORY. The term “ Apotheke” was applied in olden times to a place of storage for wines, books, etc. From this is derived “apothecary” (Lat. apothecarius). Since the Middle Age, it is restricted to those localities where medicinal substances are kept and dispensed. The term Pharmacy, is derived from the Greek pharmakon meaning medicine. It is the art which treats of the identification, preparation, testing, and dispensing of medicinal substances. A Pharmacopoeia (from tpappaxov, medicine, and ««&, to make) is a code for the use of the apothecary and physician, which em- braces the definitions, descriptions, physical and chemical proper- ties, tests and methods of preparation of medicinal agents. The earliest work,* which may be compared to our modern pharmacopoeias, and of which we have any definite knowledge, is an Egyptian treatise, preserved to us in the Papyrus Ebers, dating back to 1552 B. C. This contains a large number of formu- las, some of them quite complex, the ingredients being ordered by certain weights and measures. Nothing else has been pre- served to us, in the nature of such a work, within historic times, until we descend to the age of Hippocrates (about 460 to 377 B. C.), who, with his disciples founded a school of medicine, gradually rendering the employment of formularies, to secure uniformity in the preparation of medicines, necessary. Real formularies, how- ever, were not composed until much later, about the time of Andro- machus, Nero’s court physician (about 60 A. D.). After Galen’s time, their number gradually increased, but it was not until about the thirteenth century that more elaborate works (usually called “Antidotaria”) made their appearance. The Arabian physicians and their translators during the middle age considerably enriched the literature in this direction. The first work which really de- serves the name of a pharmacopoeia was composed by Valerius Cordus, and was published, after his death, by the city of Nurem- berg, in 1546. It was customary in those times to apply the name of “Dispensatorium” to formularies of this kind, and up to com- paratively recent times, the term Dispensatory has been used, in *A very exhaustive article on the subject of Pharmacopoeias and History of Pharmacy, by Dr. Chas. Rice, will be found in “A Reference Handbook of the Medical Sciences,” Vol. V and Supple- ment Vol.—Wm. Wood & Co., N. Y. 1 2 HANDBOOK OF PHARMACY. various countries, in the sense of our “pharmacopoeia,” while we now usually apply it to unofficial commentaries on the latter. The first United States Pharmacopoeia (in English and Latin) was published in Boston in 1820; this has been followed since by a new edition every ten years, prepared by a Committee of Revision appointed or elected by a convention of medical and pharmaceu- tical colleges and societies. Nearly all foreign pharmacopoeias are issued by the authority of their respective governments; the United States Pharmacopoeia is not thus issued, but at the same time it is recognized by our government. There are a number of smaller countries which have no national pharmacopoeia, but recognize those of other countries; among these, the South American States and West Indies, recognize gen- erally the Spanish with, in some instances, the French Pharmaco- poeia. In China, the foreign apothecaries employ their various national pharmacopoeias; while the natives usually follow a volu- minous work, entitled Pun-tsao, dating back to about 1560 B. C. Any work which takes up the various official (pharmacopoeial) and non-official remedies, and treats upon them exhaustively, in all their applications and uses in Medicine and Pharmacy, is called a “ Dispensatory.” TABLE OF THE MOST IMPORTANT PHARMACOPCEIAS. Country. Title of Pharmacopceia. Language. Number of Remedies. Entered into Force. Austria, .... Pharmacopcea austriaca. Edi- tio septima. Latin. (578) 1890 Belgium, .... Pharmacopcea Belgiea. Editio secunda. Latin and French. 1140 1885 Chili, Farmacopea Chilena. Spanish. — 1886 Denmark, . . . Pharmacopcea Danica. Editio tertia Danish. 584 1893 England, .... British Pharmacopceia. English. 898 1885 (Supplement 1889) Finnland, . . . Pharmacopcea Fennica. Editio quarta. Latin. 400 (about) 1885 France, .... Codex medicamentarius; Phar- macopee fran<;aise. French. 2039 (about) 1884 Germany, . . . Arzneibuch fur das Deutsche Reich ; dritte Ausgabe. German. 603 1891 Greece, ‘EAAtjvlkt) 4>ap/xaKO7rotca. Latin and Greek. 976 1868 Hungary, . . . Magyar Gyogyszerkonvy. MA- sodik kiadAs. Latin and Hungarian. 576 1888 Japan, Pharmacopcea Japonica. Edi- tio altera. Latin. 448 1891 Italy, Farmacopea ufficiale del regno d’Italia. Italian. 597 1892 Mexico, .... Nueva Farmacopea Mexicana. Spanish. — 1884 (Supplement 1890) Netherlands, . . Pharmacopcea Neer]andica. Editio tertia. Latin and Dutch. 533 1890 Norway Pharmacopcea Norvegica. Edi- tio tertia. Norwegian. — 1898(f) Portugal, .... Pharmacopea Portugueza. Portuguese. 1600 (about) 538 1876 Roumania, . . . Pharmacopcea Romana. Roumanian. 1874 Russia, Rossiiskaja Pharmakopeya. Russian. 808 1891 Sweden, .... Pharmacopcea Suecica. Editio octava. Swedish. — 1893 Switzerland, . . Pharmacopcea Helvetica III. German- French-Italian. 1038 1894 Spain, United States of Farmacopcea oficial Espanola. Sexta edicion. Spanish. 1598 1884 America, . . . Pharmacopoeia of the United States of America. Seventh decennial revision. English. 994 1893 3 INTRODUCTORY. In earlier times, the different pharmacopoeias or treatises ap- peared entirely in the Latin language; of late years, however, the text of these works has usually been written in the native language of the country in which it is issued, the Latin being retained in the various titles. Latin has been retained, chiefly because, being a dead language, it is not subject to the various changes and modifications of the different modern tongues. Even with the employment of Latin, various pharmacopoeias differ slightly in their nomenclature; thus in the case of the chemicals, one will place the electro-positive, another the electro-negative element first; for instance, sulphate of iron is variously named Ferrum sulphuricum, Ferri sulphas, Sulphas ferri and Sulphas ferrosus. Some pharmacopoeias employ the term kalium for potassium and natrium for sodium. In the Dutch, Danish, and Swedish pharmacopoeias, the titles of the chemical salts are expressed by treating the base as an adjective placed after the general name of the salt, corresponding, for example, to the English “Sodic Sulphate.” For Potassii acetas or Kalium aceticum they have Acetas kalicus; for Sodii bro- midura or Natrium bromatum they have Brometum natricum; for Bismuthi subnitras or Bismuthum subnitricum they have Subnitras bismuthicus. The various parts of the text of each article in the U. S. Phar- macopoeia are arranged in the following order:— 1. The official Latin title. 2. The English title. 3. In the case of chemicals, the symbolic formula and mole- cular weight. 4. In certain cases, one or more synonyms. 5. Definition, wherever necessary. 6. Mode of keeping, where necessary. 7. Description, physical, chemical, or botanical, followed, where necessary, by tests of identity, purity, and strength. 8. Preparations which may be considered as forms of adminis- tration of the drug. 1st. The Official Latin Title.—This is expressed in Latin, and is intended to express concisely the nature of the chemical, drug, or plant-part recognized. The U. S. P. ignores all remedies not included in itself, hence only that part of a drug or plant is used which it recognizes. Thus, under the title Aconitum, the Pharmacopoeia refers only to the tuber, and to no other part of the Aconitum napellus. When two different parts of a plant are recognized, then the Latin name of the particular part is added to the title; thus, “Belladonna Folia” for belladonna leaves, and “Belladonna Radix” for the root. For the galenical prepara- tions, such titles are selected as will most nearly indicate the nature or the composition of the preparation, attention being given also to simplicity and brevity of expression. Thus, “ Pulvis Ipecacuanhas et Opii ” indicates at once the composition of the 4 HANDBOOK OF PHARMACY. powder; but where several constituents enter into the composi- tion of a preparation, the title includes only the main constituent, the remainder being indicated by the term compositus. The various pharmacopoeial titles conform to the rules of Latin grammar.* Thus, we write: Solution of Potassa, Liquor (nominative) Potassa) (genitive); Cyanide of Mercury, Hydrar- gyri (gen.) Cyanidum (nom.); Pills of Phosphorus, Pilulae (nom. plural) Phosphori (gen.). Where there are two different oxides, iodides, or salts of the same base, a distinguishing adjective is usually appended in order to discriminate between the two; thus, we distinguish the two chlorides of mercury by the adjec- tives “ corrosivum ” and “ mite,” respectively. When an adjective is employed, it must agree in gender with the principal noun; thus, the masculine form “compositus” (compound) becomes “composita” with feminines, and “com- positum ” with neuters. We write Pulvis Cretse Compositus (masc.), Tinctura Benzoini Composita (fem.), and Decoctum Sar- saparillae Compositum (neut.). 2d. The English Title.—That is, the English name which the Pharmacopoeia selects or coins to designate the article. Very generally, this is identical with the vernacular name of the article, or that by which it is known in the market. In some cases the Pharmacopoeia coins a new name, for valid reasons. In the case of vegetable drugs, the genus name of the plant is often selected as the official English title, so that in many cases the official Latin title and the English title are identical. 3d. The Symbolic Formula and Molecular Weight.—In writing the symbolic formulas of acids, the replaceable hydrogen atoms are written before the other elements (thus, HC1, H2SO4, H3PO4, HC2H3O2, etc.). A period is used in the case of some com- pounds, where it is desired to show the existence of several inti- mately connected radicals or constituents (thus, in Ammonium Carbonate, NH4HCO3.NH4NH2CO2). Water of crystallization is separated from the formula of its salt by a + sign. 4th. The Synonym, that is, the name by which the article is popularly known.—Synonyms are only added where special rea- sons exist ; for instance, where the English title introduced by the Pharmacopoeia is not usually employed in commerce, or where a change has been made either in the Latin or English title, and attention is to be drawn to this. For example, under the title “ Hydrargyri Oxidum Rubrum ” we have the synonyms “ Red Mercuric Oxide ” and “ Red Precipitate ; ” this latter name arises from its old title, “ Mercurius Precipitatus Ruber.” Salts of hydrochloric acid have formerly been called muriates, the term being derived from muria (salt water). The term Cremor (creme) was applied during the Middle Age to substances which separated on the surface of a fluid ; later, * A good work of reference is Robinson’s “Latin Grammar of Pharmacy and Medicine.” INTRODUCTORY. 5 this term was applied to all precipitates; hence this title was given to the acid potassium tartrate (argols) which precipitates on the sides of wine casks, being called Cremor tartari, hence the source of the synonym, Cream of Tartar. These synonyms are some- times misleading and inaccurate; for instance, sugar of lead for Plumbi acetas, or white vitriol for Zinci sulphas, or blue vitriol for Cupri sulphas. 5th. The Pharmacopoeial Definition.—This is not necessary in all cases, but, where applied, it embraces in a few words a de- scription of the chemical or botanical nature and source of the substance. Thus, the U. S. P. defines Coca as “ the leaves of Erythroxylon Coca Lamarck (nat. ord. Linese),” and Gallic Acid as “an organic acid, usually prepared from tannic acid.” 6th. Modes.of Keeping.—In those instances where the prepara- tion or drug is sensitive to the influence of air, light, heat, etc., the Pharmacopoeia specifies that certain precautions should be taken in regard to its proper preservation. 7th. The Description.—This is intended to be a concise state- ment of the characteristic physical properties of the drug, followed wherever necessary, and particularly so in the case of chemicals, by tests of identity and purity. PART I. CHAPTER I. WEIGHTS AND MEASURES* A perfect system of Metrology should bear a simple relation to some constant and indestructible object, the length or size of which is known or can be readily determined with accuracy. Any three units (of which no one is derivable from the other two) may be selected as fundamental units. In the systems in present use the units of Length, Mass, and Time have been set aside as fundamental units, and the various systems of absolute units differ only as to the particular unit selected for measurement of Length, Mass, and Time. Mass and Weight are not identical. Mass is constant; it is the quantity of matter. Weight is the force with which the mass is drawn toward the center of the earth. The weight of Mass varies. When a body (Mass) is attached to a spiral balance (Jolly’s) and weighed at the sea- level, then on a mountain-top, it will be found to have decreased, and at the equator it will weigh less than at the poles. At the equator of the sun a pound would -weigh 27.62 lbs., owing to the difference in the force of gravity. When we say a body weighs 10 pounds, we mean that the body is drawn toward the earth with ten times the force with which the standard pound is drawn toward the earth. The Unit of Time is the Second. This is stthrto °f mean solar day. The Unit of Length, recognized as the standard in England and North America, is the English Yard of 36 inches. The yard and inch were formerly based upon a standard yard-stick in the custody of the British Board of Trade. Later on, it was found that a pendulum swinging seconds of time in vacuo at the level of the mid-tide in the latitude of London, measured 39.13929 inches, such as are derived from the standard yard. Should the latter become lost or destroyed, therefore, a new standard yard identical with the present one may readily be constructed. The Unit of Length, or absolute standard, is the Meter, a ten-millionth part of the earth’s quadrant (from pole to equator). As this unit was based on calculation, a practical standard was * A good work of reference is Oldberg’s “ Manual of Weights and Measures.” 7 8 HANDBOOK OF PHARMACY. constructed by marking the above-mentioned distance on a bar made of an alloy of Platinum and Iridium (chosen because of its great hardness and durability) preserved in the French Archives. Copies of this were furnished to all nations who bore a share of the expense, among others, to this country. The meter is the compulsory standard of measure in all civilized countries except the United States and Great Britain; it is the recognized standard for all scientific observations. The Unit of Weight.—The British standard Pound is a cer- tain mass of platinum in the London Standards Office. If one cubic inch of distilled water, in vacuo, weighs 252.892 grains, then the standard pound contains 5760 of these grains. The unit of weight is the Kilogramme, a mass of platinum kept in the French Archives, copies of which were also furnished to certain other countries, among them the U. S. A. This is the weight of Ttyjjo Part °f a cuhic meter, or the weight of one cubic decimeter of distilled water at its greatest density (4° C.). Weight * has always been determined from Measure. From the remotest of times, we find various physical standards of weight and measure. The ancient Egyptians employed the Cubit and Foot, for which the human body furnished the basis. The Greek Talent was obtained from a cubic foot of water, and the Mina, or the part of this, is nearly identical with the modern Pound. Two distinct pounds have always been in use, one for monetary, and one for commercial purposes. The oldest known set of standard weights was discovered in the ruins of Nineveh by Mr. Layard. The earliest standard in England was the old Saxon pound, identical with the old Apoth- ecaries’ pound of Germany (5500 Troy grains). The Pound Sterling was determined from this weight in silver. In 1266, Henry III decreed the following standards: “ 32 grains of wheat from the middle of the ear, well dried, should weigh a pennyweight, of which 20 should go to the ouncetwelve such ounces made the pound, eight pounds one gallon of wine. The denomination of the grain originated with the French. The term “ Troy,” as applied to this system, is derived from the fact that it was brought from the East at the time of the Crusades, and first adopted at Troyes, a commercial town of France. The Troy weights were readily adopted by jewelers and apothecaries for the sake of convenience. The term “Karat” is employed by jewelers, being equivalent to four Troy grains; when meant to express the fineness of gold, the karat means the twenty-fourth part; thus, 14-karat gold means of gold and of base metal. Troy weights are no longer employed in medicine. Sometimes * True and Apparent Weight.—The Zrwe weight of a body is its weight “ in vacuo.” The appar- ent weight is its weight in air under ordinary conditions of atmospheric pressure and temperature. This apparent weight of a body weighed in any medium, as air or water, is less than its true weight, the difference being the weight of the air or water displaced by the body itself, less the weight of the air or water displaced by the weights used. In pharmacy and ordinary commercial weighing the apparent weight only is considered. WEIGHTS AND MEASURES. 9 the words “Troy ounce” are employed,meaning the apothecaries’ ounce. Both are the same, being, however, differently subdivided. Fig. 1. The Pound Weight—Ancient and Modern Standards.* 1. Exchequer Standard Avoirdupois Pound of Queen Elizabeth. 2. Assyrian Bronze Lion Standard Weight. 3. Assyrian Stone Duck Standard Weight. 4. Form of Modern Local Standard Avoirdupois Weight. 5. Official Secondary Standard Pound of Gilt Metal. 6. Imperial Stand- ard of Platinum. 7. Platinum Troy Pound of the Royal Society. 8. Platinum Troy Pound of the Standard Department. 9. Standard Troy Pound of 1758. ’ 10. Exchequer Standard Troy Pound of Queen Elizabeth. 24 grains,.... 1 pennyweight. 20 pennyweights, 1 ounce 480 grains. 12 ounces, 1 pound, 5760 grains. Troy Weight. Signs. Grain, Gr. or gr. Ounce, Oz. or oz. Troy. Pound, lb. * Illustration taken from article by F. H. Taylor, Western Druggist, 1892, p. 175. 10 HANDBOOK OF PHARMACY. Apothecaries’ Weight. 20 grains, 1 scruple. 3 scruples, 1 drachm, 60 grains. 8 drachms, 1 ounce, 480 grains. 12 ounces, 1 pound, 5760 grains. Grain, Gr. or gr. Scruple, 9. Drachm, Ounce, 2. Pound, ib. Signs. AVOIRDUPOIS WEIGHT. This system first appears in use at the time of Edward III (1327-1377), who decreed that “ we will, and establish, that one weight, one measure, and one yard be throughout the land, and that woolens and all manner of avoirdupois be weighed.” The term “avoirdupois” is derived from aver or avoirs (Fr.), meaning “ havings,” the old appellation for portable goods, chattels, etc., and poids (Fr.), meaning “weight,”—“aver de pois,” goods of weight. In time, the term lost its meaning, and later, at the time of Henry VIII (1532), it was ordered that “ beef, pork, mutton, and veal shall be sold by weight” called “ haverdupois;” hence, in early times, the term was applied to goods themselves, and later on to the system of weights employed for these kinds of goods. All goods bought by the apothecary are weighed by the avoir- dupois system. For instance, a |-ounce vial of morphine does not contain | of 480 grains, but | of 437.5 grains, or 54.68 grains; or one ounce of sulphate of quinine is 437.5 grains, and not 480. Avoirdupois Weight. 437.5 grains, 1 ounce, 16 ounces, 1 pound, 7000 grains. 100 pounds, ... 1 hundredweight. 20 hundredweights, 1 ton. 27.34 Troy grains, . . 1 drachm. 16 drachms, ... 1 ounce. Signs. Ounce, Oz. or oz. Pound, . Ib. Hundredweight, cwt. Ton, T. We have one unit common to all, viz.: “ the grain.” The Troy- ounce contains 42.5 grains more than the Avoirdupois ounce. The Troy pound contains 1240 grains less than the Avoirdupois pound. Avoirdupois, . . 437.5 grains in ounce, .... 7000 grains in pound. Troy, J80.0 grains in ounce, .... 5760 grains in pound. Difference, 42.5 grains. 1240 grains. WEIGHTS AND MEASURES. 11 The term “ grain,” is derived from Latin “ granum,” and was originally based on the weight of a grain of wheat * as already stated. Its value is now derived from the weight of a cubic inch of distilled water, weighed in vacuo against brass weights, at 60° F., under a barometric pressure of 30 inches; this, according to the latest calculation, is said to be 252.892 grains. In 1834, the English standards of weight and measure, con- sisting of a yard and a pound Troy of brass, were destroyed at the burning of the Houses of Parliament. Prior to this, great con- fusion existed, three different gallons being in use: The Wine gallon of 231, Corn gallon of 268, and Ale gallon of 282 cubic inches. After this, a revision and restoration was resolved upon, since the duplicates of the standards of brass had suffered oxida- tion. A cubic inch of distilled water weighed in air, against brass weights (of density of 8.3) at the temperature of 62° F., and the barometer at 30 inches (760 Mm.), was determined to be equal to 252.458* grains, of which the standard Troy pound con- tains 5760. As to the unit of length, they adopted the length of a pendulum, swinging seconds of mean time, in a vacuum, at the level of mid-tide in the latitude of London (or 39.13929 inches). From this is now derived the new British standard yard, which is the length at 62° F., between two marks, on the gold plugs of a bronze bar in the Standards Office, London, being 36 of the before-mentioned inches. The Imperial gallon contains 277.24 cubic inches; the Wine gallon being 231 cubic inches. In 1826 this set of weights and measures was finally adopted as a rival to the Metric system, which was then being introduced from France. This system is now employed in medicine and pharmacy in Great Britain. The Imperial standard pound is declared to be the weight of an avoirdupois pound in a vacuum. The Imperial standard of platinum balances the brass weights in a vacuum. The volume of 70,000 grains, or 10 avoirdupois pounds, of pure water at 62° F., and barometer at 30 inches, is the Imperial gallon. The Im- perial pint is divided into 20 fluidounces, and weighs at 62° F. 20 avoirdupois ounces. The gallon, quart, and pint are nearly 20 per cent, larger than the corresponding volumes in wine measure. The fluidounce is about four per cent, smaller than the United States fluidounce. The weights and measures employed in the United States are assumed to be copies of the units of length, and of the old wine and Winchester measures, formerly employed in England, which were discarded years ago. In 1827 the United States procured a copy of the British brass Troy pound for the use of the Mint. This was declared by law in *The value now employed by the United States Coast and Geodetic Survey is 252.333 grains, based on the French determination of the mass of a cubic decimeter of water at its maximum density. 12 HANDBOOK OF PHARMACY. 1873 to be the “standard Troy pound of the Mint of the United States, to which the coinage thereof shall be regulated.” This is the only actual standard we have, a copy of a standard long discarded. Our wine gallon of 231 cubic inches was many years ago abolished by England. So our present system of weights and measures rests upon discarded standards. The Metric System was made lawful, though not compulsory, by Act of Congress in 1866. (The unit of capacity for liquids is the wine gallon of 231 cubic inches.) United States Liquid Measure. Signs. 4 gills,1 pint. Gill,gi. 2 pints, ... 1 quart. Pint,pt. 4 quarts, .... 1 gallon. Quart,qt. Gallon,gal. United States Apothecaries’ or Wine Measure. 60 minims, . . 1 fl. drachm. 8 fl. drachms, . 1 fl. ounce, . 480 minims. 16 fl. ounces, . 1 pint, . . . 128 fl. drachms, . 7680 minims. 8 pints, ... 1 gallon, . . 128 fl. ounces, . 1024 fl. drachms, . 61,440 minims. Signs. Minim, Fluidrachm, fg. Fluidounce,flj. Pint,O. Gallon, Cong, or C. Distilled Water at 15.5° C. (60° F.). 1 minim, 0.95 grains weight. 60 minims, ... 1 fluidrachm, .... 56.96 “ “ 480 “ ... 1 fluidounce, .... 455.69 “ “ 7,680 “ ... 1 fluid pint,7,291.11 “ 61,440 “ ... 1 fluid gallon, .... 58,328.88 “ “ (1 Imperial Gallon, 277.274 cubic inches.) 60 minims, . . 1 fl. drachm. 8 fl. drachms, . 1 fl. ounce, . 480 minims. 20 fl. ounces, 1 pint, . . . 160 fl. drachms, . 9600 minims. 8 pints, ... 1 gallon, . . 160 fl. ounces, . 1280 fl. drachms, . 76,800 minims. Imperial Measure, B. P. Equivalents of Imperial Measure in United States Fluid Measure. (The Imperial Gallon being the weight of 10 avoirdupois pounds of distilled water at 60° F. (15.5° C.). Imperial Measure. United States Wine Measure. 1 minim. 0.96 minims. 1 fluidrachm, .... 57.60 “ 1 fluidounce, .... 460.86 “ ... 7.68 fluidrachms. 1 fluid pint, ... 9,217.34 “ ... 19.202 fluidounces. 1 gallon 73,738.75 “ ... 9.601 pints. WEIGHTS AND MEASURES. 13 We have thus four different ounces: the Troy of 480 grains, the Avoirdupois of 437.5 grains, the Fluidounce of 455.69 grains,* the Imperial B. P. fluidounce of 460.86 (U. S.) minims. The Minim is a very convenient unit of fluid measure; it is nearly equal to the average “ drop ” of distilled water. A minim of distilled water at normal temperature weighs 0.95 grains. The drop varies in size. The measurement of liquids by drops does not give uniform or accurate results. A drop is the resultant of three forces,—gravity, cohesion, and adhesion,—and as these vary, so do drops vary in size; heavy mobile liquids form small drops, viscid liquids form large drops. The quantity of liquid in the vessel, the rapidity of dropping, the size and shape of the lip of the vessel (influencing the adhesive force), and the temperature of the liquid, are all conditions which influence the size of drops. Aqueous solutions average .... 50 to 60 minims to the fluidrachm. Fixed oils “ . . . 65 to 80 “ “ “ “ Volatile oils “ .... 90 to 110 “ “ 4‘ “ Alcohol and alcoholic liquids . . 120 to 140 “ “ “ ‘‘ Ethereal liquids (chloroform) . . . 200 to 300 “ “ “ “ Foreign pharmacists, who are accustomed to weigh fluids, measure the fluid in drops for quantities weighing less than two Fig. 2. Position of Stopper for Dropping. grammes. Some pharmacopoeias state that, on an average, from 20 to 25 drops of distilled water are equivalent to one gramme (one cubic centimeter). Among these, some give tables of the number of drops equivalent to the gramme of each of the official liquids. Thus water, aqueous solutions, fixed oils, heavy volatile oils, tinctures, fluid extracts, etc., may be reckoned as 20 drops to the gramme, light volatile oils, ethereal liquids (Spiritus /Etheris Compositus, Spiritus 2Etheris, etc.), as 25 drops, and ether as 50 drops to the gramme. When drops are to be measured, the bottle should not be over three-fourths filled ; then by means of the stopper, moisten the neck and lip, and allow * Variously stated as 455.6216, 455.6994, and 455.6910 grains. Consult Oldberg’s “ Manual of Weights and Measures.” 14 HANDBOOK OF PHARMACY. the liquid to flow slowly past the stopper held at an angle to the lip (Fig. 2). This insures more regularity in the size of the drops, and prevents the liquid from forming a stream. There area great variety of arrangements for producing drops; none however, are capable of producing drops of the same size from different liquids. Fig. 3. Fig. 4. Fig. 5. Vials for Producing Drops. It is customary for many pharmacists to note on the label of the dispensing bottle the number of drops to the gramme in each special case. APPROXIMATE MEASURES. The following is the approximate capacity of the various household measures:— A tumblerful,fSviij. A teacupful, A wineglassful, ij. A tablespoonful,f£ iv. A dessertspoonful, A teaspoonful,fg j. WEIGHTS AND MEASURES. 15 A TABLE SHOWING THE NUMBER OF DROPS IN A FLUIDRACHM, ALSO THE WEIGHT OF ONE FLUI- DRACHM IN GRAINS AND GRAMMES FOR EACH OF THE PREPARATIONS NAMED. From, a list by S. L. Talbot, Printed in “Era Dose Book," and corrected to agree with the U. S. P, 1890. DROPS IN A FLUIDRACHM. Name. 1 DROPS IN FLUI- DRACHM, 60 MIN. WEIGHT OF FLUI- DRACHM. Name. DROPS IN FLUI- 1 DRACHM, 60 MIN. WEIGHT OF FLUI- DRACHM. 1 In Grains. CO In Grains. — ® Acetuni Opii, 90 61 3.95 Liquor Hydrargyri Nitratis, . 131 123 7.97 Scillie, 68 57 3.69 lodi Compositus, 63 59 3.82 Acidum Aceticum, 108 58 3.75 Potassa, 62 58 3.75 Aceticum Dilutum 68 55 3.56 Potassii Arsenitis, 57 55 3.56 Carbolicuni, 111 59 3.82 Soda Chlorata, 63 62 4.01 Hydrochloricuni, 70 65 4.21 Zinci Chloridi, 89 88 5.70 Dilutum, 60 56 3.62 Oleoresina Aspidii, 130 52 3.36 Hydrocvanicum Dilutum, . . 60 54 3.49 Capsici, 120 51 3.30 Lactieum, 111 66 4.25 Cubeba 123 52 3.36 Nitricum, 102 77 4.98 Oleum zEthereum, 125 50 3.24 Dilutum, 60 58 3.62 Amygdala Amara, 115 55 3.56 Nitrohydrochloricum, .... 76 66 4.27 Expressum, 108 48.5 3.14 Phosphoricum Dilutum, . . . 59 57 3.69 Anisi, 119 54 3.49 Sulphuricum, 128 101 6.54 Bergamottae, 130 46 2.98 Aromaticum, 146 53 3.43 Can, 132 50 3.24 Dilutum, 60 58.5 3.79 Caryophylli, 130 57 3.69 Sulphurosum, 59 55 3.56 Cinnamdmi, 126 53.5 3.46 JEther, 178 39 2.52 Copaiba, 123 49.5 3.20 Alcohol, 146 44 2.85 Cubeba, 125 51 3.30 Dilutum 137 49 3.17 Faniculi. 125 53 3.43 Aqua, 60 55 3.56 Gaulthena, 125 62 4.01 Ammonia Fortior, 66 50 3.24 Juniperi, 148 49 3.17 Destillata, 60 53.5 3.46 Lavandula Florum, 138 52 3.36 Balsamuni Peruvianum, .... 101 60 3.88 Limonis, 129 47 3.04 Bromum, 250 165 10.69 Mentha Piperita, 129 50 3.24 Chloroformum, 250 80 5.18 Ricin i 77 51.5 3.33 Copaiba, 110 51 3.30 Rosa, 132 47 3.04 Creosotum, 122 56.5 3.66 Rosmarini, 143 50 3.24 Extractuni Belladonna Radicis Sassafras, 133 58 Fluiduni, 156 57 3.69 Terebinthina, 136 45.5 2.94 Cimicifuga Fluiduni, .... 147 48 3.11 Tiglii, 104 50 3.24 Cinchona Fluidum, . . 138 58 3.75 Spiritus zEtheris Compositus, . 148 45 2.91 Colchici Radicis Fluiduni, . . 160 37 3.69 zEtheris Nitrosi, 146 47 3.04 Seminis Fluidum, 158 55 3.56 Ammonia Aromaticus, . . . 142 48 3.11 Digitalis Fluidum, 134 62 4.01 Chloroformi, 150 48 3.11 Gelsemii Fluidum, 149 49 3.14 Mentha Piperita, 142 47 3.04 Hyoscyami Fluidum, .... 160 59 3.82 Syrupus, 65 72 4.66 Ipecacuanha Fluidum, . . . 120 60 3.88 Ferri lodidi, 65 77 4.98 Pareira Fluidum 140 51 3.72 Tinctura Aconiti, 146 46 2.98 Rhei Fluidum, 158 61 3.95 Belladonna Foliorum, . . 137 53 3.43 Sarsaparilla Fluidum Com- Cantharidis, 131 51 3.33 positum, 134 60 3.88 Cinchona Composita, .... 140 49 3.17 Senega Fluidum, 137 62 4.01 Digitalis, 128 53 3.43 Serpentaria Fluidum, . . 148 47 3.07 Ferri Chloridi, 150 53 3.43 Uva Ursi Fluidum, 137 60 3.88 lodi, 148 47 3.04 Valeriana Fluidum, .... 150 49 3.17 Nucis Vomica, 140 44 2.85 Veratri Viridis Fluidum, . . 150 50 3.24 Opii, 130 53 3.43 Zingiberis Fluidum, . . . 142 48 3.11 Camphorata, 130 52 3.36 Glyeerinum 67 68 4.40 Deod'orati 110 54 3.49 Liquor Acidi Arsenosi, .... 57 55 3.56 Valeriana, 130 52 3.36 Ammonii Acetatis, 75 56 3.62 Veratri Viridis, 145 46 2.98 Arseni et Hydrargyri lodidi, 58 55 3.56 Zingiberis, 144 46 2.98 Ferri Citratis, 71 72 4.66 Vinum Colchici Radicis,.... 107 55 3.56 Nitratis, . . 59 59 3.82 Colchici Seminis, 111 54 3.49 Subsulphatis, 73 83 5.37 Opii 100 55 3.56 Tersulphatis, 83 72 4 66 This originated in France in 1790, with the selection of a defi- nite value, the one ten-millionth part of the earth’s quadrant, the calculated distance from the earth’s equator to the pole; this METRIC SYSTEM, OR DECIMAL SYSTEM. 16 HANDBOOK OF PHARMACY. value can be calculated at any time it may be necessary. Any immaterial object may be taken as a standard for a system, pro- vided it represents a fixed and absolute value, which can always be calculated and reproduced, should the standard be lost. This is fulfilled by the Metric System. Its name originated from the Greek word pLpov, meaning “measure.” The original standard Meter, represented by the distance between certain marks on a bar of platinum, is preserved in the French Archives in Paris, duplicates of which have been furnished to a number of other countries. It is universally employed in scientific work, and is the legal standard in most European countries, except Great Britain, receiving official sanction in the English-speaking countries. Although Washington called the attention of Congress to the advantages of this system in 1795, and Madison in 1816, again later in 1821, it did not receive official recognition until the year 1866, when, by act of Congress, it was declared “ lawful in the United States to employ the weights and measures of the metric system.” It was officially introduced into the Marine Hospital service, and later endorsed by various scientific societies. The U. S. Pharmacopoeia of 1890 has adopted the system entirely. For the student, in learning this system, it is preferable to refrain from comparing each term, mentally, with the correspond- ing term in the system familiar to him. Such comparisons or conversions have, of course, frequently to be made, but while fixing the system into the memory, it is best to treat it independ- ently of any other system. The Metric System is based on the meter, which is the standard unit of linear measurement. The Standard Metric Unit of Weight is the weight of one cubic decimeter of pure water at 4° C., represented by a piece of metal preserved at Paris, called the Kilogramme. The Standard Unit of Volume is the Liter, which is the volume of one cubic decimeter of pure water at 4° C. (weighing one Kilogramme). Of these standards, there are a few derivatives commonly employed, namely, the cubic centimeter, which is a volume- capacity represented by a cube, each face of which is 1-100 of a meter, 1000 of these constituting a Liter. The Gramme is the weight of one cubic centimeter of pure water at its greatest density. 1000 grammes constitute the kilo- gramme. This system is called decimal, since the various units and parts thereof, are derived from the standard unit by a system of deci- mals (decern—10). On the same principle we divide our dollar into fractions, represented by tenths, hundredths, or thousandths, or into multiples thereof, by tens, hundreds, and thousands. For the sake of simplicity, a system of prefixes is employed derived from Greek ERRATA. Page 17.—The 25th, 26th, and 27th lines from the top should read, 10 milligrammes = 1 centigramme = 0.01 gramme. 100 “ = 10 “ 1 decigramme = 0.1 gramme. 1000 “ =100 “ 10 “ 1.0 “ Page 19. — The 7th line should read decigramme instead of decimeter. Page 19. — The 8th line should read centigramme instead of centimeter. WEIGHTS AND MEASURES. 17 numerals to express the upward scale, or multiple fractions, and from Latin numerals to express the downward scale, or decimal fractions. Greek increases Deca, ... 10 times. Hecto, . . 100 Kilo, . . . 1000 “ Latin decreases Deci, . . . 1-10 part. Centi, . . 1-100 “ .Milli, . .1-1000 “ In the following table we find a general view of the system with its application of decimals:— 1000. Kilometer, Km. 1000. Kiloliter, KI. 1000. Kilogramme, Kg. 100. Hectometer, Hm. 100. Hectoliter, Hl. 100. Hectogramme, Hg. 10. Dekameter, Dm. 10. Dekaliter, DI. 10. Dekagramme, Dg. 1. Meter, M. 1. Liter, L. 1. Gramme, Gm. 0.1 Decimeter, dm. 0.1 Deciliter, dl. 0.1 Decigramme, dg. 0.01 Centimeter, cm. 0.01 Centiliter, cl. 0.01 Centigramme, cg. 0.001 Millimeter, mm. 0.001 Milliliter, ml. 0.001 Milligramme, mg. M.,meter. Cm.,centimeter. Mm.,millimeter. L.,liter. Cc., cubic centimeter. Gm.,gramme. Cg.,centigramme. Mg.,milligramme. 1 milligramme = 0.001 gramme 10 milligrammes = 1. centigramme = 0.01 gramme 100 “ 10. “ 1. decigramme = 0.1 gramme 1000 “ 100. “ 10. “ 1.0 “ All of the before-mentioned terms are not in common use. Of measures of weights, the kilogramme (often called simply the Kilo), gramme, centigramme, and milligramme are usually employed in pronouncing a given weight. For instance, 16.143 Gm. is not read “ sixteen grammes, one decigramme, four centi- grammes, and three milligrammes,” but 1116 grammes and 143 milligrammes.” Of measures of capacity, only the liter and cubic centimeter are usually employed. Of measures of length, the meter, centimeter, and millimeter are commonly in use. In microscopic work, the thousandth part of a millimeter (micromillimeter—mkm ; also called micron, the symbol of which is m) is often employed. One side of the cube (Fig. 6) is supposed to measure one-tenth of a meter or one decimeter, and if each side be the same, the ca- pacity of the cube represents one liter (1000 Cc.); the lower edge is divided into ten parts, each representing in length the one- hundredth part of a meter, or one centimeter; the capacity of a cube constructed on this, represents one cubic centimeter, which 18 HANDBOOK OF PHARMACY. when filled with pure water at 4° C. weighs one gramme; the upper edge is subdivided into centimeters and millimeters, (urn)* . , For the purpose of approximately converting terms of the Metric into our own United States system, and vice versa, it is Fig. 6. Scale of Milxt 3.9370432 Inches. I L itre = I OO O C.C. Metric Diagram—Comparison of Measures of Length, Capacity, Weight. not necessary, for practical purposes, to apply a series of rules, but merely to remember the comparative value of the chief standards. For instance :— 1 meter (for measures of length), 39.37 inches. 1 gramme (for measures of weight), .... 15.432 grains. 1 cubic centimeter (for measures of capacity), 16 minims (30 Cc. = 1U. S. fiuidounce). WEIGHTS AND MEASURES. 19 From these we can readily calculate the different values:— 1 meter, 39.37 inches. 1 decimeter, 3.93 “ 1 centimeter, 0 39 “ or about f of an inch. 1 millimeter, 0.039 “ “ “ “ 1 gramme, 15.432 grains. 1 decimeter, 1.5432 “ 1 centimeter, 0.15432 “ or about | of a grain. 1 milligramme, 0.015432 “ “ “ “ 1 kilogramme, 15432. “ “ “ 2.2 av. lbs. 1 cubic centimeter, 16 minims, or about | U. S. fluidrachm. 4 Cc., 1 fluidrachm. 16 Cc., 4 “ 32 Cc., 1 fluidounce. 500 Cc., 16.9 fluidounces. 1000 Cc., 33.8 “ The above figures are approximately correct and answer for all practical purposes. For table of equivalents of the various systems refer to the Appendix. For reading and writing the various quantities of the Metric system, the following examples may be given:— 25 grammes are written, 25.0 (25X1.0, 25.0 ) 25 decigrammes are written, . . . 2.5 (25 X 0.1, 2.5 ) 25 centigrammes “ “ ... 0.25 (25X0.01, .... 0.25 ) 25 milligrammes “ “ ... 0.025 (25 X 0.001, .... 0.025) or 1000 grammes are written, . . . 1000.0 or 1 Kilo 1 Kg. 500 “ “ “ ... 500.0 “ j Kg. 250 “ “ “ ... 250.0 “ | Kg. 100 decigrammes are written, . . 10.0 (100X0.1, . . . . 10. ) 100 centigrammes “ “ . . 1.0 (100X0.01, .... 1.0) 100 milligrammes “ “ . . 0.1 (100X0.001, . . . 0.1) 1000 cubic centimeters are written, 1000 Cc., or 1 Liter. 500 “ “ “ “ 500 Cc., “ i “ 250 “ “ “ “ 250 Cc., “ J “ 20 HANDBOOK OF PHARMACY. EQUIVALENTS OF METRIC WEIGHTS AND MEASURES.* Avoirdupois Weight in Grammes. 1-16 oz. = 1.772 grammes. % oz. = 3.544 grammes. U oz. = 7.088 grammes. % oz. = 14.175 grammes. 1 oz. = 28.350 grammes. 2 ozs. = 56.699 grammes. 3 ozs. = 85.049 grammes. 4 ozs. = 113.398 grammes. 5 ozs. = 141.748 grammes. 6 ozs. = 170.098 grammes. 7 ozs. = 198.447 grammes. 8 ozs. = 226.796 grammes. 9 ozs. = 255.146 grammes. 10 ozs. = 283.496 grammes. 11 ozs. = 311.846 grammes. 12 ozs. = 340.195 grammes. 13 ozs. = 367.544 grammes. 14 ozs. = 396 894 grammes. 15 ozs. = 425.243 grammes. 1 pound = 453.592 grammes. 2 pounds = 907.18 grammes. 3 pounds = 1360.78 grammes. 4 pounds = 1814.37 grammes. 5 pounds = 2267.96 grammes. 6 pounds = 2721.55 grammes. 7 pounds = 3175.14 grammes. 8 pounds = 3628.74 grammes. 9 pounds = 4082.33 grammes. 10 pounds = 5435.92 grammes. U. S. Fluid Measure in Cubic Centimeters. 1 minim = .06 cubic centimeter. 2 minims = .12 cubic centimeter. 3 minims = .18 cubic centimeter. 4 minims = .25 cubic centimeter. 5 minims = .31 cubic centimeter. 10 minims = .62 cubic centimeter. 20 minims = 1.23 cubic centimeters. 30 minims = 1.85 cubic centimeters. 1 fluidrachm = 3.70 cubic centimeters. 2 fluidrachms = 7.39 cubic centimeters. 3 fluidrachms = 11.09 cubic centimeters. 4 fluidrachms = 14.79 cubic centimeters. 5 fluidrachms = 18.48 cubic centimeters. 6 fluidrachms = 22.18 cubic centimeters. 7 fluidrachms = 25.87 cubic centimeters. 1 fluidounce = 29.57 cubic centimeters. 2 fluidounces = 59.14 cubic centimeters. 3 fluidounces = 88.72 cubic centimeters. 4 fluidounces = 118.29 cubic centimeters. 5 fluidounces = 147.86 cubic centimeters. 6 fluidounces = 177.44 cubic centimeters. 7 fluidounces = 207.01 cubic centimeters. 8 fluidounces = 236.59 cubic centimeters. 1 pint = 473.17 cubic centimeters. 1 quart = 946.35 cubic centimeters. 1 gallon = 3785.51 cubic centimeters. Metric in United States Fluid Measure. 1 cubic centimeter = 16.23 minims. 2 cubic centimeters = 32.46 minims. 3 cubic centimeters = 48.69 minims. 4 cubic centimeters = 1.08 fluidrachms. 5 cubic centimeters = 1.35 fluidrachms. 10 cubic centimeters = 2.71 fluidrachms. 25 cubic centimeters = 6.76 fluidrachms. 30 cubic centimeters = 1.01 fluidounce. 50 cubic centimeters = 1.69 fluidounces. 100 cubic centimeters = 3.38 fluidounces. 500 cubic centimeters = 16.90 fluidounces. 1000 cubic centimeters = 38.81 fluidounces. Troy Weight in Grammes. 1-100 grain = 0.00065 gramme. 1-64 grain = 0.00101 gramme. % grain = 0.00810 gramme. % grain = 0.01620 gramme. % grain = 0.03240 gramme. 1 grain = 0.0648 gramme. 1% grains = 0.0972 gramme. 2 grains = 0.1296 gramme. 5 grains = 0.3239 gramme. 10 grains = 0.6479 gramme. 20 grains = 1.2960 grammes. 30 grains = 1.9440 grammes. 60 grains (1 troy drachm) = 3.8880 grammes. 2 drachms = 7.7760 grammes. 4 drachms = 15.5520 grammes. 1 ounce = 31.1035 grammes. 2 . ounces = 62.201 grammes. 3 ounces = 93.31 grammes. 4 ounces = 124.41 grammes. 5 ounces = 155.51 grammes. 6 ounces = 186.62 grammes. 7 ounces = 217.72 grammes. 8 ounces = 248.82 grammes. 9 ounces = 280.00 grammes. 10 ounces = 311.03 grammes. 11 ounces = 342.14 grammes. 12 ounces = 373.24 grammes. 14 ounces = 435.44 grammes. 16 ounces = 497.65 grammes. 24 ounces = 746.48 grammes. 48 ounces = 1492.95 grammes. 100 ounces = 3110.40 grammes. U. S. in Metric Linear Measure. = 6.35 millimeters. %inch = 12.70 millimeters. %inch = 19.05 millimeters. 1 inch = 2.54 centimeters. 2 inches = 5.10 centimeters. 3 inches = 7.62 centimeters. 4 inches = 10.20 centimeters. 5 inches = 12.70 centimeters. 6 inches = 15.24 centimeters. 7 inches = 17.78 centimeters. 8 inches = 20.32 centimeters. 9 inches = 22.86 centimeters. 10 inches = 25.40 centimeters. 11 inches — 27.94 centimeters. 12 inches = 30.48 centimeters. Metric Weights in Grains. .050 gramme = .772 grain. .100 gramme = 1.543 grains. .250 gramme = 3.858 grains. .500 gramme = 7.716 grains. 1 gramme = 15.432 grains. 2 grammes = 30.865 grains. 3 grammes = 46.297 grains. 4 grammes = 61.729 grains. 5 grammes = 77.162 grains. 10 grammes = 154.323 grains. 25 grammes = 385.809 grains. 50 grammes = 771.617 grains. 100 grammes = 1543.235 grains. 500 grammes = 7716.174 grains. 1000 grammes = 15432.350 grains. * The Era Dose Book. WEIGHTS AND MEASURES. 21 WEIGHTS. Weights are small pieces of metal (or glass, etc.) so adjusted as to correspond with the legal standards. Commercial weights are of iron, brass, or bronze. Analytical weights are made of brass, and should be plated with either gold or platinum, to protect them from corrosion or oxidation, which usually takes place in brass or other metals. Those of smaller denomination, from 0.5 Gm. down, are usually made of aluminum or platinum. Weights of agate are also to be had; the value of these is at once apparent. The balance is any instrument based upon the principle of the equal or unequal lever, for determining the relative weights or THE BALANCE. Fig. 7. Balance. masses of bodies. A balance consists of an inflexible metallic beam (A B) supported horizontally, exactly over its center of gravity, by the fulcrum (n), which consists of a steel or agate prism, passing through the beam, and resting with its sharp edge upon two supports of steel or agate. At the extremities of this beam, pans are suspended in such a manner, that they may turn freely about axes passing through the extremities of the beam, and parallel to its axis of rotation. Thus we have three steel or agate edges; the middle one edge downward supporting the beam, and those at the extremities edge upward. On these are 22 HANDBOOK OF PHARMACY. supported the agate or steel plates to which the pans are attached. Every equal-arm balance possesses three important points,—the fulcrum (point of support) and the extremities of the two arms. At one extremity the force acts, and at the other the weight. The two arms must be precisely equal in length, the pans must also be of equal weight. To prove these two conditions, place two equal weights, one in each pan, until the beam becomes exactly horizontal, as shown by the pointer; then interchange the weights, and it will remain horizontal if the arms are equal. The center of gravity of the lever or beam should be as near as possible, yet immediately below, the fulcrum. In Fig. 8 the effect of a change in the position of the center of gravity, is shown by raising or lowering the fulcrum c by means of screw b. When the fulcrum is at the top of the groove, the center of gravity of the beam is below its edge, and the latter os- cillates freely about a position of stable equilibrium. By lower- ing the fulcrum it may be brought to the exact center of gravity, where the beam no longer oscillates, but remains in equilibrium Fig. 8. Beam with Movable Fulcrum. in all positions. When the fulcrum is brought below the center of gravity, the beam is in a state of unstable equilibrium and is overturned by the least displacement. In balances for heavy weights, the center of gravity is placed lower than in delicate instruments, for by this arrangement the beam oscillates more readily, though it requires a larger weight- to start it. Single Beam, Equal-Armed Lever Balances.—In a delicate or analytical balance, the axes of rotation are formed by agate knife edges bearing on polished agate plates. The beam is pro- vided with three agate edges, the middle one, edge downward, serving as support of the beam itself, and those at the extremities with knife-edges upward, on which are supported the agate plates, to which the pans are attached. The beam is made as light as pos- sible. There should also be a frame support to both the pans and beam, so that the beam may at any moment be released from contact with the agate plates, and the delicate knife-edges may not sustain injury from pressure or shocks. In order to define the position of the beam of the balance, a long metal pointer is fixed to it and oscillates with it. A small graduated index is fixed 23 WEIGHTS AND MEASURES. near the base of the pillar and the motion of the beam is observed by noting the motion of the pointer along this index. When the balance is in good adjustment, the pointer should be opposite the central mark of the in- dex, showing the beam to be horizontal. Levels should be placed in the glass case containing the balance, to show that it is in proper position, for a balance must always stand perfectly level? A balance is delicate when a very minute difference be- tween the weights in the pans, causes a per- ceptible deflection of the pointer. To assist this, the beam should be as light as possible consistent with its rig- idity. Since friction opposes the action of the forces, the number of points of friction should be as few as possible, and, in addition to this, the edges upon which the beam and pans are supported, should be made as hard as possible; hence agate is chosen with preference, as it is not liable to corrosion, like steel. In the more accurate balances, the beam is divided into ten parts with subdivisions, in- dicating milligrammes and tenths thereof. Above the beam is a brass rod, provided with a small hook, which can be moved back and forth from the outside. By its aid a small w’eight, in the form of a bent wire called a rider, usu- ally weighing 1 milligramme, may be placed on any of the divisions of the beam. By means of this, minute weigh- ings may be made where larger weights are not suitable. In weighing a body on an analytical balance, place it clean and dry upon one pan, then place a corresponding weight on the other pan, and slowly remove the frame supports of the arm and pans by means of the key; if on so doing, the indicator shows that one Fig. 9. Analytical Balance. Fig. 10. Prescription Balance. 24 HANDBOOK OF PHARMACY. pan is heavier than the other, restore the supports and change the weights accordingly, continuing this until the pointer swings equally about the center point, or remains stationary at the center. What has been said about the analytical balance also holds good for the prescription balance. Never load or unload a pan when the beam is rotating, but first arrest the scale-pans. Weights should be placed and removed by means of a pair of ivory-pointed pincers. Loads and weights must be placed on the pan carefully, and not suddenly. In weighing powders, employ watch-glasses, which should have been carefully adjusted to equilibrium. No fuming liquids should be weighed on a delicate balance, unless in a properly closed vessel. Each object, before being -weighed, should be wiped perfectly dry. Before attempting to load any balance, first see that the beam moves freely about, and finally rests in a state of equilibrium. An analytical or prescription balance should be kept in a dry and clean room, where there is but little variation of temperature, and should be enclosed in a suitable glass case. A balance should never be overloaded. Each one has its safe limit of capacity, and suffers accordingly when overtaxed. It is customary to place a wide-mouthed flask or capsule con- taining sulphuric acid or calcium chloride inside of the balance case, to keep the air as dry as possible. Hand Scales.—This form of scale consists of a brass beam MAXIMS. Fig. 11. Fig. 12. Hand Scales. Proper Way of Holding Hand Scales. with a central knife edge, which is enclosed, to protect it from dust and corrosion as much as possible. The two pans are of horn supported by silken cord from wire hooks, which are hung from perforations in each end of the beam; a pointer, perpendicular to 25 WEIGHTS AND MEASURES. the beam, oscillates between the supporting arms. In weighing, the scales should be grasped by the hook above (Fig. 12), between the thumb and fore-finger, the equilibrium of the beam being pre- served by holding the fourth and fifth fingers on either side. While the pans are loaded, any slight deviation to either side is felt at once by the indicator oscillating to the right or left; before the material is removed, the balance should be allowed to swing free. These hand balances, with care, can be used for weighing quantities as low as one centi- gramme. They should not be em- ployed for weighing alkaloids or po- tent drugs. For this purpose, only the sensitive prescription balance (Fig. 10) should be employed. A similar form called the Army Bal- ance (Fig. 13), in which the beam is supported upon a rigid pillar, is very convenient for prescription use, but in- asmuch as they are made of brass and all the metal bearings are exposed, they soon corrode; the sensitive parts become filled with Fig. 13. Army Prescription Scales. Fig. 14. Counter Balance. dust, and the balance becomes worthless. Such a balance should be kept under a glass cover protected from moist air and dust. Fig. 14 illustrates a form of Counter Balance, which is very con- 26 HANDBOOK OF PHARMACY. venient and quite accurate. They should be lacquered to prevent rusting. Figs. 15, 16 illustrate two forms of the counter scale, in which the pans are above the beams; the one (Fig. 16) is provided with Fig. 16. Fig. 15. Counter Balance (Laboratory). Counter Balance (Dispensing). a graduated parallel bar, upon which a poise slides back and forth. This is very useful for counterpoise weighing. Single Beam, but Unequal-Armed Lever Balances.—The simplest form of these is the old steelyard or Roman balance, in which only the shorter arm bears a pan; the longer arm, by Fig. 17. Gorham Dispensing Balance. means of notches, is divided into a scale, over which slides a counterpoise weight. An embodiment of this same idea is the Gorham dispensing balance (Fig. 17) in which a rod or tube, slid- ing within a tubular arm, replaces the external movable weight. The same principle, is shown in the Fairbank’s druggists’ scale, in which the inequality in the length of a beam permits the use WEIGHTS AND MEASURES. 27 of a sliding counterpoise weight along the longer graduated arm. This possesses the advantage that it dispenses witli the use of small weights. Fig. 19 illustrates a new form of Double Beam and Un- equal-Armed Balance, which is specially adapted for weighing liquids. It will weigh liquids up to ten kilos and over with an accuracy, that cannot be approached by ordinary methods. The scale is provided with two weigh- ing beams and sliding poises. One of these is divided into one hundred parts, each part represent- ing one gramme; the other beam is divided into ten parts, each representing one hun- dred grammes. A bar with a sliding poise is placed under and between the weighing beams, for the purpose of balancing the empty bottle or con- tainer, which is quickly done by sliding the poise along the bar until equi- librium is secured. A convenient form of vest-pocket prescription scale based on this principle, is that made by Shepard & Dudley, of New York. Fig. 18. Fairbank’s Druggists’ Scale. Fig. 19. Balance for Weighing Solutions. Fig. 20. Physician’s Vest-pocket Scale. It is very convenient for physicians, and answers very well as a substitute for the horn-pan balance. Compound Lever Balances.—This system is based on the old Robervahl balance, in which the pans are above a system of 28 HANDBOOK OF PHARMACY. levers (which is usually concealed in a box). In this system, practical convenience and rapidity are gained, at the expense of accuracy. The great objection to this form is that it will never vibrate as smoothly as the other forms of balances, because of the great friction in the numerous pivots. The Counter Scale, illus- Fig. 21. Counter Scale. trated in (Fig. 21), is constructed upon this principle, having a large number of points of friction. The Box Prescription Scale (Fig. 22) is constructed upon this same principle. These scales are, indeed, very convenient, being enclosed and protected from dust and air. They do not, however, long retain their accuracy, hence are not well adapted for prescription use. These defects of the Com- pound Lever Balance have been overcome to a great extent by the Springer Tor- sion Balance, in which the knife edge, upon which the old form of balance depends, is replaced by thin steel springs, stretched tightly between bearings, the center of the beam being fastened to the center of the strained spring and at right angles to it. Under this condition, the beam will vibrate precisely as an ordinary beam, balanced upon knife edges. Torsional resistance tends to hold the beam in a horizontal position. This is overcome, however, by placing an adjustable weight (supported on a perpendicular rod attached to the beam) just over the center of gravity; this has the tendency to produce unstable equilibrium, and induces vibration to either side. This weight (ball) can be raised or lowered on the perpendicular rod, thereby regulating sensitive- ness (Fig. 23); it is now replaced by two smaller weights, one on either side of the central frame (Fig. 24). From the illustra- Fig. 22. Box Prescription Scale. WEIGHTS AND MEASURES. 29 tions, the balance will be seen to consist of two beams (upper and lower), supported on three frames of like size. Over each of these, Fig. 23. Fig. 24. Torsion Counter Scale. Torsion Counter Scale. a steel wire (band) is stretched, which forms the support for the beam. Figs. 23, 24, illustrate two forms of counter scale which are sensitive to | grain, and will carry 20 pounds without injury. The one shown in figure 24, is provided with a triple graduated beam with sliding weight, inside the glass case; this beam is graduated in the Metric, Troy and Avoirdupois systems. Fig. 25, illustrates the prescription bal- ance, enclosed in a glass case with rider and adjustment, by means of which, from | grain to 8 ouncescan be weighed with the upper half of the graduated beam, and from J centi- gramme to 5 decigrammes, with the lower half. The balance is said to be sensitive to of a grain. Fig. 26. Triple Graduated Beam. The principal advantage possessed by this balance, is its freedom from friction; hence its greater accuracy; the only objection it is open to, is the unavoidable rigidity of the elastic wires. 30 HANDBOOK OF PHARMACY. Care.—The Counter scale should be placed on a firm, level surface, where it will not be exposed to any jarring or corrosive vapors. It should be frequently cleansed with soft leather, care being taken to remove particles of dust that may collect on any exposed points; when used, the pans should always be covered with counterbalanced pieces of glazed paper, to avoid the adher- ing of moist powders, which, in time, would cause corrosion; when the pans are to be cleaned, they are best washed with warm soap- suds and well dried. Never scour the pans or any of the working parts of a balance. Weights.—The commercial weights are usually circular and flat; the older styles were made cup-shaped, fitting one into the other. These forms will answer very well for commercial pur- Fig. 27. Fig. 28. Fig. 29. Avoirdupois Iron Weights. Metric Iron Weights. Cup Weights (Troy). poses, for weighing by the pound, but will never do for weighing small amounts, where any degree of accuracy is required, since, owing to the numerous cavities, filth is apt to collect in them. It is always preferable to buy the so-called Block-weights, lacquered. These are conveniently arranged in regular order in a wooden block, thus enabling the user readily to find any desired weight; Fig. 31. Fig. 32. Block Weights. Prescription Weights (Metric). Analytical Weights. also, they do not receive the rough usage and wear in handling, as the cup-shaped form. Every apothecary should be provided with a set of accurate prescription weights (Fig. 31); these usually come in wooden blocks with hinged covers, and are generally made of brass, except those of denominations from 10 grains, or from 500 milligrammes down, which are usually made of alumi- num. Each box of weights should be provided with a pair of WEIGHTS AND MEASURES. 31 smooth-pointed pincers (preferably tipped with ivory), for the purpose of handling the weights. Never handle prescription or analytical weights with the fingers. Figs. 33, 34. Aluminum Wire Weights. Aluminum Grain W eights. The apothecaries’ coin brass weights, as usually employed throughout the country, are very inaccurate, owing to the careless, cheap manufacture, and constant rough handling and corrosion. The brass-foil grain weights are subject to the same objection; the Figs. 35, 36, 37, 38. Apothecaries’ Coin Weights. Brass-foil Grain Weights. Brass Metric Weights. Aluminum Wire Weights (Metric). Aluminum Metric Weights, best form of grain weights are those of aluminum wire, their angular form rendering them easily distinguishable; these do not corrode. 32 HANDBOOK OF PHARMACY. MEASURING FLUIDS. For the measurement of fluids, the apothecary employs almost altogether the glass graduate. This has entirely supplanted the old form of porcelain measuring cup, which being graduated inside, made it very difficult to measure off' fluids with any degree of accu- racy. Glass graduates are now furnished in various forms and designs; the tumbler-shaped is generally preferred, because of the ease with which it is cleaned. These are recommended for measuring quantities over one fluidounce (30 Cc.). Because of its smaller diameter near the bottom, the conical form admits the meas- uring of the smaller quantities with more accuracy; however, some forms of these are not as easily cleansed as those of wider bottom. Lately, an im- provement has been made by graduating measures doubly; upon one side, the U. S. fluid measures are marked, while on the other, measures of the metric system are indicated. For the accurate measurement of smaller volumes, small graduated cylinders are preferably employed. These are graduated into fluidrachms and minims, or cubic centimeters and fractions thereof. Fig. 39. Porcelain Measuring Cup. Fig. 40. Fig. 41. Fig. 42. Tumbler-shaped Graduate. “Acme” Graduate. Conical-shaped Graduate. Great care should be exercised in the selection of graduates, and only measures of guaranteed accuracy, or such which have been verified, should be accepted. It is advisable to select meas- ures in which the graduating mark passes entirely around the graduate, which assists in securing the level of the fluid with more accuracy. We cannot expect to measure accurately, if the graduate be WEIGHTS AND MEASURES. 33 held at an angle, instead of perpendicularly, as it should be. The measure should be grasped just above the base, between the thumb and forefinger, the weight being supported upon the other three fingers; and it should be held so that the rings of graduation are in a perfectly horizontal plane. In order to test the accuracy of a graduate or measuring cylin- der, it should be carefully counterbalanced on a pair of sensitive scales, then the requisite weight of distilled water corresponding to a given volume at 60° F. poured in, for which purpose the fluidounce may be reckoned equal to 455.69 grains, or the cubic centimeter equal to 1 gramme. Then the measure should be Fig. 43. Fig. 44. Fig. 45. Cubic Centimeter and Minim Measures. placed on a perfectly level surface, and the height of the water as compared with the marks of the measure carefully noted. For measuring very small volumes, such as 20 minims (or 1 Cc.) or less, the minim graduate should not be used, since there is a considerable loss of fluid in draining off, which adheres to the side of the measure. If the graduate can be rinsed out with other fluids subsequently entering the same mixture, the loss is avoided. Where such is not the case, recourse is had to the measuring pipette (page 165). These pipettes are constructed of various capacities ; the larger sizes, which usually have a bulb, hold 5, 10, 20, and 50 cubic centimeters respectively ; the smaller, which are plain, graduated tubes, hold one fluidrachm, graduated into fractions and minims, or one cubic centimeter divided into tenths CHAPTER II. SPECIFIC GRAVITY. DENSITY* Specific Gravity may be generally defined, as the weight of a body compared with the weight of an equal volume of some standard substance. For liquids and solids, the standard chosen is distilled water at 4° C. (39° F.). Specific gravity expresses a relative, and not an absolute value. It states how many times lighter or heavier the known volume of a body is, than the same volume of another, which is taken as a standard. When we say that the specific gravity of mercury is 13.5, we mean that 1 cubic centimeter, or 1 fluid ounce, or 1 liter, etc., of it is 13.5 times as heavy as the same volume of water. A knowledge of specific gravity often assists qualitative tests in the identification of miner- als, metals, salts, organic substances, fluids, etc. It often enables us to ascertain their purity, as the presence of foreign bodies exerts an influence upon their specific gravities, causing them to be raised or lowered. It enables us to tell at once what any given volume of a liquid should weigh, or conversely, what volume will be required to contain any given weight. From the specific gravity we can readily calculate the percentage strength of many fluids, such as acids, alkaline solutions, solutions of salts, etc. From the specific gravity of urine, the physician diagnoses certain diseases. Since all bodies expand or contract by change of temperature, it is necessary carefully to observe this when determining specific gravities, for 1 Cc. of water at the temperature of 4° C. or 39° F. (its greatest density) weighs 1 gramme, while the same volume at a temperature of 15.5° C. or 60° F. weighs 0.999 Gm. The standard volume of water for unity (1000) used for comparison, varies in different nations, being on the Continent of Europe generally taken at its maximum density (4° C.), in Great Britain at 16.6° C., and in the United States at 15.5° C., together with the Pharmacopoeia standard of 15° C. For general purposes, we express the value of any specific * On account of its more general use the term specific gravity is retained, although “ density” is more accurate. The former involves the consideration of the action of the earth’s attraction on the body to be examined. This attraction is not uniform over the whole of the earth’s surface, being 1 to 2 per cent, less at the Equator than at the Poles. Practically, no difficulty arises from this fact, for we generally take the specific gravity or density of a body by means of a balance, in which case the relationship between object weighed and the weights, remains unchanged. When we employ the .Tolly spring balance (Fig. 61), the above difficulty arises, in which the object is less attracted at the Equator, than at other parts of the earth’s surface. 34 35 SPECIFIC GRA VITY. DENSITY. gravity to three places of decimals, which usually involves more or less error in the third place; however, where greater accu- racy is required, it is expressed to four, five, or more decimal places, the necessary corrections being applied to eliminate errors as far as possible. SPECIFIC GRAVITY OF SOLIDS. The methods for the determination of the specific gravity of solids depend on the principle discovered by Archimedes, that when a solid is immersed in water, it loses in weight an amount equal to the volume of water it displaces. The solid whose specific gravity is to be taken—assuming it to be insoluble in water—is well cleansed and freed from adhering moisture, then accurately weighed (denote this weight by x); then, by means of a horse-hair, silk thread, or fine platinum wire, it is suspended Fig. 46. Fig. 47. Hydrostatic Balance. Immersion of Solid. from one arm or pan of a balance, so that it is entirely sub- merged, and does not come in contact with the sides of the vessel holding the water (Fig. 47); its weight is then noted (denote by i/). A thermometer placed in the water indicates the tempera- ture (t). The specific gravity is then found by the rule (1):— “ Divide the tveight of the body in air by its loss of weight in water: the quotient will be the specific gravity.” That is, the specific gravity at the temperature t° is equal to 36 HANDBOOK OF PHARMACY. Example:— A piece of metal weighs in air, 40 grammes. Immersed in distilled water (60° F.) it weighs, . . 35 “ Loss of weight in water, 5 “ Then its specific gravity at 60° F., ..... = —---— = - ~ = 8.00. 40 — 35 5 This determination may be carried out more expeditiously by means of the hydrostatic balance (Fig. 46), which consists of two counterbalanced pans (hung at unequal heights); under the shorter one is placed a hook, from which the body is suspended. The latter is first weighed alone in the usual manner in air, then immersed in the vessel of water at the proper temperature; this causes the short pan to become lighter. Weights are then added until the balance gains its equilibrium; the weight thus placed in the short pan to accomplish this, constitutes the loss of weight in water. Displacement in Graduated Cylinder.—Into a cylinder graduated in cubic centimeters, or better, fractions thereof, water of the proper temperature is poured, until it reaches some definite mark on the graduated scale. The body previously weighed in air is now dropped into it, which causes the level of water to rise, and thereby shows the exact bulk of water displaced by the solid; this is equivalent to the loss of weight in water, since each cubic centimeter of water weighs one gramme. Then apply the rule:— Example:— A piece of metal weighs, 3.0 grammes. The bulk of water displaced, 1.5 cubic centimeters = 1.5 Gm. 3 0 The specific gravity will be = 2.0. Separation of Different Insoluble Bodies by Means of their Specific Gravities.—This method is employed mainly by mineralogists for separating various minerals from crushed rock ore. Dense liquids of known specific gravity are employed, in which these solids will just float. For substances lighter than water, dilute spirits may be used; for those heavier than water, solutions of common salt, solution of mercuric nitrate, solution of potassio-mercuric iodide (3.196 sp. gr.), ethylene bromide, etc., are used. All that is neces- sary, is that the density of the liquid be known, it being pre- sumed that the solid is not acted upon by the fluid. Specific Gravity of Insoluble Powders Heavier than Water.—Weigh off a portion of the powder, then introduce it into a counterpoised specific gravity bottle, which is so con- structed as to hold a known weight (1000 grains, etc.,) of dis- tilled water. Some water is poured in, and the contents gently rotated so as to remove any air bubbles that may adhere to the powder, then the flask is filled to the mark indicating its capa- city, and weighed. From the weight of the powder in the air, SPECIFIC GE A CITY. DENSITY. 37 plus the known weight of water which the bottle will hold, sub- tract the weight obtained in the second operation. The remainder represents the weight of water displaced by the powder. Then apply the rule:— Example:— 10 grammes of a powder is taken, poured into a counterpoised specific gravity bottle of 100 grammes’ capacity, which, when filled with water, weighs 108.8 Gm. 10 grammes + 100 grammes = 110.0 grammes. Weight of flask containing water and powder, = 108.8 “ Difference or weight of water displaced 1.2 “ Therefore, the weight in air (10 grammes) divided by the loss of weight in water (1.2 grammes), gives us 8.33 as the specific gravity of the powder. This method may be employed for solids, provided they are in pieces of such size as to admit of being placed in the specific gravity bottle. Specific Gravity of Solids Insoluble in, but Lighter than Water.*—Inasmuch as such a body floats on the surface of water, it necessarily follows, that we must attach it to a heavier body in order to secure the submersion of both. The loss of weight of the heavy body in water must be known, and when this is deducted from the loss of weight of both together, the difference will give the amount of water displaced by the light body alone. The light body is first weighed in air, it is then at- tached to a sinker (a piece of lead or iron) and again weighed; then both are suspended by a thread under the surface of dis- tilled water and their combined weight in water noted. The light body is detached and the weight of the sinker alone in water is ascertained. The loss of weight of the sinker alone in water is now deducted from the loss of both; this gives the loss of weight of the light body; then apply the rule.— Example:— A piece of brass weighs 5 grammes ; in water it weighs 4.4 grammes. A piece of wax weighs in air 13.37 grammes ; when attached to sinker, both weigh 3.88 grammes in water :— Weight of brass in air, . 5.00 grammes. Wax weighs in air, . . 13 37 grammes. “ “ “ “ water, 4.40 “ Brass “ “ “ . . 5.00 “ Loss of weight of brass in Sum of both, 18.37 “ water, 0.60 “ Both weigh in water, . 3.88 “ Both lose in water, . . 14.49 “ Loss of weight of both in water, 14.49 grammes. “ “ “ “ brass “ “ 0.60 “ “ “ “ “ wax alone, 13.89 “ weight of wax in air, 13.37 , Then - == = 0.962 specific gravity. loss of weight in water, 13.89 *The method of Symons (Phar. Jour. Trans., (3) xix, 206) may be employed. He fixes an in- verted funnel under one scale-pan, attaches a ten-gramme weight to it, and restores equilibrium. The previously weighed light solid is now held under water until air-bubbles are removed, and then placed under the funnel; the weight lost will represent the volume of the solid, or, in other words, will be the weight of a volume of water equal to the volume of the solid. 38 HANDBOOK OF PHARMACY. Specific Gravity of Solids Soluble in Water.—We pro- ceed exactly in the same manner as in the case of solids heavier but insoluble in water; but instead of water, we employ some liquid in which the body is not soluble. The liquids usually selected for this purpose are the oils of turpentine, olive, or almond. The specific gravity of the body having been obtained just as if water had been used, the result is multiplied by the known specific gravity of the oil employed. Example:— A crystal of citric acid weighs 10.0 grammes ; when immersed in Oil of Turpen- tine it weighed 4.8 grammes. Then :— The weight of the citric acid in air was, 10.0 grammes. “ “ “ “ “ oil of turpentine, . . . 4.8 “ Loss of weight in turpentine, 5.2 “ then dividing 10 hy 5.2 we get 1.92, the specific gravity of citric acid referred to oil of turpentine as standard, and multiplying this by 0.870, the specific gravity of oil of turpentine, we obtain 1.67 the specific gravity of the sample of citric acid, as referred to the usual standard, viz.: water. SPECIFIC GRAVITY OF LIQUIDS.-METHODS OF DETERMINING. (a) By means of the Pycnometer. (&) “ “ “ Hydrometer. (c) “ “ “ Specific Gravity Balance. (d) “ “ “ Sprengel’s Specific Gravity Tube. (e) “ “ “ Weight of given Volumes. (/) “ “ “ Lovi’s Specific Gravity Beads. (a) Determination of the Specific Gravity of Liquids by means of the Pycnometer.—For ascertaining the specific gravity of a fluid we employ the Pycnometer or specific gravity bottle, which, in its simplest form, is a small, light glass flask with a long and narrow neck.* The flask, after being counter- balanced, is filled with any convenient amount of distilled water at the proper temperature, the height of the fluid marked, and its weight noted. These flasks are usually constructed to hold 25, 50, or 100 grammes, or 1000 grains of distilled water at 15.5° C. (60° F.). The bottle when emptied and dried, is filled to the mark with the liquid to be tested and weighed. The weight found bears a simple ratio to the specific gravity. Thus if the flask holds 100 grammes of distilled water at 15.5° C., when filled with ether, it will hold 72.5 grammes, and with glycerin, 125 grammes. The specific gravi- ties of these two liquids are, then, 0.725 and 1.250, respectively, Fig. 48. Pycnometer. * Some of the older forms are quite short, as shown in figure 48. SPECIFIC GE A CITY. DENSITY. 39 obtained by dividing 72.5 and 125 by 100. Any ordinary vial may be converted into a specific gravity bottle, by selecting one as light as possible, which will hold either 50 or 100 grammes of water. The distilled water is accurately weighed into the vial, and the exact height of the water is indicated by a mark (scratch) on the neck. An exact counterpoise is prepared for the empty flask. When used, the flask is filled to the mark with the liquid at the proper temperature, and its weight is divided by 50 or 100 as the case may be. Supposing, for example, that, when filled to the 50 cubic centimeter mark with sulphuric acid, it weighed 92.15 grammes, then = 1.843, the specific gravity of the acid.* Pycnometers are either sold with a brass counterpoise or their exact weight is etched upon the bottle. Before the pycnometer is used, it should be first well rinsed with water, then with alcohol, and dried. After bringing the liquid to the proper temperature, by placing the vessel containing it in a bath of known tem- perature, the flask is filled nearly to the top of the neck, and the stopper is in- serted, care being taken to avoid the retention of air bubbles. The super- fluous fluid displaced by the stopper is then removed, and the flask then wiped perfectly dry and clean, and weighed. This form of specific gravity bottle has the objection that the temperature cannot be carefully observed, which renders it unsuitable for very accurate work. A better form of specific gravity bottle (Fig. 49) is that in which the stopper consists of a thermometer. The liquid is introduced in the side tubulure until it reaches the mark at m. Care should be taken that no air bubbles be allowed to collect around the neck at h. Fig. 49. Pycnometer with Thermometer. * It should be borne in mind that the temperature of observation should always be stated, and also that at which the standard was determined. To illustrate the importance of this Dr. Wright (Jour. Soc. Chem. Ind., XI, -298) cites the following“ A sample of oil at 20° C. is stated by one observer to have the specific gravity of 0.92475 referred to water at 4° C., another the specific gravity of 0.92560 referred to water at 15.5° C., and the third the specific gravity of 0.92635 referred to water at 20° C. from appearance, these figures do not seem concordant, but if we remember that when reduced to “ weight per cubic centimeter,” it will be seen that they are identical. Taking the specific gravity of water at 4° C. as 1.000, then at 15.5° C. it is 0.99908, and at 20° C. it is 0.99827, hence “0.92475 X 1.0000 = 0.92475. 0.92560 X 0.99908 = 0.92475. 0.92635 X 0.99827 = 0.92475.” For the various corrections to secure accuracy in taking specific gravities, see the above-cited reference. 40 HANDBOOK OF PHARMACY. Another form is that devised by Dr. Squibb (Fig. 50), in which the neck of the bottle is lengthened, so that it will permit the bottle to hold the volume of water at any temperature between 4° C. and 25° C., thus adapting it to all standards in use. The capacity and tare is indicated on each bottle. A leaden collar is placed over the neck to keep it in position in the bath in which it is placed. Fig. 50. Squibb’s Pycnometer. (6) Determination of the Specific Gravity of Liquids by means of the Hydrometer or Areometer.—This instrument depends for its use on the fact that, when a solid is immersed in a liquid specifically heavier, it will sink until it reaches a point where the weight of the liquid displaced is equal to the weight of SPECIFIC GRA VITY. DENSITY. 41 the floating body. Hydrometers are long glass tubes with two bulbs blown at one end. The lower (smaller) bulb is weighted with sufficient mercury or shot to cause the tube to float upright, the upper (larger) bulb is to impart buoyancy. Hydrometers are divided into two classes, the “ Weighing Hy- drometers ” and “ Scale Hydrometers.” The weighing areometer or hydro- meter OF CONSTANT IMMERSION BUT VARIA- BLE weight is so called because it is always immersed to the same mark, but requires different weights to effect this. The first of these was constructed by Fahrenheit; the same principle, however, is followed in Figs. 51, 52. Fig. 53. Nicholson’s Hydrometer. that of Nicholson’s hydrometer (Fig. 53), which consists of a hollow metal cylinder b with a cone c, weighted so that the cylinder may float vertical. At the top is a stem terminated by a pan, in which the substance whose specific gravity is to be determined is placed. When floated, the apparatus stands partly out of the liquid, hence, the first step would be to ascertain what weight is necessary to cause it to sink to the standard point o; let this weight be 100 grammes. Let us assume that we desire to as- certain the specific gravity of a piece of metal; the weights are removed from the pan, and replaced by the sample; weights are now added, until the instrument again sinks to o; in order to accomplish this, we have added 44 grammes; then the actual Hydrometers. a. Weighing Hydrometer. b. Scale Hydrometer. 42 HANDBOOK OF PHARMACY. weight of the piece of metal would be the difference between 100 grammes and 44 grammes, which is 56 grammes. Thus far, we have ascertained the actual weight of the metal; it is next neces- sary for us to ascertain its loss in water, or the weight of an equal volume of water. With this object in view, we place it in the lower cone c, at m; the instrument does not sink to o, for the metal, by immersion, has lost a part of its weight equal to that of the water displaced. Weights are added to the upper pan until the hydrometer sinks again to o; this being 27.5 grammes, is the weight of water displaced; then on dividing its actual weight (in air), by its loss in water V6y we obtain 2.03 as its specific gravity. Bodies lighter than water are placed in the covered cup, thus securing immersion. Rousseau's Densimeter.—This instrument (Fig. 54) is of use in ascertaining the specific gravity of liquids where only a small amount is available. The cup above is gradu- ated to hold 1 cubic centimeter. When empty, the instrument sinks in distilled water to the point b; when the cup is filled with distilled water (1 Cc.), the point to which it sinks is marked as 20; then, the interval between 0 and 20, on the stem, is divided into 20 equal parts, the graduation being continued to the top, each division representing 0.05 gramme. Example: Supposing that the cup is filled with oil of neroli, the densimeter will sink to the mark 17.5; hence the specific gravity of the oil of neroli would be 0.05 X 17.5 = 0.875. Neither of these instruments gives such accurate results as the specific gravity bottle. Scale Areometers or Hydrometers of Variable Immersion, but Constant Weight.— These are divided into different classes, according to their uses, being designated as Alcoholometers, Salimeters, Lactometers, Acido- meters, Saccharometers, Urinometers, etc. There are two systems of these; in the one, the specific gravity is indicated directly on the scale; in the other (that of BaumS, Cartier, Twaddell, Tralles, etc.) an empirical scale is employed which may be reduced to specific gravity by referring to tables constructed for this pur- pose. The most important of these instruments is that of Baum6, under which name two distinct instruments are used. One of these is used for determining the densities of liquids heavier than water, such as acids, alkaline solutions, syrups, glycerin, milk, etc.; the other for liquids lighter than water, as alcohols, ethers, most volatile oils, etc. In the former (Fig. 55), for liquids heavier than water, the zero mark is obtained by placing it in distilled water; another mark is made at the place to which it sinks by floating it in a 15 per cent, solution of common salt. Fig. 54. Rousseau’s Densimeter. SPECIFIC GRA CITY. DENSITY. 43 The space between these two marks is then divided into 15 equal parts, the graduation being continued to 60° below. For liquids lighter than water (Fig. 56), zero is the point designated to which it sinks when placed in a 10 per cent, salt solution, and 10° the point to which it sinks in distilled water; the distance between these is divided into 10 equal parts, the scale being extended up to 60°.* TwaddelVs areometer, for liquids heavier than water, is common in England. It is so graduated that the reading multiplied by 5 and added to 1000 gives the specific gravity : thus, 15° Twaddell is equal to specific gravity 1.075. Alcoholometers are hydrometers for ascertaining the percentage strength of alco- holic liquids. They are often so constructed as to combine a thermometer, the mercury in the lower bulb answering for the bulb of the thermometer. The Tralles hydrometer is an alcoholometer having a centesimal scale, each division cor- responding to a certain per cent, of absolute alcohol, by volume. Tables giving the equivalents may be found in the Dispensatories and other works of reference. Sikes’ hydrometer is used in England by the Excise Revenue officers for ascertaining the percentage strength of spirituous liquors. The instrument is of brass, the stem being gradu- ated from 0 to 10, and a set of nine weights to place beneath the bulb. On noting the temperature, the weight employed, and Fig. 55. Fig. 56. Baumd’s Hydrometers. * TABLES OF DEGREE BAUME. 15° C. For Liquids Heavier than Water. Baumi. Specific Gravity. 0°, . . ... 1.000 5°, . . . 1.036 10°, . . . . . 1.075 15°, . . . . 1.116 20°, . . 1.161 25°, . . . . . 1.210 30°, . . . 1.261 35°, . . . . . 1.321 40°, . . . 1.384 45°, . . . . . 1.454 50°, . . . . . 1.532 60°, . . . . . . 1.715 65°, . . . . . . 1.823 70°, . . . . . . 1.946 144.3 Sp-Gr'- 144.3- n. For Liquids Lighter than Water. Baumi. Specific Gravity. 10°, . . . . . . 1.000 15°, . . . . . .0.966 20°, . . . . . . 0.935 25°, . . . . . . 0.905 30°, . . . . . 0.878 35°, . . . . . . 0.852 40°, . . . . . . 0.827 45°, . . . . . . 0.804 50°, . . . . . . 0.783 55°, . . . . . . 0.762 60°, . . 144.3 . . . . 0.742 sp- 134 3 + n n = degree of BaumA Such scales are unsatisfactory, as their equivalents vary in different instruments and different countries. 44 HANDBOOK OF PHARMACY. the point to which it sinks on the stem, and referring to a series of tables belonging to the instrument, the specific gravity is ob- tained. Saccharometers are intended to show the specific gravity of sugar solu- tions; the scale is so arranged as to indicate directly the percentage of sugar. The Elaeometer is an instrument for ascertaining the specific gravity of fixed oils. The Lactometer is employed to as- certain the specific gravity of milk, the scale indicating the percentage of added water. The Urinometer is a small areometer with its scale limited to the specific gravity of urine, usually from 1.000 to 1.060. Most of these instruments are usually very faulty and inaccurate and should never be relied upon un- less obtained from a reliable source, or verified. A form offered by Dr. Squibb (Fig. 57), is furnished with a special cylinder having its sides in- dented so as prevent the instrument from remaining in contact with the sides of the cylinder. Should this happen, the friction and cohesion with the sharp edge of one of these indenta- tions will be reduced to a minimum. In using an areometer it must be ob- served that the instrument should float freely, and should not adhere to the sides of the jar, otherwise the co- hesion between the instrument and sides of the jar would prevent a free movement up and down in the liquid, and thus give rise to false readings. The bulb of an areometer is best shaped after that of a double cone, as in Fig. 57, so that there is but a single point which may come in contact with the side of the jar, thus reducing the friction and cohe- sion to a minimum. Fig. 57. Urinometer with Cylinder. (Squibb.) SPECIFIC GE A VITY. DENSITY. 45 (c) Determination of Specific Gravity by Means of the Specific Gravity Balance.— Westphal Specific Gravity Balance.— The application of this depends upon the principle that any selected body, when immersed in different liquids, loses exactly the weight of its own volume of that liquid. If the same body be immersed in different liquids, it will be seen that its loss in weight will be in proportion to their specific gravities. The small thermometer Fig. 58. Westphal Specific Gravity Balance. suspended from the arm at K is held in equilibrium by a counter- balancing weight at J. When placed in a liquid, the arm HK rises; riders are then placed upon the beam, in the notches indi- cated, until equilibrium is restored. The riders L or Li are equal in weight to the loss sustained by the thermometer in dis- tilled water (4° C.), the rider M = tV, the rider N = and O — nW °f the weight of LorLp When L or Li is placed on the hook at K it indicates the specific gravity of 1.000; when the 46 HANDBOOK OF PHARMACY. other L is placed at 3 it denotes 0.3. Hence, when one of these riders (L or Lx) is placed at K, and the other at 3, and equili- brium is thus restored, the liquid has the specific gravity 1.300. The rider M the second, and N the third, and O furnishes the fourth decimal place. Fig. 59 illustrates the use of the apparatus sufficiently. Fig. 59. Beam of Westphal Balance, showing Position of Weights. Fig. 60 illustrates a simpler form, known as Mohr’s Specific Gravity Balance ; it will be seen from this, that any balance can be used for this purpose by detaching a pan and suspending a short thermometer in its stead by means of a fine platinum wire, then counterpoising both arms by adding weights to the side requiring it. The further operation is the same as that with the Westphal balance. Jolly’s Spiral Balance.—This consists of a spiral vertical spring suspended from an upright beam ;■ on the side of this 47 SPECIFIC GRA CITY. DENSITY. beam facing the spiral, is a long mirror which is graduated Fig. 60. Mohr’s Specific Gravity Balance. Fig. 61. into millimeters. The spiral supports two scale pans, one some distance above the other. Just above the upper pan (at b) is a glass bead which serves as an indicator. To take the specific gravity of a solid, the lower pan (d) is immersed in water, the solid placed in the upper pan (c), and the division on the index on the mirror opposite the bead is noted. The solid is removed and weights added until the bead is opposite the same scale division as before. This constitutes the weight of the solid. The solid is then placed in the lower pan and the weights adjusted until the bead again comes to the same number; this constitutes the weight of the volume of water displaced by the solid; then apply rule 1 (page 35). (d) Sprengel Specific Gravity Tube.— This instrument is well adapted for small quantities of fluids and is extremely accurate. It consists of a U-shaped tube terminating in two capillary tubes bent in opposite direc- tions. The liquid to be examined is aspi- rated into the tube until the latter is filled; the tube is then placed in a beaker of water having the desired temperature, the two arms resting on the edge of the beaker. When the Jolly’s Spiral Balance. 48 HANDBOOK OF PHARMACY. temperature of the contained liquid is constant (shown by the cessation of movement of the liquid in the capillary tube), the excess of fluid is removed by means of filter paper from the tip a until the liquid in the other capillary reaches the mark m; the tube and contents are then weighed, and the ca- pacity of the tube in distilled water being known, the specific gravity is obtained as usual. (e) Determination of Specific Gravity by Weighing given Volumes of Solu- tions.—A cylinder or graduate is counter- balanced, and the liquid to be examined is poured in to any definite measure and weighed. This weight is then divided by the weight of a like volume of water at the same temperature. Thus, if we were to weigh a fluidounce of a liquid, we would then divide that weight by 455.7 (the weight of one fluidounce of distilled water at 15.5° C.). Should we have measured off 10 cubic centi- meters of the fluid, we then divide its weight in grammes by 10 (the weight of 10 Cc. of distilled water). (/) Lovi’s Specific Gravity Beads.—These are small hollow globes of glass, having specific gravity figures etched on their Fig. 62. Sprengel Specific Gravity Tube. Fig. 64. Fig. 63. Specific Gravity of Solid Fats, by means of the Westphal Balance. Specific Gravity of Solid Fats, by means of Areometer. SPECIFIC GPA VITY. DENSITY. 49 surfaces. When thrown into a fluid they will rise and float to the surface if lighter than the fluid, or sink to the bottom if heavier; but when any of them remain indifferently suspended at any level, then the liquid has the specific gravity engraved on the beads, if these are correct. These are of special use in the evaporation of liquids to attain certain densities. They will show a difference in specific gravity of 0.001. They are sometimes used in the distillation of ether, the operation being carried on until one of them of specific gravity 0.735 begins to float. Determination of the Specific Gravity of Fats and Oils (solid at normal temperature).—Fig. 63 illustrates the appa- ratus of Benedikt, in which the fat is placed in the tube D, the temperature of which is regulated by the paraffin bath C, which in turn is heated by the water bath B. The specific gravity is ascertained as usual with the Westphal’s balance, the temperature being taken into consideration. Fig. 64 illustrates another form, in which an areometer is floated in the melted fat. SPECIFIC VOLUME * As applied in pharmacy, specific volume is the volume of a certain liquid compared with the volume of an equal weight of another, which is selected as standard. The standard for com- parison is distilled water, usually at 15.5° C. (60° F.). As specific gravity is obtained by the comparison of the weight of a given volume of a liquid or solid with an equal volume of water (as unity), so is specific volume obtained by the comparison of the volume of a given weight of a liquid body with an equal volume of water. Specific volume, therefore, is simply the reverse of specific gravity. Specific volume is the quotient obtained by dividing unity by the specific gravity; that is, sFecific°GtfaVity = Specific Volume. We find that a pound of glycerin measures less, while a pound of ether measures more, than a pound of water; a kilogramme of mercury will occupy less bulk, while the same weight of benzin will occupy more than a kilogramme (1000 Cc.) of water. The knowledge of the specific volume of a fluid will then enable us to ascertain the bulk occupied by a given weight of it. Since the capacity of all graduated or gauged vessels is based on the volume of water they will hold, the specific volume factor will express at a glance the weight capacity of the container. Water at 15.5° C. being unity (1.000), we thus find the specific volume of glycerin to be = 0.8; that of ether, = 1.38; that of chloroform, <,r = 0.674. Therefore, one fluid pint of water, about f of a pint of glycerin, about of a pint of ether, ♦This term should not be confounded with the term “specific volume” as applied to chemical physics, which is also defined as “ atomic volume,” or “ molecular volume.” 50 HANDBOOK OF PHARMACY. and about f of a pint of chloroform will all be of the same weight. The actual volume occupied by a given weight of a liquid is found by the following rule:— Multiply the volume of an equal weight of water by the specific volume of the liquid. Example.—How many cubic centimeters will one kilogramme of chloroform measure? A kilogramme of water weighs 1000 grammes ; then, 1000 X 0.674 = 674 cubic centimeters of chloroform. Example.—How many lluidounces will 100 av. ounces of glycerin measure? 100 av. ounces of water measure 96.01 fluidouuees ; then, 96.01 X 0.80 (sp. vol. of glycerin) = 76.8 + fluidounces of glycerin. PRACTICAL EXERCISES IN SPECIFIC GRAVITY AND SPECIFIC VOLUME. Example.—If 10 cubic centimeters of a liquid weigh 15 grammes, what is its 15 specific gravity? 10 Cc. of distilled water weigh 10 Gm., hence = 1.50 is the specific gravity. Example.—If one fluidounce of a liquid weighs 569.63 grains, what is its specific 569.63 gravity ? One fluidounce of distilled water weighs 455.7 grains, hence 455'7" = 1-25 is the specific gravity. Example.—What is the weight of a pint of glycerin? We know that a pint of distilled water weighs 7291.11 grains, and the specific gravity of glycerin is 1.25 ; hence we multiply 7291.11 by 1.25, which gives us 9113.8 + grains. Example.—Liquor Ferri Chloridi (sp. gr. 1.387) contains 37.8 per cent, of anhy- drous salt; how much of this salt is in each 100 cubic centimeters of the solution ? The weight of 100 Cc. of water is 100 Gm., this multiplied by 1.387 gives the weight of 100 Cc. of the solution, which is 138.7 Gm. ; now, 37.8 per cent, of this weight would be 52.42 -]- Gm. Example.—What will be the capacity of a flask which will hold 7 av. pounds of glycerin U. S. P. ? Seven avoirdupois pounds of distilled water weigh 49,000 grains ; this, divided by 455.7 gives 107.52 + fluidounces, the bulk occupied by 7 avoirdupois pounds of water ; since the specific volume of glycerin is 0.80, we have 107.36 X 0.80 — 86.01 + fluidounces (5.37 + pints), which will be the capacity necessary to hold this weight of glycerin. Example.—An apothecary returned to his dealer 5 pints of oleic acid (sp. gr. 0.900), valued at 40 cents per pound (av.), and received in return 117 cubic centi- meters of mercury (sp. gr. 13.5), valued at 54 cents a pound (av.) : did the dealer gain or lose by the transaction ? 5 pints of water weigh 5.205 av. pounds ; then, if the specific gravity of the oleic acid be 0 900, the weight of 5 pints of it would be 5.205 X 0.900 = 4.684 av. pounds. Its value would then be $0.40 X 4.684 = $1.87 + . 117 Cc. of water weighs 117 Gm., and if the specific gravity of mercury is 13.5, it would weigh 117 X 13.5 = 1579.5 Gm or 3.48 + av. pounds. The value will be $0.54 X 3.48 — $1.87 -j-. Hence, there will be neither loss nor gain. Example.—A piece of metal weighs 100 grammes ; its specific gravity is 7.6. When immersed in syrup it loses 16.9 grammes weight. What is the specific gravity of the syrup? We use the following proportion : as the weight of the body in air is to its specific gravity, so is its loss of weight immersed in the liquid, to the specific gravity of that liquid. That is, as 100 : 7.6 :: 16.9 : x. x = 1.28, sp. gr. of the syrup. SPECIFIC VOLUME. 51 Example.—A piece of mineral weighs 1 av. ounce ; when placed in a graduate containing 1 fluidounce of water, the volume of water was increased to 9 flui- drachms. What is the specific gravity of the mineral ? The volume of water displaced is 1 fluidrachm, which weighs 56.96 grains, then apply rule (page 35), = 7.68 the specific gravity of the mineral. TABLE OF SPECIFIC GRAVITIES, U. S. P. Temperature, 15° C., 59° F., unless otherwise specified. Acidum Acetieum,1.048 Acidum Acetieum Dilutum,1.008 Acidum Acetieum Glaciate,1.058 Acidum Hydrobromicum Dilutum, .... 1.077 Acidum Hydrochloricum1.163 Acidum Hydrochloricum Dilutum, .... 1.050 Acidum Hypophosphorosum Dilutum, . . 1.046 Acidum Lacticum, about,1.213 Acidum Nitricum, about,1.414 Acidum Nitricum Dilutum, about, .... 1.057 Acidum Oleicum, about,0.900 Acidum Phosphoricum, not below, . . . 1.710 Acidum Phosphoricum Dilutum, about, . . 1.057 Acidum Sulphuricum, not below, .... 1.835 Acidum Sulphuricum Aromaticum, about, 0.939 Acidum Sulphuricum Dilutum, about, . . .1.070 Acidum Sulphurosum, not less than, . . . 1.035 Adeps,0.932 .Ether, 0.725 to .728 .Ether Aceticus, 0.893 to 0.895 Alcohol, about,0.820 Alcohol Absolutum, not higher than, . . .0.797 Alcohol Deodoratum, about,0.816 Alcohol Dilutum, at 15° C., about0.936 Alcohol Dilutum, at 15.6° C., about, .... 0.937 Alcohol Dilutum, at 25° C., about, .... 0.930 Amyl Nitris, 0.870 to 0.880 Aqua Ammoni®,0.960 Aqua Ammoni® Fortior, . . 0.901 Aqua Hydrogenii Dioxidi, about, . 1.006 to 1.012 Balsamum Peruvianum,1.135 to 1.150 Benzinum, 0.670 to 0.675 Bromum,2.990 Camphora,0.995 Carbonei Disulphidum, 1.268 to 1.269 Cera Alba, 0.965 to 0.075 Cera Flava, 0.955 to 0.967 Cetaceum, about,0.945 Chloroformum, not below, at 15° C., . . . 1.490 Chloroformum, not below, at 25° C., . . . .1.473 Copaiba, 0.940 to 0.990 Creosotum, not below,1.070 Eucalyptol,0.930 Fel Bovis,1.018 to 1.028 Glycerinum, not less than,1.250 Hydrargyrum, 13.5584 lodoformum,2.000 lodum, at 17° C.,4.948 Liquor Ferri Acetatis, about,1.160 Liquor Ferri Chloridi, about,1.387 Liquor Ferri Citratis, about,1.250 Liquor Ferri Nitratis, about,1.050 Liquor Ferri Subsulphatis, about,1.550 Liquor Ferri Tersulphatis, about,1.320 Liquor Hydrargyri Nitratis, about, .... 2.100 Liquor Plumbi Subacetatis, about, .... 1.195 Liquor Potass®, about,1.036 Liquor Sod®, about1.059 Liquor Sod® Chlorat®, about,1.052 Liquor Sodii Silicatis, 1.300 to 1.400 Liquor Zinci Chloridi, about,1.535 Mel1.375 Methyl Salicylas,1.183 to 1.185 Oleum Adipis0.910 to 0.920 Oleum AEthereum,0.910 Oleum Amygdal® Amar® 1.060 to 1.070 Oleum Amygdal® Expressum, . . 0.915 to 0.920 Oleum Anisi, about (17° C.), . . . 0.980 to 0.990 Oleum Aurantii Corticis, about,0.850 Oleum Aurantii Florum, 0.875 to 0.890 Oleum Bergamott®, 0.880 to 0.885 Oleum Cadinum, about,0.990 Oleum Cajuputi, 0.922 to 0.929 Oleum Cari0.910 to 0.920 Oleum Caryophylli,1.060 to 1.067 Oleum Chenopodii, about0.970 Oleum Cinnamomi, 1.055 to 1.065 Oleum Copaib®, 0.890 to 0.910 Oleum Coriandri, 0.870 to 0.885 Oleum Cubeb®, about,0.920 Oleum Erigerontis, about,0.850 Oleum Eucalypti,0.915 to 0.925 Oleum Foeniculi, not less than,0.960 Oleum Gaultheri®,1.175 to 1.185 Oleum Gossypii Seminis, 0.920 to 0.930 Oleum Hedeom®, 0.930 to 0.940 Oleum Juniperi, 0.850 to 0.890 Oleum Lavandulae Florum, .... 0.885 to 0.897 Oleum Limonis, 0.858 to 0.859 Oleum Lini, . 0.930 to 0.940 Oleum Menth® Piperit®, 0.900 to 0.920 Oleum Menthae Viridis, 0.930 to 0.940 Oleum Morrhuae, 0.920 to 0.925 Oleum Myrciae, 0.975 to 0.990 Oleum Myristieae, 0.870 to 0.900 Oleum Oliv®, 0.915 to 0.918 Oleum Picis Liquid®, about,0.970 Oleum Pimentae, 1.045 to 1.055 Oleum Ricini, 0.950 to 0.970 Oleum Rosae, 0.886 to 0.880 Oleum Rosmarini, . 0.895 to 0.915 Oleum Sabinae,0.910 to 0.940 Oleum Santali, 0.970 to 0.978 Oleum Sassafras, 1.070 to 1.090 Oleum Sesami0.919 to 0.923 Oleum Sinapis Volatile,1.018 to 1.029 Oleum Terebinthin®, 0.855 to 0.870 Oleum Terebinthin® Rectificatum, 0.855 to 0.865 Oleum Theobromatis, 0.970 to 0.980 Oleum Thymi, 0.900 to 0.930 Oleum Tiglii, 0.940 to 0.960 Petrolatum Liquiduni, .... 0.875 to 0.945 PetrolatumMolleat 60° C., (140°F.), 0.820 to 0.840 Petrolatum Spissum, at 60° C. (140° F.), 0.820 to 8.50 Phosphorus, at 10° C. (50° F.), 1.830 Resina, 1.070 to 1.080 Spiritus AEtheris Nitrosi, about,820 Spiritus Ammoni®, about,0.810 Spiritus Ammoni® Aromaticus, 0.905 Spiritus Frumenti,0.917 to 0.930 Spiritus Glonoini, 0.826 to 0.832 Spiritus Vini Gallici, 0.925 to 0.941 Syrupus, about,1.317 Syrupus Acidi Hydriodici, about1.313 Terebenum, about,0.862 Thymol (as solid)1.069 Tinctura Ferri Chloridi, about,0.960 Vinum Album, at 15 6° C., not less than, . 0.990 Vinum Album, not more than,1.010 Vinum Rubrum, at 15.6° C., not less than, . 0.989 Vinum Rubrum, not more than,1.010 Zincum, cast 6.900, rolled,7.200 CHAPTER III. HEAT. ITS VARIOUS APPLICATIONS IN PHARMACY. Combustion is chemical combination attended with evolution of light and heat. A flame is a stream of gas or vapor raised to the temperature of ignition. Its illuminating and heating power varies with the nature of the products formed; the presence of a solid body in the flame increases the illuminating power. The flame of hydrogen or alcohol is pale, or almost colorless, because Fig. 66. Fig. 65. Alcohol Lamp. Berzelius’ Alcohol Lamp for High Temperatures. it only contains gaseous products of combustion. The flames of candles, lamps, and coal gas possess high illuminating power, because the high temperature produced decomposes certain of the gases with the production of carbon, which not being entirely consumed, becomes incandescent in the flame. Coal gas, when burnt so that it may become mixed with an adequate supply of air, as in the Bunsen burner, gives a flame which is almost devoid of luminosity. For technical purposes the valuation of different fuels is important. The comparative value of fuel is ascertained by estimating the number of heat units (calorics) disengaged during combustion. By caloric is meant the number of heat units necessary to raise one gramme of water from 0° to 1° C. 52 HEAT. 53 It may also be expressed by the quantity of water warmed one degree by one kilogramme of the material; for example:— 1 kilo of hard wood heats 3600 kilos of water from 0° to 1° C. 1 “ “ bituminous coal “ 6000 “ “ “ “ “ “ “ Then the value of wood as a heat-producer, compared with coal, is as 3600 is to 6000, or 3 to 5; that is, 3 parts of coal will give as much heat as 5 parts of wood. Compared as to their heating or evaporating power we have :— 1 kilo of Hydrogen evaporates 53 kilos of water. 1 “ “ Illuminating Gas “ 18 “ “ “ 1 “ “ Coal Oil “ 11.8 “ “ “ 1 “ “ Alcohol “ 11.2 “ “ “ 1 “ “ Coal “ 9.0 “ “ “ 1 “ “ Wood “ 5.5 “ “ “ For detailed explanations of the value and uses of different fuels, with the arrangement of furnaces, ranges, etc., the reader must he referred to the text-books on Technical Chemistry. The modern apothecary employs, as a source of heat, either alcohol, benzin, coal oil, illuminating gas, or steam. Owing to the high price of alcohol, this liquid is at present used for heating purposes, only where coal-gas is not accessible, or for some reason objection- able. For purposes where a lower degree of heat is needed, the simple form of the al- cohol lamp (Fig. 65) is employed; should it be desirable to have a more luminous flame, a small amount of oil of tur- pentine may be added. For a higher degree of heat we have heretofore employed the Berzelius lamp(Fig.66). This has, however, been greatly improved upon in the newer Bunsen lamp of Barthel (Fig. 67). This is a very practical and safe lamp, capable of producing a very high degree of heat, equal to that of the Bunsen gas burner. The burner consists of a thick metal tube supported on a foot and separated in the center into two parts (c, d). In the upper portion the flame is generated, and the heat therefrom vaporizes the alcohol in the lower portion. A uniform vapor is obtained by the interposition of a wire gauze (m), and the size of the flame is regulated by the screw (s, r) which governs the flow of vapor. The tube h conveys the alco- Fig. 67. Barthel Spirit Lamp. 54 HANDBOOK OF PHARMACY. hol to the flame and contains a sieve to filter the alcohol. The container is connected with the burner by a metallic tube. To heat one liter of water from a temperature of 15° C. to 100° C. (59° F. to 212° F.), Barthel’s alcohol Bunsen burner, after model B, requires seven and three-fourths minutes, with a con- sumption of 25 Gm. alcohol. This lamp may be used for benzin as well as alcohol. The market affords all forms of coal- oil stoves which are cheap and convenient, but they must be kept scrupulously clean, and the wicks well trimmed to avoid a smoky flame. The cheapness of illuminating gas has led to its Fig. 68. Fig. 69. Bunsen Burner in Sections. Bunsen Burner. general adoption for heating purposes. All the various forms of gas stoves depend on the principle of the Bunsen burner, the in- vention of which revolutionized our methods of heating, and made coal gas the most important of fuels. It was found by Bunsen in 1855, that the admixture of a certain portion of air with coal gas before combustion, caused it to burn with a non- luminous flame of high temperature. Figs. 68 and 69 illustrate the construction of a Bunsen burner. The gas enters at b, having its exit at a, where it becomes mixed with air which enters at the openings at the base of the burner. The volume of air can be regulated by the movable collar d; when this is closed, a lumi- HEAT. 55 nous, smoky flame is obtained. The cone g placed on /,/ is in- tended to prevent the flame from flickering, which is liable to be caused by slight draughts. On viewing a well regulated Bunsen Fig. 70. Bunsen Flames, x. Proper Flame, y. Flame Struck Back. flame (Fig. 70 x), it will be seen to consist of an inner colorless or pale-blue cone, which is a mixture of cold air and gas, and an Fig. 72. Fig. 71. Bunsen Burner (Seven-tubed). Erlenmeyer’s Burner. outer mantle, which is the burning mixture of gas and air. If the admission of air below is limited, the outer mantle and tip of the flame become smoky, with a loss in temperature. Should too much air and too little gas be admitted, the flame either be- 56 HANDBOOK OF PHARMACY. comes extinguished or strikes back and burns at the bottom of the lamp where the gas enters; the flame at the orifice then becomes Fig. 73. Fig. 74. Solid Flame Heating Burner. Fletcher Gas Stove. Fig. 75. Gas Stove. small (Fig. 70 y), is colored, and devoid of the blue cone; a peculiar, pungent odor (due to acetylene) is at once detected; the lamp be- comes very hot, causing the rub- ber tube to melt, and the escaping gas igniting gives rise to danger of fire. In such cases the gas should be at once turned off, and then readmitted in greater or lesser volume, as may be re- quired. For various operations where a higher degree of heat is required, we have such burners as are illustrated in Figs. 71, 72. For purposes of evapora- tion, the forms of stoves illus- trated in Figs. 73, 74 and 75 are employed. In many chemical operations we employ the “ blast lamp ” (Figs. 77, 78) which gives an intensely hot flame. The Instantaneous Water Heater. HEAT. 57 gas enters at a and the air is forced by means of a pair of bellows (foot blower) through b. The current of either may be regulated to produce any sized flame at will. Figs. 77, 78. Blast Lamp with Cross Section. A thermometer is an instrument which is employed to measure temperature. All bodies expand by the action of heat; gases being the most expansible, followed then by liquids and lastly by solids. Liquids are best suited for the construction of ther- mometers, for the expansion of solids is too small and that of gases too great. Mercury and alcohol are the liquids most generally employed, the former boiling at a very high tempera- ture (350° C.) and solidifying at - 29.4° C.; the latter does not solidify until it reaches -130.5° C. The mercury thermometer is employed most commonly. It consists of a capillary glass tube, at one extremity of which is blown a small bulb, either cylindrical, spherical or coiled. When it is to be filled, a rubber tube and small funnel is attached at the upper, open end, then a very pure mercury is poured into the funnel; on warming, the air is partially driven out, and on cooling, a portion of the mer- cury is forced down the capillary into the bulb, by the pressure of the atmosphere. This is repeated until the bulb is filled. Then the bulb of the thermometer is heated until the mercury rises and fills the entire tube; at this moment it is quickly sealed at the extremity. On cooling, the mercury contracts, leaving a vacuum above. The space above the mercury is often filled with nitrogen gas. This is done to avoid any oxidation of the MEASURING OF HEAT. 58 HANDBOOK OF PHARMACY. surface of the mercury, which would follow, should any air be present. After filling, the tubes are allowed to stand for some time (six months to two years), to allow for the complete con- traction of the glass, after which they are ready for graduation. For this purpose two fixed points are selected which can always be readily reproduced. Experiment has proven to us that ice always melts at the same temperature, no matter how great the amount of heat may be. Again, distilled water under the same Fig. 79. Fig. 80. Fig. 81. Thermometer (Opaque Milk-glass scale). Thermometer (Gradu- ated on Tube). Fahrenheit, Centigrade, Reaumur Thermometers. pressure and in a vessel of the same kind, always boils at the same temperature. Hence the first unit selected is the tempera- ture of melting ice, also designated as “ freezing point ” (viz. of water); and the second unit is the temperature of distilled water boiling in a metal vessel under normal atmospheric pressure (760 Mm). The space between the freezing and boiling points may be divided into any even number of parts. In the case of the Centigrade or Celsius thermometer, it is divided into 100 HEAT. 59 equal parts, the same scale of graduation being continued above the boiling point (100°) and below the freezing point, which is here marked (0°). The degrees below the zero point are indi- cated by a minus sign, and those above, by a plus sign before the figure. The latter, however, is omitted in practice. The three most popular thermometric scales are those of Fahrenheit, Reau- mur, and Celsius (Centigrade). The Fahrenheit thermometer, which is the household thermometer of England and America, was invented by Fahrenheit, a merchant of Dantzic, in 1709. The temperature of melting ice was marked as 32° and that of boiling distilled water as 212°. There are 180° between these two points, this being done in view of some old observations on the expansion of mercury. The Reaumur scale, the domestic thermometer of Germany, Austria, and some other European countries, selects the temperature of melting ice as the 0° point, and 80° as the boiling point of water, or more accurately stated as the temperature of the steam arising from boiling distilled water, under the standard pressure of 760 Mm. Between these points it is divided into 80 parts, from the observation, that there are 80 thermal units absorbed, in bringing one kilogramme of ice of the temperature 0°, to water of the temperature 0°. For scientific purposes, the Celsius (Centigrade) scale is the only one employed. The two fixed temperatures are that of melting ice, viz., 0°, and the temperature of steam which issues from distilled water boiling under the standard pressure of 760 millimeters, viz., 100°. Rules for converting Degrees of the Centigrade Thermometer into those of Fahrenheit, and vice versa*—(Rules for Reaumur are omitted):— 1. Given Celsius (C.) degrees, sought Fahrenheit (F.). + 32 = F. 5 2. Given Fahrenheit (F.) degrees, sought Celsius (C.). 5 (F. - 32) c 9 Examples.—Convert 100° C. into ° F. 9X1°? + 32 = F. ;900- 4- 32 = F. ; 180 + 32 = F212 = F. 5 5 or, F. = 9 x 100 + 32 = (9 X 20) + 32 = 180 + 32 = 212. 5 Convert 212° F. into ° C. 5 (212 - 32) c 5 X180 = c 5 y 20 — C . 100 C 9 ’9 ’ or, C 5 (212 — 32) 5 X 180 — 5 y 20 = 100 9 9 * Thermometric Tables, see Appendix. 60 HANDBOOK OF PH AB MACY. Of late years a number of improvements have been made in the manufacture of thermometers, particularly in those which are to be employed for estimating extremely high or low tem- peratures. A Jena laboratory for glass industry has produced a new glass of great resistance, so that a glass thermometer has been made to read to 550° C. (1,022° F.). In this instrument, the capillary above the mercury column is filled with carbonic acid gas. At low temperatures, mercury thermometers have the drawback that, when the temperature sinks to - 39° C., the mercury freezes. For low temperatures alcohol thermometers are usually employed; but since it is difficult, if not impossible, to obtain the alcohol entirely free from water, their registration cannot be entirely trusted. Anhydrous toluol (colored black) has been proposed as a substitute, its limit being ff- 170° C. and - 70° C.* Because of its black color, the column is easily dis- tinguished ; it expands with great regularity, and being of much less density than mercury, the bulb of the thermometer can be made larger, thus securing greater exactitude in the registration. It, however, does not receive impressions of heat and cold very readily, hence it is very slowly sensitive.f Conditions of Delicacy.—A delicate thermometer should indicate very small changes of temperature, and should quickly assume the temperature of the surrounding medium. To fulfil this con- dition, the capillary tube should be very narrow, so that each degree occupies as great a length on the stem as possible, and may easily be subdivided into small fractions. The bulb should be as small as possible, so that it may rapidly assume the tem- perature of the surrounding medium. Thermometers, even when constructed with the greatest of care, are subject to various sources of error. These are 1st: The bore or calibre of the thermometer may not be uniform. 2d: A gradual contraction of the bulb may cause the zero point to rise. 3d: A gradual expansion of the bulb may cause a lowering of the zero point. A thermometer bulb after being blown and allowed to cool, con- tinues to contract long after the glass has attained its normal tem- perature, even for a period of two years or more. Thermometers which have been exposed to prolonged high temperatures suffer a marked expansion of the bulb. For this reason, thermometers which are employed for scientific purposes should be examined from time to time. The most convenient for purposes of compari- son and correction, are the so-called “ Normal Thermometers.” These are very accurate instruments, having been compared with the air thermometer, and are usually accompanied with a table of corrections furnished by some authority engaged in the verifi- * Must be under pressure, as its boiling point is 111°. t Messrs. Baly and Chorley have constructed a thermometer of a very resistant glass, which will stand a red heat; employing in place of mercury an alloy of sodium and potassium. The boiling point of this is near 700° C., and congealing point at -8° C. It is graduated from 200° C. on. The capillary above is filled with Nitrogen under a pressure equal to that of the atmosphere outside. 61 HEAT. cation of standards. The thermometer to be tested is suspended alongside of a normal instrument, and the bulbs of both immersed in a bath of sulphuric acid, which is slowly heated, under the same conditions as in the determination of melting points (Fig. 88), the temperatures being compared and noted. When such an instru- ment is not at hand, the best plan is to ascertain the accuracy of the zero and boiling points. To determine the accuracy of the zero point, we fill a funnel with crushed (well washed) ice, so that the "water may have free escape; in this the thermometer is im- mersed so that the top of the mercury column (0° C. or 32° F), is below the surface of the ice. Here it is allowed to remain from 15 to 30 minutes, then the height of the column is noted without removing the instrument, when it should stand at 0° C. or 32° F. For making the readings, a lens should be employed. To ascertain the accuracy of the boiling point, suspend the entire thermometer at least a few degrees above its boiling point mark, in the steam which issues from boiling dis- tilled water, as illustrated in Fig. 82. With the barometer standing at 760 milli- meters, the mercury should be stationary at 100° C., or 80° R., or 212° F. If the barometer varies from the standard of 760 Mm., then an increase of pressure of 1 Mm. of mercury produces an elevation of the boiling point by 0.0375° C.; or, an eleva- tion of the boiling point by 1° C. cor- responds to a difference of pressure of 26.8 Mm. of mercury. This correction is applied thus: supposing that the boil- ing point reading was 99.5° and the height of the barometer 752 Mm.; then the required correction would be —= 261 — 0.3°, therefore, the corrected boiling point would be 99.5° + 0.3° = 99.8°. The results of examination would be entered thus:— Fig. 82. Boiling-point Determination. Freezing point, -0.1°. Boiling “ 99.8°. To calibre the tube, that is to ascertain whether the calibre is uniform throughout, a short portion of the mercury column is detached from the remainder by a slight jerk, and, on inclining the tube it may be made to pass from one portion of the bore to another. If the scale is properly graduated, the column will fill an equal number of divisions throughout.* * For the accurate calibration of a thermometer see Kohlrausch’s “ Leitfaden der Praktischen Physik.” 62 HANDBOOK OF PHARMACY. BOILING POINT. Boiling is the conversion of a body from the liquid into the gaseous condition, which takes place from the surface as well as the interior, elastic bubbles of vapor being rapidly produced, which give rise to a bubbling movement throughout the entire liquid. The boiling of a liquid takes place at a constant tempera- ture which depends on the nature of the liquid and the atmos- pheric pressure. The Boiling Point is “the temperature at which the evolved vapors overcome the atmospheric pressure” or at which the tension of its vapor equals the atmospheric pressure. The tem- perature of ebullition or the boiling point, rises with increasing, and falls with decreasing pressure. For instance, water boils on the Montblanc under a pressure of about one-half an atmosphere at 86.5° C. Under a pressure of of an atmosphere, it would boil at 0° C. The temperature of the evolved vapors is known as the boiling point, and this is entirely independent of the various conditions which influence the boiling of liquids, since the tem- perature of the boiling liquid depends on the amount of air bub- bles, the nature of the containing vessel, its surface, the nature and cohesion of the fluid, the atmospheric pressure, etc. Since the boiling point is an un- changeable physical con- stant, the determination of this affords, like that of the “melting point,” a means of identification, and gives us a very important criterion concerning the purity, of many substances. For determining the boil- ing point of liquids, an ap- paratus arranged as shown in Fig. 82 may be em- ployed ; but should the liquid be inflammable, the apparatus must be so ar- ranged that the vapors may be removed and condensed, asshowninFig. 84. Forthis purpose a “ fractionating flask ” (Fig. 83) is selected. The thermometer should extend far enough down the neck to have its bulb slightly below the side exit, and it should never come in contact with the boiling liquid itself. The flask, which should never be filled more than about f full, as shown in the Fig. 83. Fractionating Flask (Measurements in Centimeters) HEAT. 63 illustration, is then connected with a condenser and distillation commenced, by heating the flask very slowly over a low flame. As soon as the liquid begins to boil, the thermometer ceases rising and remains stationery. Care must be taken not to heat too rapidly, beginning with a small flame and slowly increasing if necessary. Fig. 84. Apparatus for Fractional Distillation. By determining the melting point we are able to judge, not only as to the identity, but also as to the purity of many organic solids. The presence of but minute amounts of admixtures mostly influences the melting point by either raising or lowering it. The constancy of the melting point of a substance after re- crystallization, is a proof of its purity. To determine the melting point, we first prepare one or more suitable tubes. This is done by heating uniformly a tube of light fusible glass in a strong gas flame, drawing it out when sufficiently soft, as illustrated in Figure 85, then cutting it in the middle of the capillary and at both of the enlarged extremities, and closing the tips of the pointed extremities in the flame. The substance to be examined is then reduced to a fine powder, placed on a watch glass and either dried in an oven at 100° C., or allowed to stand over sul- phuric acid in a desiccator, until it ceases to lose weight. The fine powder is introduced into the tube and by careful tapping is brought to the bottom. The capillary is filled to a height equal MELTING POINT. 64 HANDBOOK OF PHARMACY. to that of the mercury in the bulb of the thermometer. Care should be taken that the powder is not packed too firmly in the tube. Then the one or two tubes are fastened to the ther- mometer by means of a rubber band (Fig. 87), care being taken that it is at least 4 Cm. (1| inches) above the surface of the liquid into which the tubes are inserted. The thermometer with attached tube, is secured in a clamp and lowered into a beaker glass (100-120 Cc.), which is filled about two-thirds full Fig. 85. Drawing Out Tubing. with any clear liquid which is a good conductor of heat. The extremity of the thermometer should extend to within about 1.2 Cm. (or | inch) of the bottom. The beaker is then placed on a wire gauze and heated slowly by a low flame, the liquid being carefully stirred so as to insure a uniform equalization of the temperature throughout. Most substances shrink just before melting, which usually takes place suddenly. The moment when this occurs, note the temperature of the thermometer. It Fig. 86. Capillary Tubes for Melting Point Determination, a. Properly drawn, b, c. Poorly drawn. should be observed whether the body melts suddenly and en- tirely, or whether a portion melts and the balance requires a higher temperature and greater length of time until a clear fluid results, this extending over several degrees of temperature. When such is the case, the substance is not uniform, that is, there may be an admixture of some foreign or allied body of a higher or lower melting point, or it is sometimes due to imperfect drying of the substance. Some bodies melt with decomposition, gener- HEAT. 65 ally giving off gases or charring. As fluids for heating, we usually employ Distilled water for substances which do not melt above, . . . 80° C. Pure concentrated sulphuric acid for substances which do not melt above, 180° C. Paraffin for substances which do not melt above, 300° C. Sulphuric acid is most generally employed for this purpose. Fig. 87. Fig. 88. Melting Point Tubes in Position. Taking Melting Point in Bath of Sulphuric Acid. Another form of apparatus (Fig. 90) is often employed, which is essentially a double-mantled tube. The outer tube (b, b) is filled with sulphuric acid, introduced at d, the inner one (c) serves as an air-bath, in which the entire thermometer is sus- pended, being thus subjected to a uniform temperature. MELTING AND CONGEALING POINT OF FATS AND WAXES. There are various methods in use for determining the melting point of fats, which yield more or less discordant results. Some methods rely upon the temperature at which the fat begins to melt, others upon the temperature at which the mass is entirely 66 HANDBOOK OF PHARMACY. melted and clear; still others, upon the temperature when the fat begins to soften. The simplest method is to draw, by suction, a little of the melted fat into a capillary tube, to fuse the end of this in a flame; when cool, to fasten it to a thermometer and to proceed as already directed. Bensemann suggests that a few drops of melted fat be brought to the position a (Fig. 91), by holding the tube horizontally and tipping, then cooling by drop- Fig. 90. Fig. 89. Fig. 91 Long-neck Flask for Melting Point Determinations. Air-Bath for Melting Point Determinations. Tubes for Fusing Point Determinations. ping water or ether on the outside; placing in a beaker of cold water, attaching to a thermometer, and then warming very slowly. The moment when the solid particle of fat becomes loosened and begins to flow down the side, the temperature is taken as the “ Beginning Point; ” the moment it unites at b to form a clear globule of melted fat, the temperature is taken as “ Complete Melting Point.” CHAPTER IV. APPLICATIONS OF HEAT IN VARIOUS OPERATIONS. Under this head, those operations which require a high degree of temperature will be considered first. Use of the Blowpipe.—A knowledge of the uses of the blow- pipe is important, because of its various applications in analytical chemistry. For a thorough treatise upon this subject, the student is referred to Plattner’s “ Blowpipe Analysis.” In using the blow- pipe (Fig. 93), a constant and uniform blast of air must be kept Fig. 92. Fig. 93. Sectional View of Bunsen Flame. Blowpipe. up through the tube by the operator, who must use the muscles of his cheeks as bellows, keeping them constantly distended, sup- plying air as needed. This blast of air passing through the dark cone of any illuminated flame, produces the same effect as that of the Bunsen flame, only that the flame becomes long and pointed and of a very high temperature, being concentrated on a very small amount of space. The flame (Fig. 92) is divided into 67 68 HANDBOOK OF PHARMACY. two parts, the inner or deoxidizing zone at a a (or a, Fig. 94), for here, where some of the gas is yet unoxidized or unconsumed, oxygen is removed from metallic oxides. The outer zone at e (or b, Fig. 94) is called the oxidizing flame, for by the high temperature and free ac- cess of oxygen, metals are easily oxi- dized. When a flame of very high temperature is desired, the Blast- lamp (Figs. 77-78) is best employed. Operations with the Cruci- ble.— Crucibles are cup-shaped vessels of round or triangular shape, made of such material that they will stand extremely high temperatures. They are em- ployed in carrying on the process of ignition or smelting. For large operations the Hessian or graphite crucible is employed. The former is somewhat porous, hence only adapted for crude work ; the latter withstands a very high degree of heat and rapid changes of temperature without fracture. For general operations of the chemist or apothecary, the porcelain, platinum, silver, or Fig. 94. Blowpipe Flame. Fig. 95. Crucibles, a, b. Hessian, c. Graphite, d. Platinum, e, f. Porcelain, g. Clay. A. Copper. nickel crucible is employed. Porcelain crucibles are best adapted for general use, because of their cheapness, and also because less care is necessary to keep them in order. Moist substances should never be heated in such a crucible over the naked flame; the APPLICATIONS OF HEAT IN VARIOUS OPERATIONS. 69 substance should be first dried by placing the crucible and moist contents on a water bath or in a drying oven, and when thor- oughly dry, placing the substance in the crucible and the latter on a pipe-stem triangle and carefully heating, increasing gradu- ally to redness. These crucibles should not be employed for fusing caustic alkalies. Platinum crucibles are best adapted for all kinds of work ; wet precipitates may be thrown in and ignited at once. They will stand an intense degree of heat, and may be also rapidly heated and cooled. • Mixtures that give off free chlo- rine or contain lead compounds should not be heated in them.* They should be cleansed from time to time by scouring with moist rotten stone; sand should not be used. Silver or nickel crucibles are best adapted for fusing caustic alkalies. Care should be observed not to heat too strongly, for there is danger of melting the silver. The following operations require a high degree of heat. Ignition.—Ignition is employed in analysis to remove the last portions of moisture, or of organic or volatile constituents, from inorganic substances, in order to convert the latter into stable weighable com- pounds. The filter containing the pre- cipitate is folded, laid in the crucible, which is then placed on the triangle and heated slowly, until the filter is reduced to ash; then the heat is increased to dull redness, in which case the blast lamp is necessary; when sufficiently cool it is placed in the desiccator, being handled with a pair of crucible tongs. In the early stage of the operation the crucible lid is removed, until all carbonace- ous matter is burned off; then the cover is replaced and strong heat applied. Examples:—A solution of ferric salt is precipitated by an alkali, and the precipitate washed and dried; ignition then converts the ferric hydrate into ferric oxide, in which condition it is weighed. Fe2(OH)6 = Fe2O3 + 3H2O. Phosphoric acid is precipitated as magnesium ammonium phosphate (2MgNH4PO4 + 6H2O), this on ignition yields 2NH3, 7H2O and magnesium pyrophosphate, Mg2P2O7. The latter, a stable compound, is weighed. Fusion.—This is liquefaction of solids by heat. We fuse those solids which liquefy and do not suffer chemical change by heat. In analytical operations, we fuse silver chloride, to preclude the presence of any moisture. Caustic potash and soda are fused to Fig. 96. Ignition with Blast Lamp. * Also caustic alkalies, cyanides, or metallic salts mixed with organic matters. 70 HANDBOOK OF PHARMACY. remove all traces of moisture, then moulded into sticks for the sake of convenience. Calcination.—Some inorganic substances are strongly heated (until of constant weight), to remove some volatile constituent, as water of hydration or carbonic acid gas. Example.—Limestone or marble, on being strongly heated, yields calcium oxide (burnt lime). CaCO3 = CaO + CO2. Mag- nesium carbonate (MgCO3)4 Mg(OH)2, when calcined, yields mag- nesia (MgO), water, and carbonic acid gas. Deflagration.—The subjecting of inorganic salts to strong heat, whereby decrepitation takes place, with the giving off of oxygen. Example:— NaNO3 = NaNO2 + O. 2KC1O3 = 2KC1 + 3O2 Sodium Nitrate. Sodium Nitrite. Oxygen. Potassium Chlorate. Potassium Chloride. Oxygen. Torrefaction.—The subjection of drugs to roasting, whereby an alteration in their properties and constituents takes place. Example.—Roasting of coffee. Rhubarb possesses cathartic properties, but on roasting, the cathartic principles are destroyed and an astringency is developed. Carbonization.—The subjection of organic substances to strong heat, out of contact with air. Example.—Wood charcoal and animal charcoal. When these are burnt in open air, ashes result. CHAPTER V. VAPORIZATION. OPERATIONS REQUIRING A LOWER DEGREE OF HEAT. The slow conversion of a liquid into the gaseous condition is designated by the general term—Vaporization. As applied in pharmacy, when it is intended to separate a volatile liquid or solvent from a solid, or a more volatile from a less volatile liquid, or for the purpose of concentrating a liquid, the process is called— Evaporation. When the volatile portion or portions are sought for, it is called— When a volatile is to be separated from a non-volatile solid, it is called—Sublimation. When solids are deprived of moisture at a low temperature, it is called—Desiccation. When crystalline salts are deprived of their water of crystalli- zation by means of heat, it is called—Exsiccation. EVAPORATION. In pharmaceutical operations, we resort to evaporation for the concentration of liquids, the collection of a dissolved body (extracts), or for the purposes of crystallization. For pharmaceu- tical or technico-chemical purposes, the principal object to be considered, is the saving of time and fuel. In quantitative analy- sis this is not considered, care and attention being directed to guard against loss or contamination of the substance operated upon. According to the nature of the solvent and dissolved body, the method of evaporation may vary, as to the vessel in which it is carried on, or the nature of the source of heat. The rapidity of evaporation depends upon: 1st. The amount of surface of the liquid exposed. 2d. The temperature of the liquid. 3d. The nature of the liquid and dissolved body. 4th. The atmospheric pressure, also the atmospheric humidity. 5th. The nature of the vessel. 1st. The larger the amount of surface exposed to the atmos- phere, the more rapid is the rate of evaporation, for it is evident, that a liquid, contained in a shallow evaporating dish, will evap- orate more rapidly if exposed to the same temperature, than the same quantity contained in a deep narrow vessel. Shallow vessels favor ebullition, since there is a lesser weight of liquid above the source of heat, thereby affording less resistance to the 71 72 HANDBOOK OF PHARMACY. escape of bubbles. When we evaporate below the boiling point, we endeavor to present as much surface as possible to the air; Fig. 97. Mechanical Stirring Apparatus for Evaporating Fluids. hence, by stirring, a fresh surface is constantly brought into con- tact with the air. This operation may be carried on mechanic- Fig. 98. Mechanical Stirring Apparatus (Kaehler and Martini). ally by means of rotating paddles or stirrers as shown in Figs. 97, 98. This method of evaporation is largely employed in phar- maceutical laboratories, when we desire to rapidly concentrate a VAPORIZATION. 73 fluid at as low a temperature as possible, to avoid injury to the drug. In various industries, where surface evaporation is re- sorted to, large surfaces are exposed in shallow tanks, over which the flame or hot gases from the furnace are allowed to pass. Fig. 99 illustrates the same principle, but in another form. This patented apparatus of Siebert (Hanau a/M) is employed, particu- larly in the concentration of sulphuric acid. The acid to be con- centrated flows into the pocket at d, the blade f controls the flow so that only a thin stream trickles down the steps of the heated cascade, the vapors being removed through b. 2d. The increase of temperature in a liquid accelerates evap- Fig. 99. Cascade Evaporator (Siebert). oration by increasing the elastic force of the vapors, thereby facilitating their rapid liberation. 3d. The nature of the liquid or solvent, that is, the density and cohesion of liquids, influence the elastic force of the vapors. Relatively light and mobile liquids, as ether or alcohol, evaporate far more rapidly than water, since they allow a rapid escape of the bubbles, while on the contrary, the cohesiveness of a solution, like that of syrup or mucilage, offers considerable resistance. The presence of a dissolved body raises the boiling point of a liquid materially,* hence, not only is a higher degree of heat re- quired, but the rapidity of evaporation may also be greatly im- * See Saline Solutions. 74 HANDBOOK OF PHARMACY peded, by the formation of a crust of saline or other solid matter on the surface of the liquid, which would prevent the escape of steam bubbles. 4th. Influence of atmospheric pressure. As already stated, the boiling point of water at normal atmospheric pressure of 760 Mm. is 100° C. If the pressure be decreased, the boiling point likewise decreases, with an increase of rapidity of evaporation.* If pressure be exerted upon the surface of the liquid, it causes a material rise in the boiling point, diminishing the rapidity of evaporation.f Again no evaporation can take place in a space Fig. 100. Fig. 101. Evaporation. already saturated with the vapor of the same liquid; hence the rapidity of evaporation is influenced according as the surround- ing atmosphere is more or less charged with the same vapor. If we direct a current of air over the surface of the fluid, we remove these vapors, thereby facilitating the rapidity of evaporation. * See Vacuum Apparatus. t At barometric pressure of 760.00 Mm. 1 atmosphere, the boiling point of distilled water is 100° C. “ “ 88.74 “ “ “ 50° C. “ “ 23.10 “ “ “ 25° C. “ “ 5.06 “ “ “ 0° C. With tension of 1 atmosphere the boiling point of distilled water is 100° C. “ “ 15 atmospheres “ “ 200.5° C. « « 100 « “ « 311.4° C. VAPORIZATION. 75 With this end in view, various forms of apparatus have been devised. Figs. 100,101, illustrate a very simple and old mode of creating a current of air during evaporation. By means of a clamp, the funnel is held inverted over the evaporating dish, the vapors rising upward through the funnel, and, like a smoke-stack, cause (by suction) a current of air to flow in over the surface. In Fig. 100 the edge of the funnel is curved inward, forming a trough to collect any vapors that may be condensed, thereby pre- venting them from running back into the fluid. Fig. 101 consists of a plain funnel with a glass tube fitted into the neck by means of a cork, the lower end extending close to the surface of the liquid. 5th. Nature of the vessel and surface. Evaporation proceeds more rapidly with less heat, in vessels of copper, platinum, iron, tin, etc., than in those of porcelain or stoneware, because of the greater heat-conductivity of the former. If the inner surface of the vessel be rough, corrugated, or uneven, more surface is Fig. 102. Evaporating and Crystallizing Dishes, thereby exposed to the source of heat, imparting therefore a greater amount of heat to the fluid, thereby facilitating evapora- tion. In a glass vessel of smooth surface, the temperature of water may rise to 105° C. before boiling, because the water be- comes superheated ; if, however, a piece of broken glass be placed in the vessel, ebullition will proceed rapidly and quietly at the usual temperature of 100° C., the sharp edges of the glass acting mechanically, in assisting the disengagement of heat bubbles. Evaporating Vessels.—Porcelain dishes are best suited for the general uses of the apothecary. They should be as shallow as possible, as illustrated in Fig. 102. The last four, flat-bottomed, are intended as crystallizing dishes. Because of their fragile nature, to avoid injury to either the vessels or the substance, they are best heated on a steam, water, oil or sand bath. Where it is necessary to heat directly, the precaution should be taken carefully to dry the outside of the vessel, then to place on a wire 76 HANDBOOK OF PHARMACY. gauze (Fig. 103), and to begin heating gradually. When heated over a naked flame, porcelain cracks readily if the residue is allowed to set or cake in the bottom ; hence, in evaporating any saline so- lution, we should always carry on the operation on a bath, thereby not only avoiding the danger of break- ing the dish, but also the sputtering of the boiling liquid and decrepita- tion of the drying salt. Enameled sheet iron dishes (agate ware), are very useful and lasting; they should be discarded should the enamel chip off inside. Copper and earthen ves- sels are employed only by the manu- facturer for larger operations. In many chemical and pharmaceutical operations, it should not be forgotten that the material of the evaporating vessel exercises considerable influ- ence on the liquids to be heated. Distilled water, when boiled some time in glass vessels, dissolves appreciable quantities of this material, owing to the formation of soluble silicates. The particles dissolved, consist chiefly of potassa, or soda or lime, in combination with silicic acid. A much larger Fig. 103. Evaporating over Direct Flame. Fig. 104. Fig. 105. Evaporating with Properly Regulated Flame. Evaporating Flame Unnecessarily High. proportion of glass is dissolved by water containing caustic or carbonated alkali. Traces of copper are generally found in extracts which have been evaporated in copper vessels. Vacuum Apparatus—Distillation under Diminished Pres- sure.—The boiling point of a liquid is materially lowered by the VAPORIZATION. 77 removal of atmospheric pressure (page 74). We find a practical application of this fact in the “Vacuum Apparatus.” It is of the greatest value in pharmacy, for the rapid concentration of certain solutions, chiefly of organic substances, such as the preparation of solid extracts. By means of this, we not only increase the rapidity of evaporation, but avoid injury to the sensitive plant principles by the lower degree of heat employed Fig. 106. Pharmaceutical Vacuum Apparatus. and absence of the oxidizing influence of the atmospheric air. Fig. 106 illustrates a smaller vacuum apparatus for the use of apothecaries. Its construction and use is exceedingly simple. The copper vessel A, serves as a water or steam bath; in this is suspended a porcelain or copper evaporating dish, which is covered with a glass dome B made air-tight by means of a rubber joint; the thermometer is inserted at C, the air is exhausted from the apparatus by means of the water-pump 78 HANDBOOK OF PHARMACY. E, the glass vessel D serves as receiver, and this is closed by a metallic lid to which is attached the indicator F, enabling the operator to control the vacuum. Fig. 107 illustrates a sectional view of a vacuum pan of modern construction, such as is employed in the industries in the evaporation of sugar solutions, or the pre- paration of extract of beef or of condensed milk. Rapid Evaporation.—Besides the usual methods of facilitating evaporation as already mentioned, another deserves mention, and that is the method of evaporation by the application of heat over the surface of the liquid. This method is applicable to all non- Fig. 107. Vacuum Apparatus (Sectional View). inflammable liquids such as are not injured by heat. Fig. 108 illustrates Hempel’s method, in which a flame burns directly above the surface of the liquid, the entire apparatus being enclosed in a cylindrical glass vessel, which is connected with a pump, for the rapid removal of the vapors and gases. Another method, is that of the Government laboratory of the Netherlands. The apparatus consists of an iron plate standing on four legs; near each corner is an opening, through which the tubes of four Bunsen burners are adjusted to such a height that their tops will be a little higher than the edge of the capsule, which is placed on the iron plate. A second plate is then adjusted over the burners. When the four flames are lit, the upper iron plate causes the flame to spread out along the plate, the direct flame and radiation of heat causing a rapid evaporation to take place. In evaporating inflammable liquids on the water bath, it is best to surround the flame by a VAPORIZATION. 79 wire gauze (Fig. 109), to prevent any danger of the liquid or vapor igniting. For evaporating or concentrating small amounts of very vol- atile solvents, such as ether, carbon disulphide, or petroleum-ether, it is best to place the vessel in a drying closet or desiccator, or under a bell jar which contains an absorbent, such as sulphuric acid, burnt lime, etc. For wThen we allow these fluids to evaporate in the open air, owing to the lowering of temperature, and the rapidity of evaporation, water is condensed on the sides of the vessel and contaminates the residue. Evaporating vessels of perpendicular sides should be employed for volatile fluids containing solids in solution, as such liq- uids tend to crawl up over the edge of the dish and deposit solid matter on the out- side. In evaporating liq- uids which give off irritating or corrosive vapors or gases, the operation should be carried on in a “ Draught Chamber ” (Fig. 110). This may be built into a chim- ney-flue or imme- diately in front of it, the flue leading off from the top of the chamber as shown in Fig. 111. A gas flame above, serves to create a strong, steady draught. The chamber may be ar- ranged as shown in Fig. 110, where the draught chimney extends up one side of the chamber, there being an opening below, where the gas may be lit. Above, near the top, is a similar opening which serves to remove all gases. In absence of such arrange- ments, we can remove noxious vapors by inverting a large glass funnel over the evaporating liquid, it being held in position by means of a clamp over the neck, a rubber tube being attached to the end of the stem, and the other end of the tube being led to a water pump. The suction produced will carry off all traces of noxious vapors. In evaporating such liquids as contain salts in solution, it is necessary to stir constantly, for, as they become concentrated, a saline scum forms upon the surface, which prevents further evap- Fig. 108. Fig. 109. Bath for Evaporating Inflammable Liquids. Hempel’s Evaporator. 80 HANDBOOK OF PHARMACY. oration. Those liquids which form a scum or skin on the surface (for instance, milk), or frothy solutions, should be mixed with washed sand or pulverized glass and then constantly stirred while evaporating. Spontaneous Evaporation.—Water, and many other liquids, will evaporate without the application of heat, simple exposure to the air, with as large an area of surface as possible, being all that is necessary. We apply this method of concentration to those liquids which contain bodies that are injured by any degree of Fig. 110. Fig. 111. Draught Chambers. heat, also for the slow vaporization of solutions of crystallizable bodies, so as to obtain well formed crystals. Instead of placing these vessels in the open air, wre sometimes place them in a dry- ing closet (Fig. 172), always taking the precaution to cover the vessel loosely with muslin or filter paper, to prevent particles of dust from dropping into the fluid. We sometimes carry on slow evaporation, by placing the dish on a tripod and setting this upon the flat top of a stove or over a hot-air radiator. VAPORIZATION. 81 Baths.—For general purposes of evaporation we employ various baths, in order that we may control the temperature of evapora- tion. Sometimes it is necessary to subject a liquid to a prolonged Fig. 114. Fig. 112. Fig. 113. Iron Water-Bath with Constant Level. Copper Water-Bath. Iron Water-Bath. high degree of heat; again in others it is necessary that the tem- perature should not rise above a certain limit. For the purpose of regulating the degree of heat, we use various liquids of different Fig. 116. Fig. 115. Water-Bath with Constant Level (Kekulti). Water-Bath with Constant Level. boiling points. The most common of these is water (used in the water-bath), by means of which we reach a temperature of about 97° C. A water-bath is generally constructed of copper or iron 82 HANDBOOK OF PHARMACY. (Figs. 112,113). In order to avoid the inconvenience of constant watching, to prevent them becoming dry, the water-bath with Fig. 117. Fig. 118. Water-Bath (Landolt). Steam Evaporating Kettle. “ constant level ” (Figs. 114,115, 116) is preferably employed. In this, the water enters through B, flows through the horizontal tube Fig. 119. Iron Sand-Baths. C into the bath; this when filled to a certain height, causes an overflow in B which is drawn off by A. By connecting this with Fig. 120. Filling Sand-Bath. a hydrant, the supply of water can be automatically regulated. Fig. 116 illustrates another design in which the water is supplied from a self-regulating flask. Fig. 118 illustrates a large copper VAPORIZATION. 83 bath heated by a steam jacket; this is adapted for evaporating large quantities of liquids, as in the preparation of extracts. J. Sand-bath (Fig. 119) consists of an iron vessel with either round or flat bottom, which is filled with clean, dry sand. The vessel to be heated is partly embedded in the sand and the entire apparatus placed on a tripod (Fig. 120) and heated. We employ the sand-bath where we desire to heat a body to a high temperature; it also prevents a too rapid rise or fall of tempera- ture which might fracture the vessel. Sea-sand answers best for this purpose, but it should be well washed and dried before use. Not more than a | inch layer of sand should be between the bottom of the vessel and the flame. The Oil-bath is intended for temperatures not rising above 250° C. (482° F.). For this purpose paraffin is best adapted, since most fixed oils evolve very unpleasant odors when heated. Glycerin may be employed for temperatures up to 165° C.,(329° F.). Fig. 121. Tripods. Baths of Saline Solutions are occasionally employed in oper- ations where we desire a certain regulated temperature, without the precaution of a thermometer. The boiling point of distilled water is 100° C. (212° F.), but if we add any inorganic salt, the boiling point will be raised in proportion to the quantity and nature of the salt added. If we form saturated solutions we find their boiling points constant. The following table gives the tem- perature obtained by boiling saturated solutions of C. F. Sodium Sulphate, 100.5° 213.5° Copper Sulphate, 102.° 215.6° Sodium Borate, .... 105.° 221.0° Sodium Chloride, 106.° 222.8° Ammonium Chloride, 112.° 233.6° Sodium Nitrate, 117.° 242.6° Sodium Acetate, 122.° 251.6° Calcium Chloride, 141.° 285.8° Zinc Chloride, 160.° 320.0° Zinc Chloride, Fused, 700.° 1292.0° 84 HANDBOOK OF PHARMACY. Air-bath*—“ Dr. H. Fleck recommends the simple air-bath, illustrated by Fig. 122, which has been in successful use for several years, doing all the duty of a water-, oil-, or paraffin- bath. By a circular cut, or other means, glass rings are prepared from cylinders of various sizes. These rings, from 2 to 10 Cm. in height, are set upon an iron plate, and covered with a similar one, having suitable openings for receiv- ing a thermometer and the vessels intended to be set upon it. If high temperatures are re- quired, low cylinders (of about 2 Cm. in height) are selected; low temperatures require higher cylinders (5 to 10 Cm.). The cylinders are scratched with a diamond, in a vertical direc- tion, so that, if they should crack, the fracture would always be up and down. This simple apparatus permits the maintenance of constant temperatures of 50 to 300° C. (122 to 572° F.) and over. Its transparency is an additional advan- tage, when it is of importance to watch the pro- gress of reactions, as often happens, in synthetical experiments.” Fig. 122. Fleck’s Air-Bath. * As described in the “ Proceed. Amer. Phar. Ass’n,” 1882, p. 53. CHAPTER VI. DISTILLATION. Distillation is a process whereby a liquid, by means of heat, is converted into a vapor, and this in turn condensed to a liquid by Fig. 123. Simplest Form of Distillation. means of a properly arranged cooling apparatus. This process is resorted to as a means of purification, or for the separation of Fig. 124. Distillation (Improvised Condenser). 85 86 HANDBOOK OF PHARMACY. the more volatile from less volatile liquids. The apparatus (Fig. 125) consists of a distilling flask (or retort) A, in which the fluid is heated; the cooling apparatus B, in which the vapors are Fig. 125. condensed, is called the condenser, and the receiver C, which serves to collect the condensed liquid. The distilling flask may Distillation. Fig. 126. Fig. 127. Fractionating Flask with Thermometer. Flask with T-Tube for Fractionating. be either a retort as illustrated in Fig. 123, or an ordinary flask fitted with a bent tube serving as a beak (Fig. 125), or we may employ the “fractionating flask” (Fig. 126), which admits the use DISTILLATION. 87 of a thermometer, the projecting side tube being connected with the condenser. Retorts are either closed as illustrated in Fig. 128, a, b, or pro- Fig. 128. Glass Retorts, a, 6. Plain, c, d. Tubulated. vided with tubulures as in c, d, through which liquids may be introduced, and a thermometer or safety tube inserted. This tubulure must be so placed, that the ther- mometer or safety tube may stand erect and not come in contact with the sides of the retort. The retort must be bent in sharp at the throat, without, however, Fig. 130. narrowing the tube (see Fig. 128, a). The form b should not be used, because, in boiling, the fluid is liable to be carried over mechanic- ally. Fig. 128, d illustrates a poorly placed tubulure. Besides glass re- torts, we find them made of porce- lain, earthenware, iron, lead, copper and platinum. Condensers.—Fig. 132 illustrates the most simple form of the so-called “Liebig’s Condenser,” which consists of a long glass tube surrounded by another of larger diameter, but somewhat shorter. At either end of the larger outside tube, is inserted a perforated cork, Filling Retort. Earthenware Retorts. Fig. 131. Lead Retort. 88 HANDBOOK OF PHARMACY. which serves to hold the inner tube and admits a short bent tube at both ends, serving for the admission and discharge of water which circulates in the space between the smaller and larger tubes. Figs. 133, 134, 135, illustrate other forms, in which the openings for water are made in the upper and lower ends of the outer tube. Another form is that in which the inside condensing tube con- sists of a spiral; this offers a very large condensing surface, which is necessary in distilling volatile liquids, such as ether or carbon disulphide. Fig. 136 illustrates the “worm condenserthese are made of glass or metal. When of metal, the condensing pipe should be of block tin; it is cooled by means of water or a mixture of salt and ice. Fig 132. Fig. 133. Fig. 134. Fig. 135. Liebig Con- denser. Liebig Condenser (Various Forms). When the boiling point of the liquid is above 150° C., it is only necessary to employ an air cooler, which consists of a straight tube of large enough diameter to slip over the tip of the fractionating flask, as in Fig. 137. The Receiver is that vessel into which the distillate is discharged. For this purpose we employ flasks or beaker glasses. The tip of the condenser should reach inside of the receiver, and these con- nections should, if the liquid is volatile, be as tight as possible, making allowance however, for the escape of air. Adapters are conical or tapering tubes of glass, which are 89 DISTILLATION. intended to be attached to the extremity of the condenser for conveying the distillate into the receiver, or for attaching the retort or flask to the condenser (Fig. 142). Pinch-cocks.—For the purpose of regulating the flow of a liquid or gas through a rubber tube, we em- ploy the pinch-cock (Fig. 138); b illus- trates the usual form, which is in- tended for closing a tube entirely; c and d can be regulated by means of a thumb-screw, hence they are better adapted for general use. The form illustrated in Fig. 139 recommends itself, in that it can be quickly ap- plied or removed from a rubber tube, without breaking a joint; and by means of the thumb-screw, the flow of gas or water can easily be regulated. in the fitting up of apparatus, some attention must be given to the cutting and bending of glass tubing. Heavy tubing should not be used, except in special instances where strength is specially desired. Cutting.—Glass tubing is cut by means of a triangular file or a hardened knife edge. Make a single well defined scratch or cut Fig. 136. Distilling Apparatus with Worm Condenser. Fig. 137. Distillating with Air Condenser, a. Distillating Flask, b. Air Condenser, c. Receiver. across the surface, then grasp the tube on each side of the cut, (Fig. 144) with thumbs opposite, and carefully tap on the edge of 90 HANDBOOK OF PHARMACY. a table. With tubes of larger diameter or of very thick walls, the file cut should extend at least half around the tube. When the file or knife fails to cut properly, moisten with water or oil of turpentine. When it is necessary to break off a short piece, near the end of a tube, hold the shorter portion in a towel to protect the hand from accidental cutting. The rough ends of tubing should always be rounded off by holding (rotating) them in the Bunsen flame. Fig. 138. Pinch-cocks. Bending Tubing.—Tubing is best bent in the wide gas-flame, holding it horizontally, and rotating slowly and continually so as to heat the tube uniformly on all sides. As soon as the glass begins to soften, hold it steady, and allow it to slowly bend to the desired angle, as shown in Fig. 145. In bending a tube, force must not be used, the tube must be carefully and equally heated on all sides, otherwise the angle will be unevenly bent or collapse (Fig. 146, b, c). A poorly bent angle may be restored by softening it in the flame and then blowing into the tube gently, having closed one end with a cork. Drawing out of Tubing.—It is often necessary to draw a tube out to a fine point for use in the wash bottle (also called “ spritz bottle ”), or for making a capillary tube for melting point determinations. The same precautions should be observed here in regard to heating, as above stated; then, when the glass is sufficiently soft, the tube should be drawn out slowly to the desired length, constantly rotating. Fitting Joints.—For fitting the joints of apparatus, the best velvet corks should be employed. Rubber stoppers are still better, as Fig. 139. Adjustable Pinch-cocks. DISTILLATION. 91 Fig. 140. Fig. 141. Retort Stand. Receivers, a. Plain, b. Tubulated, c. Quilled. Fig. 142. Adapters (Various Forms). 92 HANDBOOK OF PHARMACY. they give a very secure joint, impervious to acids and gases. But rubber should not be employed where it might come in contact Fig. 143. with such solvents as chloroform or carbon disulphide. Corks, before being used, should be gently pressed and softened, then Retorts with Adapters. Fig. 144. Position for Breaking a Tube. perforated by means of the cork borer (Fig. 147). Cork borers are brass cylinders, the lower edges of which are sharpened, the Fig. 146. Fig. 145. Bending Tubing. Properly and Poorly Bent Tubing. DISTILLATION. 93 milled heads affording a firm hold. When dull, the edges are readily sharpened on a whetstone or by a file. In boring a cork, place it on a block of wood, then with a tube of the desired size, moistened with water, push through with a twisting motion, taking care to keep the instrument perpendicular. In boring through a thick cork, the bored portion is apt to break off, before the borer is through. If this happens, the borer should be withdrawn, cleared of the broken piece, then wetted and reinserted, when it will readily cut its way further. Never try to bore a hole by starting it from both sides; it will rarely come true. In piercing rubber stoppers, the end of the tube should be moistened with alcohol or oil of turpentine. When we desire to connect two tubes of equal diameter or where one just fits over the Fig. 148. Ftg. 147. other, it is best to slip a short piece of firmly-fitting rubber tube over the joint; this will render it air-tight and secure. Mohr’s Cork-borer. Cork-File. 94 HANDBOOK OF PHARMACY. Inverted or Upright (or Reflux) Condenser.—When it is desired to subject a substance to the action of a boiling liquid solvent, we Fig. 149. Fig. 151. Lever Cork Press. Fig. 150. Rotary Cork Press. employ a flask with inverted condenser, ar- ranged as shown in Fig. 151. The flask is heated on a water,- sand- or oil-bath, or over the free flame, according to the nature and boiling point of the solvent. Fig. 152 illustrates a Soxhlet’s spherical condenser, which possesses the great advantage of occupying a very little space. The cold water enters at a into the condensing space c, flowing out through b. The vapor enters in from below, circulates around and condenses in the space d. Distillation in a Current of Steam.—This is applicable to such substances as are injured when heated or distilled alone, as the vola- tile oils or organic bases; we also employ it in the separation of volatile from non-vola- tile bodies. The substance is placed in the distilling flask d (Fig. 153) with a little water, then steam (generated in the can a) is blown through. This carries the volatile matter over, to be condensed in the cooler e. Distillation is usually continued until oily globules cease to be driven over. Fig. 152. Flask with Upright or Reflux Condenser. Soxhlet’s Spherical Con- denser. DISTILLATION. 95 Fractional Distillation is the separation of a mixture of liquids of different degrees of volatility, by means of distillation. Mixed volatile liquids have no constant boiling point. The complete separation of two liquids, which boil at different temperatures, can only be carried out easily, when the interval between their boiling points is a large one. If they only differ by 10 to 30 degrees, then on distilling, one will observe a continuous rise of the thermometer without its remain- ing stationary at any given boiling point, and the change in the compo- sition of the distillate will be gradual instead of abrupt. In such cases, the distillate must be collected in separate “fractions,” according to the rise in boiling point, i. e., every 5 or 10 degrees. This must be repeated until the Fig. 153.—Apparatus for Distillation in Current of Steam. a. Can in which steam is generated, b. Safety valve, c. Exit tube for steam, d. Distilling flask, e. Condenser. middle fractions have been separated into the higher and lower boiling constituents. Thus, for instance, on distilling a mixture of two liquids, their boiling points being respectively 100° C. and 150° C., the liquid of lower boiling point does not come over alone at 100° C., nor the higher alone at 150° C., but the thermometer gradually rises from 100° C. up, and we obtain a mixture of both liquids, in different proportions. In this case, we collect that 96 HANDBOOK OF PHARMACY. portion which comes over between 100° and 110°, which consists almost entirely of the lower boiling fraction, then another fraction boiling between 110° and 140°, which consists of a mixture of both constituents in about equal proportions; finally, the fraction from 140° to 150°, which contains mainly the higher boiling liquid. The middle fraction (110° to 140°) is then again fractioned, the respective distillates between 100° and 110° and 140° and 150° being set aside; this is again repeated if necessary, and finally the Fig. 154. French Column Apparatus. high and low boiling fractions (i. e., those from 100° to 110°, and those from 140° to 150°), are in turn distilled, the receiver being changed at every 5 degrees. These products on repeated distilla- tion in the above manner, finally yield the two pure products. For carrying on fractional distillation, the apparatus as illustrated in Fig. 84, should be employed. Rectification is repeated distillation, whereby a distillate of DISTILLATION. 97 greater purity is obtained. It is employed more particularly in the recovery of alcohol from weak alcoholic liquids. Fig. 154 shows the construction of a Column Apparatus such as is employed in rectifying alcohol. It consists of a boiler (a) heated by a steam-pipe, containing the weak alcoholic liquids; the vapors pass upward through the rectifier (b), then over to the condenser (c) The highly concentrated spirit condenses in the refrigerator (d) while the aqueous portion flows by the tube (e) back into the rectifier. Bumping.—Certain liquids, when heated to boiling in glass re- torts, give rise to bumping. Ebullition may begin regularly and the distillation proceed steadily, when suddenly the liquid will become quiet for a few seconds. It then becomes superheated, and this is followed by a slight explosion of accumulated vapor, called 11 bumping.” By the force of the explosion, quantities of the liquid are carried over mechanically, into the condenser. This bumping may be avoided or lessened, by placing pieces of Fig. 155. Retorts for Destructive Distillation. broken glass in the retort, or where admissible, by suspending a string in the flask, reaching just below the surface of the liquid. These act mechanically in assisting the evolution of vapor bubbles. Destructive Distillation is a process by which dry organic sub- stances are subjected to heat in closed iron vessels, whereby gases, liquids, and thick tarry products are obtained. The temperature of decomposition of different substancesis very different; some decompose at a temperature below 100° C., while others require a red heat. Many bodies yield entirely volatile products with no residue, while others leave a large amount of solid residue in the retort. Amber yields Succinic Acid and Oil of Amber. Cane Sugar, C12H22On, yields Caramel, C12H18O9, and water, 2H2O. Salicylic Acid, C7H6O3, yields Phenol, C6H5OH, and Carbon Dioxide, CO2. By the dry distillation of complex organic substances, such as bones, wood, or coal, we obtain a large number of products, gas- eous, liquid, and tarry. 98 HANDBOOK OF PHARMACY. PHARMACEUTICAL STILLS. Stills are employed by the pharmacist for the purpose of recov- ering alcohol or ether, or for the preparation of distilled water. They are constructed of plain or tinned copper and are not adapted for distilling acid or corrosive liquids. They are all con- Fig. 156. Laboratory Copper Still. structed after the same general principle, differing, however, as to their form. The simplest form of a copper still is that illus- trated in Fig. 156, consisting of a boiler surmounted by a detach- able hood ; a block tin worm serves as the condenser. The Curtman Still (Fig. 157) is of simple construction, being specially adapted for recovering alcohol from weak percolates. (a) Serves as the body of the still, (d) is a perforated diaphragm which can be placed in the still when neces- sary. The alcoholic vapors pass upward through the condenser (k, n). Cold water enters at (f). After circulating around the tube (n), the heated water is discharged through the tube (l) into the still head (b), from which it may be siphoned off. The heated water at (b) serves to condense most of the aqueous vapors, while the alcohol, being more vola- Fig. 157. Curtman Still (Sectional View). DISTILLATION. 99 tile, passes over and is condensed by the colder water of the con- denser. When it is desired to prepare essences, spirits or medi- cated waters, the necessary plant parts are placed in the diaphragm d and the steam arising from a passes through, taking up the volatile products. Fig. 159 illustrates Edel’s modified Hood Still. The condenser consists of a number (22) of cylindrical tubes, closed at the upper Fig. 158. end, and fitted into the diaphragm c, c. The cold water circulates around these, thereby affording a very large condensing surface. The Prentiss Still (Fig. 160), or alcohol reclaimer, is based on very much the same principle as the “ Column Apparatus ” (Fig. 154). The boiler of the still (a) has an upright column (b) screwed to it, and inside of this are a series of perforated diaphragms Beck’s Pharmaceutical Still.* * The construction of this still is so simple that an explanation was not considered necessary. 100 HANDBOOK OF PHARMACY. soldered to a central rod (see B, 154). The mixed alcoholic and aqueous vapors pass upward through the diaphragms, which interefere with the passage, and cause the condensation of the aqueous, while the alcoholic vapors pass on through c into the Fig. 159. Fig. 160. Edel’s Hood Still. Prentiss Still. condensing worm, being discharged at g. Cold water enters at e and is discharged at spout f. Fig. 161 illustrates the Remington Still. The body of the still is made of tinned copper, the bottom being flat. The top is surmounted by a flat brass ring, upon which fits a like ring which is soldered to the still top or dome, which is held in position by the clamps l. The opening in the still dome, which is drawn over to one side, is terminated by a brass collar, over which the end of the condenser fits. The condenser, which is but a foot in length, is the special feature; this consists of seven parallel block-tin tubes, enclosed in a copper cylinder. At each end of this cylinder is a short tube, which serves for the inlet and outlet of cold water. Fig. 161. Remington Still (Sectional View.) DISTILLATION. 101 The cold water enters at b, and after circulating between the con- densing tubes, passes out at a. Thus arranged, wre have seven feet of condensing space in a very compact form. C, is a bath for evaporating small quantities of volatile liquids at a low tem- perature; this is clamped between the still body and still head ; the body being filled with water, the waste steam escapes through three apertures in the rim of the water bath. In the preparation of distilled and aromatic waters from plant parts, it is necessary that these substances do not come in contact with the heated sides and bottom of the still, hence the use of a wire cage (n) for this purpose. Fig. 162 illustrates a very useful Automatic 11 rater Still, the lower Fig. 163. Fig. 162. Automatic Water Still. Curran Water Still. vessel being the boiler, the middle one the condenser, the upper one the supply tank. Of the four pipes shown, a is the steam and condensed water tube, coiled, as shown in the condenser tank full of water, and delivering distilled water at a'; b is a pipe leading from the water level in the boiler to the top of the supply tank; c, a pipe, with cork, leading from the bottom of the supply tank to the condenser tank ; and d, a pipe leading from the top of the condenser tank to the bottom of the boiler, e is an opening, with air-tight stopper, for filling the supply tank; and f, a cock to draw off hot water from the boiler. After once starting the distillation proceeds automatically. The still can be operated by placing it on a gas stove or on top of a range or stove. 102 HANDBOOK OF PHARMACY. For the rapid and economical preparation of distilled water, the Curran Still (Fig. 163) is well adapted. Its principle and con- struction are very simple. It consists of a copper boiler a, resting in a galvanized case c, detachable at d b, which is perforated, in order to act as a flue to utilize all the heat from the gas burner, on the sides of the boiler. The vapors pass through the connect- ing pipe f into the worm p p, where they are condensed, being discharged through s w. h is a screw cover removable for filling or cleaning. These stills are constructed so that they may be heated by gas, gasoline or coal. The Mitscherlich Condenser (Fig. 164) is of very simple construction, and can be at- tached to any form of still. When the inner vessel a is twenty inches long and four inches wide, we have a total condensing surface, on the sides of b and d, of five hun- dred square inches. The con- denser consists of an inner vessel a,suspended in an outer vessel b, a space of three- fourths of an inch being allowed between these vessels. These, in turn, rest in another vessel d, d. The vapors pass from the still through e into the space b, b, between a and d, and the condensed liquid is discharged at c. Cold water enters through the tubes r and r, passing into the bottom of the vessel; as it becomes heated, it rises and is dis- charged at y and z. Rice's Pharmaceutical Still* (Fig. 165). An improvement offered here consists of a block-tin worm condenser, enclosed in the cylindrical copper casing immediately above the still-head. This may be used as a reflux-condenser as well as for ordinary distilling operations; it affords also a great saving in space. “ The apparatus consists mainly of two parts, the still and the head with condenser. The still is heated by steam, which enters at m, n being the exhaust- pipe. The condenser is a cylindrical copper vessel, with rounded bottom and closed top, having short tubes projecting from the Fig. 164. Mitscherlich Condenser. •Description taken from “New Remedies,” 1877, page 245. DISTILLATION. 103 bottom and from the top at b and c. The cold water enters through the hose a; at c the water is discharged through the waste pipe d. The head of the still carries three tubulures, one for the insertion of the safety-tube L, another for filling the still, and the third, for the insertion of a thermometer. The condens- Fig. 165. Rice’s Pharmaceutical Still. ing pipe e, e carries the vapors upward to the upper end of the block-tin worm, contained in the condenser, and emerging from it at f. Halfway between f and the end proper of worm, the pipe is tapped and a branch, carrying the faucet h, leads into the still at c, where it terminates under the center of the head in the 104 HANDBOOK OF PHARMACY. form of an Czo, forming a trap to prevent the escape of vapors by this passage. The object of this arrangement is to cause the condensed liquid to flow back into the still as long as the faucet h is open, or to collect it outside by turning off the faucet h. Prolonged digestions with alcohol may be made by means of this apparatus, without any loss of liquid. The head is attached to the still by means of a rubber or pasteboard washer and iron clamps, and when it is desired to remove it, the water is allowed to drain from the condenser, the clamps are removed, and the whole is hoisted up by the tackle k and set to one side.” CHAPTER VII. SUBLIMATION. Sublimation is distillation applied to volatile solids. Certain solids, when heated, are converted into vapor, and this, when condensed on a cool surface, yields the substance in its solid (crystalline) but purified form, called a “ sublimate.” This process can be applied only to such solids as do not undergo decomposi- tion on heating. Sublimation, like distillation, has for its object the separation of the volatile from the non-volatile or less volatile substances. In the first mentioned operation, the product (subli- mate) is solid, while in the second, the product (distillate) is liquid. Fig. 166. Fig. 167. Experimental Sublimation of Sulphur. Oddo’s Sublimation Apparatus. The object of sublimation is therefore solely the purification of the substance. As examples we have iodine, salicylic acid, camphor, sulphur, benzoic acid, etc. We have other examples where the process serves for the formation, as well as separation of the vola- tile solid, as calomel, corrosive sublimate, ammonium chloride. An apparatus for conducting the operation on a small scale (Fig. 167), consists of two circular discs of asbestos a and b. The upper disc has a hole pierced through the middle, in which the beaker c 105 106 HANDBOOK OF PHARMACY. sits, containing the body to be sublimed. Two large beakers are in- verted over this; the inside one serves for the collection of the sub- limate, while the outer beaker condenses any vapors that may escape from the inside. It is well to lay two circular discs of glazed paper (with corresponding holes) under the beakers on a. The Fig. 168. Fig. 169. disc b serves for distributing the heat. With such bodies as am- monium chloride, corrosive sublimate, and ammonium carbonate, condensation takes place at a comparatively high temperature within a small space; the substance is then deposited in compact Bruehl’s Sublimation Apparatus. Sublimation of Benzoic Acid (small scale). Fig. 170. Sublimation of Benzoic Acid (Hager’s Apparatus). masses. When the vapors of the body are conducted into large cool chambers (Fig. 170), the sublimate is deposited in small par- ticles (minute crystals), like that of sulphur. Fig. 168 illustrates a very simple form of apparatus for sublim- ing small amounts. The substance is placed in a small crucible 107 SUBLIMATION. and slowly heated, the vapors condense on the surface of the glass globe, which on cooling, can be removed for the collection of the sublimate. Should the globe become heated, it can be kept cool by laying a cone-shaped spiral of lead pipe (cooled with wrater) on the surface. Fig. 169 illustrates the old method of preparing small amounts of benzoic acid from benzoin. Benzoin in coarse powder, is mixed with dry sand and placed in a shallow tin pan, a; over the top, d, a sheet of filter paper is tied, and this is punctured full of pin holes. A hood, c, is made of glazed paper, fitted, and tied over the top of the pan at d. The apparatus is subjected to a low and uniform heat; the vapors of the benzoic acid pass up through the perforated porous cover and are condensed on the cool sides of the paper hood. Fig. 171. Apparatus for the Preparation of Calomel. Fig. 170 represents the preparation of benzoic acid by sublima- tion. In the chamber a, the mixture of benzoin and sand is heated, the vapors of the acid, by means of a regulated draft, c, e, are caused to pass into, and condense in, the large chamber. The current of air follows the direction indicated by the arrows passing through d,f. The method of the sublimation of calomel is showm in Fig. 171. In the earthenware retort, C, the crude calomel is heated, the vapors pass over into the stoneware condenser, D, where they meet a current of steam from the tube tt, which causes the calomel to condense and to drop into the water below. This treatment aids in dissolving out any mercuric chloride which might accidentally have been formed. CHAPTER VIII. DESICCATION. OPERATIONS REQUIRING A LOWER DEGREE OF HEAT. Desiccation consists in depriving solids (drugs, chemicals) of moisture at a low temperature. Pharmaceutically, its objects are the following :— 1st. It Reduces Bulk.—Vegetable drugs contain a variable amount of moisture,* and, in consequence thereof, are more or less bulky. If we can remove this moisture without injury to the constituents, we will gain a great advantage by concentrating their strength and reducing their bulk. 2d. It Facilitates Comminution.—As long as a drug or chemical contains moisture, it resists pulverization, because of the tenacity and sponginess of the drug, or the dampness of the powder, which causes it to cake. As soon as the moisture is removed, the drug becomes brittle and readily disintegrates. 3d. It Assists Preservation.—As long as vegetable drugs contain moisture, they are liable to become mouldy or to ferment, result- ing in injury to their constituents and rendering them unfit for use. Many chemical salts have the property of rapidly absorb- ing moisture from the air (see Deliquescence), while others lose crystal water and fall to a dry powder on standing in the air (see Efflorescence). In either of these cases, a decided increase or decrease of weight of the salt takes place, with a corresponding increase or decrease of strength ; hence, for the sake of accuracy, as well as convenience, we often resort to desiccation and pulveri- zation of these substances. As time is always a consideration, drugs are rarely subjected to the old process of spreading out the leaves, roots, or bark, and then exposing them to the sun, or in a dry loft. Drugs are dried by placing them, in a coarsely comminuted condition, on wooden trays with a perforated or wire netting bottom. Chemicals are placed on trays with a muslin bottom, * 100 parts of freshly gathered, yield in dry drug about Belladonnae Folia, 18 parts. Arnie® Flores, 20 “ Digitalis, 20 “ Mentha Piperita, 20 “ Taraxacum, 22 “ Scilla, 25 “ Valeriana, 25 “ yield in dry drug about Calamus, 25 parts. Althaea, 25 “ Glycyrrhiza, 33 “ Colchici Radix, 34 “ Belladonnse Radix, 38 “ Stramonii Folia, 45 “ Mezereum, 50 “ (Tschirch.) 108 DESICCATION. 109 these being then placed on a framework, in chambers which are heated to the necessary temperature, which varies according to the nature of the substance. The arrangement of such chambers is very much the same as in the drying closet, the principle of which is shown in Fig. 172. Each shelf or partition is so placed, that the draught of dry or heated air passes over and around it, escap- ing above, loaded with moisture. In some cases, the air is first passed over burnt lime to remove all moisture, before passing into the drying chamber. Drying closets may be so arranged, as to utilize the waste heat from a stove-pipe, or by passing a steam-pipe through it. The vessels containing the burnt lime, should be placed in the bottom and on the different shelves. Thus arranged, the dry- ing closet may also be utilized for storing hygroscopic drugs and chemicals. Loss in Drying Drugs.*—The drying of drugs requires the greatest care and consideration, since many of them contain volatile and active principles, which are easily injured by the slightest degree of overheating, for example, conium leaf and fruit, aconite, etc. Aromatic drugs like cloves, nutmeg, cinnamon, car- damon, etc., are apt to suffer a loss of their volatile aromatic constituents to a greater or less degree; hence when several of these enter into a pharmaceutical preparation, it is best to grind the crude aromatics together to a powder, and not mix the several dried powders. Again, such drugs as asafoetida, myrrh, ammo- niac, suffer loss of volatile oil in the process of drying and reduc- tion to powder; hence, when powdered, they are unfit for dispensing or for the preparation of the “Mixtures.” In pre- paring Emulsum Asafoetidse, or Ammoniaci, or Mistura Ferri Composita, only selected tears of the several gum-resins should be employed. Fig. 172. Drying Closet (Sectional View). *The following drugs lose, on an average, by drying and powdering:— Acacia, 0.8 per cent. Ergota, 3.62 per cent. Aloe Socotrina, 11.2 " Gentiana, 10.23 “ Acidum Tartaricum, 1.06 “ Ipecacuanha, 1.91 “ Buchu, 2.00 “ Myrrha, 5.80 “ Cantharis, 2.05 “ Opium, 19.61 “ Cardamomum, 6.02 “ Podophyllum, 0.75 “ Cassia, 2.61 “ Rheum, 1.74 “ Cinchona Flava, 2.57 “ Scilla 13.60 “ “ Rubra, 1.58 “ Tragacantha, 6.93 “ Cubeba 2.40 “ Zingiber (alb.) 9.70 “ (Squibb.) 110 HANDBOOK OF PHARMACY. Every apothecary should employ the greatest care in the selec- tion of his powdered drugs, for the market is well provided with inert and adulterated material. Storage and, Preservation.—Considerable care must be observed in the storage of powdered vegetable drugs. They should be kept in a place not subject to marked changes of temperature, and should not be stored in hermetically sealed vessels and deprived of free access of air, but should be placed in tin canisters, the tops of which are slightly perforated, so as to admit the access of air, and yet to keep out dust and insects. Wooden boxes or drawers are not suitable, for they allow the accession of mites and dust, the drug rapidly losing what odor or aroma it may possess. For storing crude drugs or roots, barks and leaves, drawers may be constructed which are lined with tin, the lids being so placed that they can only be opened when the drawer is open; these drawers answer well for storing such powders as Gentian or Columbo. When exposed to the air, powdered drugs absorb moisture (1 to 20 per cent.), the amount depending on the hygroscopicity of the particular powder; those containing fixed or volatile oils being the least hygroscopic, while the largest amount of moisture is absorbed by mucilaginous drugs. In the course of Pharmaceutical Assaying, it is frequently neces- sary to dry small quantities of substances, in which case we employ the “ Drying Oven” (Fig. 173), which is usually made of copper and placed on a stand. A Bunsen lamp is placed below and, by regulating the flame, the temperature in the oven may be regulated; an opening above is for the insertion of a thermometer. These ovens are also constructed with double walls to admit filling with water, when the desired temperature should not rise above 100° C. For very high temperatures, iron ovens are employed. After the operation of dry- ing or ignition, it is necessary to allow the substance to cool in the “ Desiccator” to prevent absorption of moisture, before weighing. If the substance has been dried on a watch-glass, then another well-fitting watch-glass is inverted over it, and the two are held firmly together by means of a spring (Fig. 176), which prevents any possible loss of powder by spilling, and also prevents absorption of moisture during the weighing. Hot cruci- bles are placed on pipe-stem wire triangles in the desiccator. Fig. 173. Copper Drying Oven. DESICCATION. 111 Many bodies, owing to their low melting point, cannot be dried by heat, hence we place them in the desiccator over Fig. 174. Copper Drying Oven (Double Wall). Fig. 175. Fig. 176. Watch-glasses for Weighing Powders. Iron Drying Oven. Fig. 177. sulphuric acid, or calcium chlo- ride, etc., where they give up their moisture readily. Desiccators are of various forms. Fig. 177 illustrates one consist- ing of a bell-glass (b), with a ground rim fitting closely to the ground glass base. The vessel (c) contains the moisture- absorbing material; above this is a porcelain table (d), upon which the substance to be dried is placed. Fig. 178 illustrates a form of desiccator, designed by Hempel, the principle of which consists in placing the absorb- ing material (H2SO4) in the rim of the cover (a-y), above the Bell-glass Desiccator. 112 HANDBOOK OF PHARMACY. substance which is placed in the lower vessel A. The cover is provided with a tube and stopcock, which fits into the neck at B, Fig. 178. Hempel’s Desiccator. for connecting with a suction-pump if necessary to dry “in vacuo.” Fig. 179 illustrates another form, provided with a stopcock a, which may be placed in connection with a vacuum- pump and the air exhausted. The ground edges of the fittings should be greased with a little fat or petrolatum. As material for the absorption of mois- ture (water), for use in desiccators, we employ usually either sulphuric acid or granulated calcium chloride; besides these we may also employ either calcium oxide (burnt lime), fused caustic potash or soda, or phosphoric oxide (anhy- drous phosphoric acid). Drying Liquids.—For removing small amounts of water from such liquids as alcohol, ether, ethyl nitrite, chloroform, volatile oils, we employ fused calcium chloride, sharply-dried potassium carbon- ate, or anhydrous copper sulphate. Care should be taken not to employ any substance which may react chemically on the liquid to be dried, for instance, calcium chloride cannot be employed in drying wood alcohol, benzyl alcohol or many esters, because it unites with them, forming crystalline compounds. Absolute alcohol is prepared from ordinary alcohol, by percolating it Fig. 179. Vacuum Desiccator. DESICCATION. 113 through burnt lime, which effectually removes all but traces of water. Fig. 180. Gas Wash Bottles. Drying Gases.—For drying (washing) gases, we employ the various forms of “wash bottles” (Fig. 180), in which the gas Fig. 181. Fig. 182. Drying Tube (Chloride of Calcium). Drying Jar (Chloride of Cal- cium). passes through a layer of sulphuric acid; the tube through which the gas enters the flask, should dip from one-half to 114 HANDBOOK OF PHARMACY. three-quarters of an inch below the surface of the acid. For “washing gases,” water or other fluids are employed. Figs. 181, 182 illustrate another form, in which the gas is dried by passing through either a U tube, or upwards through a tower, filled with granulated calcium chloride. A wad of absorbent cotton or spun glass wool is placed in the neck (Fig. 182), upon which the granu- lated calcium chloride rests, and another layer is placed on top just beneath the cork. CHAPTER IX. COMMINUTION. The collection, drying, comminution and subsequent pulveri- zation of drugs is at present seldom, if ever, performed by the retail apothecary. This branch has fallen entirely into the hands of the drug-miller. Crude vegetable drugs are first Fig. 183. reduced to coarse particles by slicing or chopping, in order to facilitate their drying and subsequent pulverization. This is called “ Comminution.” The slicing is done by means of chop- Poulain’s Pulverizing Works. 115 116 HANDBOOK OF PHARMACY. ping knives or rolling circular blades operated by machinery. In this condition, the drug is dried and then subjected to the operation of bruising, called “ Contusion,” which in other words, is pulverization by simple impact. Fig. 183 shows the opera- tion of contusion in the row to the right; in the row on the left trituration is carried on. In these two processes the piece that raises the pestles is a cam whose axis is fixed upon the main shaft, which is actuated by a steam engine. In order to pre- vent lateral action in the contusion battery, the cams revolve in a rectilinear open- ing in the rod of the pestle, which is seen to the right of the engraving. The cam, which is a spiral, having the driving shaft as a starting point, is cut off short at 180°. On reaching this point, the wiper escapes and leaves the pestle to the action of gravity. In the trituration battery, figured on the left of the engraving, the pestles must in falling turn upon themselves. To this effect the cam rubs against a wiper in the form of a horizontal circular plate that communicates, by reason of the friction, a gyrating motion to the pestle. The different positions occupied by the cam during its revolution are shown in the illustration. In order to prevent particles from being ejected from the impact, as well as the diffusion of the dust, each mortar is covered with a leather jacket. As soon as the drug has been thoroughly bruised it is ready for grinding. GRINDING is the reduction to coarse particles in properly constructed mills. The drug-miller employs a variety of mills, for the purpose of grinding. Among these are the Chaser, Buhr-Stone, and Roller Mills, Disintegrators and other patent mills, each of which is adapted to special purposes. A Hand Drug-Mill that answers the purposes of the pharmacist, must be so constructed, that it may be adjusted for all kinds of general work. According to the arrangement of the grinding surfaces hand- mills may be divided into two classes. 1. Those in which the grinding plates are arranged vertically. 2. Those in which the grinding plates are arranged horizontally. In all of them, the grinding plates consist of teeth arranged in concentric rows, one plate fitting into the other; the distance be- tween the grinding surfaces being regulated by means of a thumb- screw, thereby regulating the degrees of fineness of the powder. 1. Hand Drug-Mills with Vertical Grinding Plates.—Among these are the Swift, Troemner, and Enterprise mills. The latter (Fig. 184), because of the simplicity of its construction, and the case with which it is handled and cleansed, has become very popular. In this mill, the grinding plates are supported on a horizontal shaft, which is turned by two heavy fly wheels. The shaft rests between two hemispheres, enabling the operator, after opening the mill, to remove all the working parts. The various parts can be readily removed and replaced in case of fracture. The left-hand grinding plate, being geared to the shaft, revolves, while the right- hand one is stationary. The fineness of the powder may be easily COMMINUTION. 117 regulated by means of a thumb-screw, which regulates the distance Fig. 184. between the plates. Various sizes are made, clown to the small dispensing counter-mill. 2. Hand Drug-Mills with Horizontal Grinding Plates.—An older form is the Thomas mill; later improvements are found in Swift’s B mill, in which the grinding plates are arranged horizontally, the upper one being stationary, wThile the lower one re- volves. It can be easily opened and cleaned, the main objection being its open receptacle for the powder. An embodiment of this same idea, but vastly improved, is the Hance conical-plate mill, in which the hori- zontal grinding surfaces are given a conical shape. The main feature of this mill is that the powder yielded is always uniformly fine and free from coarse particles, while the vertical- plate mills often allow these to drop through. The conical shape of the grinding plates, allows a ready dis- charge of the powder, thereby avoiding clogging up of the mill, Enterprise Drug-Mill. Fig. 185. Hance Drug-Mill (Cross Section). 118 HANDBOOK OF PHARMACY. which is very often the case in those having horizontal plates. This mill is adapted for all kinds of heavy and light work and can be readily taken apart for cleaning. The lower plate is of conical shape, capped with a beaker, and fits upon the upper end of the upright shaft, and revolves with it, engaging with the teeth in the upper grinding-plate and hopper. Power is transmitted by means of two shafts at right angles, geared with bevel cog- wheels. The fineness of the powder is regulated by a thumb- screw at the base, which elevates the revolving plate. The Following Precautions Must be Observed in Hand- ling Drug-Mills.—The mill, if not sufficiently heavy, should be securely bolted to a firm foundation ; otherwise much of the power exerted at the wheel will be lost. The bearings should be kept clean and lubricated. Fig. 186. Hance Drug-Mill (Showing Parts). The drug should be as dry as possible, otherwise the moist par- ticles will stick to the plates and cause clogging. In grinding coarse, bulky or fibrous drugs, they should first be reduced to coarse particles by bruising, then run through the mill several times, first with a very coarse adjustment, then after sifting off the fine particles, returned to the mill, after the plates have been readjusted. The procedure is continued until the whole is ground to the proper degree of fineness. The drug should not be fed into the hopper faster than it can be ground, otherwise clogging will ensue. Dry, brittle drugs, may be fed more rapidly than moist, oily ones. Very oily drugs are best ground coarse at first, the fine powder sifted off, and the tail- ings reground, etc. After each operation, the mill should be thoroughly cleansed, all particles adhering to the plates being removed. Should these COMMINUTION. 119 have become clogged with hard lumps, the latter should be removed with boiling water, and the plates well dried. In most cases the running through of sawdust will be sufficient. Is the reduction of substances into particles of greater or less tenuity. We perform this by the operations of contusion and grinding in the case of vegetable drugs; in others, such as resinous drugs, gums, chemicals, etc., by the process of pulverization. All bodies cannot be pulverized by one and the same process; this must be altered to suit the physical and chemical nature of the body to be pulverized. Certain precautions must be observed by PULVERIZATION Fig. 187. Pulverization of Corrosive or Poisonous Substances. the workmen in carrying on some of these operations, to prevent injury or painful affections. For instance, the dust arising from the powdering of belladonna is apt to injure the eyesight; that from cantharides acts as a vesicant; certain salts of mercury and all salts of arsenic are very poisonous, etc. Fig. 187 illustrates some of the precautionary measures adopted in such cases. Some bodies cannot be pulverized alone, that is, they require the addition of a foreign body which facilitates disintegration; this method of powdering is called “pulverization by mediation.” We employ intermediates in powdering camphor, for, owing to its elastic nature, we cannot powder it alone; hence we moisten it with alcohol or ether, whereby it disintegrates immediately. Rice is softened in water before being ground. Vanilla requires the 120 HANDBOOK OF PHARMACY. intervention of sugar or milk sugar crystals. Centrifugal force is used for the reduction of zinc to fine powder, the molten metal being poured on a horizontal revolving plate of iron, which turns at the rate of 2000 revolutions a minute. By this means, the zinc is projected against the sides of the box in which the disc is enclosed. For the fine subdivision of phosphorus, it is melted under water, and the latter then agitated until cool. Gold-, silver-, and bronze-leaf are powdered in the presence of honey or sulphate of potassium, which is afterward removed by washing. Nux vomica or ignatia, owing to their tough and horny structure, are first steamed, which causes them to swell and soften, after which they are rapidly dried, and then easily reduced to powder. For powdering resins and gums, some manufacturers employ casks or iron cylinders which revolve upon an axis, and in the interior of which iron balls roll about, crushing the substance. SIFTING Is the process of separating powders of different degrees of fine- ness by passing them through some perforated medium. For this purpose sieves are employed. These consist of a frame, usually circular, over which is stretched wire- (or iron- or brass-) gauze, or better hair-cloth or silk, held firmly in place by an outer rim. Drum sieves are cylindri- cal and covered at both ends. After sifting, a powder should always be thoroughly mixed, in order to insure uniform composi- tion of the product. When we operate upon larger quantities of powder, we have special appar- atus designed for this purpose. Among the various sifters, Hun- ter’s (Fig. 188) is one of the most effective. The powdered drug or mixed powders are thrown into the hopper above, then by means of brushes, which revolve against the curved brass sieve, the lumps are thoroughly disintegrated, and the powder is brushed through into the receptacle below, where it is further mixed by revolving spiral mixers. For pre- paring impalpable powders, bolting cloth is employed. Com- mercially, powders are known by numbers. The U. S. Phar- macopoeia directs the employment of various degrees of fineness, designating the degree by a number, which corresponds to the number of meshes to the linear inch ; the powders being num- bered from 20 to 80 inclusive. Fig. 188. Hunter’s Sifter and Mixer. COMMINUTION. 121 The British Pharmacopoeia directs the numbers from 20 to 80 inclusive, designating them by the number of meshes to the linear inch, as in the U. S. P., omitting, however, the metric equivalents. The German and Austrian Pharmacopoeias designate by the num- ber of meshes to the square centimeter. Tables of Degrees of Fineness of Powders, U. S. P. and B. P. Meshes to . Meshes to the No. Linear Inch. Centimeter. 80 Very fine powder 80 30 60 Fine 60 24 50 Moderately fine 50 20 40 Moderately coarse 40 16 20 Coarse 20 8 2Vb. Meshes to the Centimeter. Corresponding to U. S. P. 50 Impalpable powder 50 40 Exceedingly tine 40 30 Very fine 30 80 25 Fine 25 about 60 20 Moderately fine 20 50 15 Moderately coarse 15 about 40 8 Coarse 8 20 Degrees of Fineness of Ph. Ger. and Ph. Aus TRITURATION Is the reduction of substances to a minute state of subdivision by means of the mortar and pestle. The pestle should be grasped firmly, and, with a slight downward pressure, worked around the Fig. 189. Fig. 190. Trituration. Motion described by Pestle. bottom and sides of the mortar with a circular motion, gradually extending from the center outwards, as shown in Fig. 190. Then the motion should be reversed toward the center, in the same manner, and this procedure should be continued until the sub- stance is reduced to the desired degree of fineness. Mortars and Pestles.—For the pulverization of hard or tough 122 HANDBOOK OF PHARMACY. drugs, where considerable force is necessary, the iron or bronze mortar is employed (Fig. 191). The interior should be bell-shaped and not conical, otherwise the drug will become packed in the bottom, hindering proper disintegration. After use, they are best cleaned by triturating in them some clean sand. When they have been used for powdering chemicals, such as iron or sodium sulphate, they should be well washed and dried. Wedgwood-ware answers admirably for general use, because of its strength, though, owing to its somewhat porous nature, it is often difficult to cleanse. Again, the handle of the pestle being of wood, it is usually set into the base by means of a resin cement; it, therefore, readily loosens and drops some of the cement off, contaminating the substance that may be triturated. The handles should be reset before using, by heating until the cement softens, then filling the pestle hole with a fused mixture of 3 parts of Fig. 191. Iron Mortars. shellac, 1 of yellow wax and 1 of turpentine, pressing in firmly, holding until the wax has hardened. Handles are now made of hard rubber which screw firmly into the pestle. Porcelain mortars and pestles are preferred for general use in the preparation of solutions, emulsions, light triturating etc. They are much more easily cleansed than the Wedgwood ware, since their inner surface is not porous like that of the latter. Porcelain mortars will not stand hard blows nor rapid heating, because of their liability to fracture. Glass mortars (Fig. 195) should likewise be carefully handled, and should not be employed for triturating hard substances. They are best adapted for pulver- izing corrosive substances, chemicals, alkaloids, and for preparing solutions of the same. Their surface is smooth, and no loss of substance is liable to occur, as would be the case when using a Wedgwood mortar, whose surface is porous or uneven. COMMINUTION. 123 Agate mortars (Fig. 196) are only employed in pulverizing very hard substances, such as minerals or ores. In selecting mortars and pestles, the apothecary should use con- siderable discretion: For general purposes of trituration a shallow mortar (Fig. 193) should be selected. For the preparation of emulsions and solutions, a comparatively deep mortar (Fig. 194) should be used. The pestle should fit the mortar accurately; a Fig. 192. Fig. 193. Wedgwood Mortar. Porcelain Mortar (Shallow). round-surfaced pestle should be used for the deep, and a flat-sur- faced one for the shallow mortar. Every apothecary should have a full set of mortars and pestles, of various sizes and shapes, adapted for all sorts of operations. It should be made a rigid rule to clean these immediately after use. When the powdered substance has been of a resinous nature, its Fig. 195. Fig. 194. Fig. 196. Porcelain Mortar (Deep). Glass Mortar. Agate Mortar. traces are best removed by means of a little alcohol or benzin, and if it has been of an oily nature, the remaining particles may be removed with sawdust, and the mortar then washed out with soap and water. If the substance possessed a powerful odor, like that of iodoform, or the mixture has badly stained the mortar, triturate a little bichromate of potassium with sulphuric acid about the sides, rinsing out well with water. 124 HANDBOOK OF PHARMACY. A Spatula consists of a long, flexible blade of polished steel, somewhat heavier at the base, where it is usually covered on both sides with hard wood, serving as a handle. Spatulas are also made Fig. 197. Ointment Spatula. Fig. 200. Fig. 198. Pill Spatula. Fig. 199. Horn Spatulas. entirely of metal (nickel plated). The so-called Lawrence spatula is the best among these; the handle not being polished affords a good grip. The only objection to these, is that after being some time in use the plating is liable to wear off from the tip, exposing the surface of the steel beneath. Spatulas are employed in the process of trituration, for the removal of the particles of powder adhering to the sides of the mortar and pestle, also in all the various phases of dispensing pharmacy, such as the division of powders, preparation of ointments, etc. Steel spatulas are adapted for general use except for such purposes where the substance is affected by contact with iron, as in the preparation of ointments containing iodine, sali- cylic and tannic acids, mercuric chloride, and corrosive substances. In such cases we employ the horn or hard rubber spatula, the latter being of flexible steel covered with hard rubber. Horn and rubber spatulas should not be used for stirring hot liquids. Too much care cannot be paid to the cleansing and care of spatulas; they should always be bright and free from traces of Powder Spatula. COMMINUTION. 125 rust, as its presence may render many a preparation unsightly and unfit for use. Trituration may also be effected, by means of the slab and muller with the in- tervention of a liquid, the operation being called “ Levigation.” The s u b- stance, in coarse powder, is placed on a slab of glass, marble, or porphyry, having a ground surface, and moist- ened with water or alcohol to form a thick paste; it is then triturated by means of the muller, using slight pres- sure, and moving the mul- ler in curves such as shown in Fig. 201, a, b. A shallow porcelain mortar (Fig. 202) is often substituted for the slab, and a flat-surfaced pes- tle for the muller. In Euro- pean pharmacy this latter operation is designated as Levigation, and the former as Porphyrization. These processes have for their object the reduction of such substances as zinc Fig. 201. Porphyry Slab and Muller. Fig. 202. Levigating Mortar. oxide, or mercuric oxide, to a very fine state of subdivision, which is not attainable by the simple process of dry trituration. 126 HANDBOOK OF PHARMACY. Is the process of separating the finer particles of an insoluble powder from the coarser, by means of suspension in water. The pasty mass resulting from the process of levigation, is washed off into a beaker or other suitable vessel, and stirred with water; the mixture is then allowed to stand a minute or so, after which the supernatant turbid fluid is poured off into another beaker. The sediment which contains the coarser particles, is then again sub- jected to the process of levigation, and the same operation is re- peated until the whole quantity is elutriated. The turbid fluid, which has been decanted, is allowed to stand at rest until the minute particles of the substance held in suspension have sub- ELUTRIATION Fig. 203. Elutriation. sided ; this deposit is then collected and dried. Instead of pour- ing off (decanting) the turbid fluid as described above, we may employ a more expeditious method, illustrated in Fig. 203, in which, by means of a long funnel tube, water is forced in at the bottom of the cylinder, which, forcing its way upward through the powder, carries the particles of powder along with it, the finer particles being carried to the top, while the coarser remain near the bottom, from their own gravity. By opening different outlets on the sides powders of various degrees of fineness may be ob- tained. The process of elutriation is employed in separating the impurities from chalk and in the sorting of emery into different grades of fineness. COMMINUTION. 127 Consists in forming conical masses of levigated substances. Insoluble powders, such as chalk, bismuth salts, or bole, while still in a pasty condition, are placed into a tin cone (d, Fig. 204). This is then grasped by the handle (c), and the leg of the frame is tapped gently upon a slab of chalk-stone, or other absorbing surface, each tap causing a conical drop to fall out. The porous block absorbs the moisture quickly, after which the cones may be dried by heat, if necessary. TROCHISCATION Fig. 204. Mould for Levigated Chalk, Etc. CHAPTER X. SOLUTION. Solution is a “ molecular ” subdivision of a body (solid, liquid or gas), in a liquid {solvent), the result being a clear homogeneous fluid. If, on bringing a solid in contact with a liquid, the whole or a portion of the solid disappears, and a clear liquid results or can be separated from the mixture, then we say that the solid is wholly or partially soluble in the liquid. Formerly, the solution of a solid in a liquid, such as that of salt in water, was designated as “ simple ” or “ direct ” solution, and where a change in the chemical nature took place, as when bases were dissolved in acids, as “ indirect ” or “ chemical ” solution. Such a distinction is not necessary, and moreover incorrect, for we must consider, that “ solution ” in such a case is only apparent, there being new bodies of a different chemical constitution pro- duced, which, as such, are dissolved in the excess of the solvent. The chemical action which takes place first, has nothing to do with the phenomena of solution. The rate or ratio, according to which a substance is dissolved by any particular liquid, is called its “ solubility.” The solvent powers of a liquid for different bodies are very different. If none of the substance is taken up by the solvent, it is said to be “ in- solubleif comparatively little is dissolved, it is designated as “ difficulty ” or “ slightly soluble ” (example, calcium hydrate); when large amounts are taken up readily, as “ very soluble ” (example, potassium iodide). When a solvent has taken up as much of the substance as it is capable of at a certain temperature, it is said to be “saturated” If there be an insufficient amount of the body present, it will be entirely dissolved and an “ unsaturated ” solution will result. The solubility of a solid depends upon several conditions: 1st. The Nature of the Substance (form, density); hence we pul- verize bodies to facilitate contact with the solvent. 2d. The Nature of the Solvent. 3d. Temperature. 4th. Presence of other dissolved Solids. The Nature of the Substance must be considered. The solubility of a solid depends primarily upon its nature, for we find, for instance, that barium sulphate requires 250,000 parts of water for solution,* while on the other hand, sodium thiosulphate is soluble in all proportions in water (at 45° C.). * Silver bromide at 20° C., is soluble 1 in 1,971,650 parts of water. 128 SOLUTION. 129 The Nature of the Solvent plays a very important part in solution. We find the solvent powers of water entirely different from those of alcohol, ether or glycerin. The chief solvents employed in pharmacy are water, alcohol, glycerin, ether, chloroform, acids and oils. Water is a general solvent of wide application. It is employed in the preparation of the medicated waters, syrups, solutions (liquores), etc. When it is used in the preparation of silver solu- tions, eye-washes, hypodermic solutions, etc., it should be distilled and fulfill all the requirements of the Pharmacopoeia. Water dis- solves most inorganic salts; from vegetable drugs it dissolves gums, starch, sugar, neutral principles, certain alkaloids, tannins, extractive and many coloring matters. Alcohol is of the greatest importance pharmaceutically, because of its excellent solvent properties and the stability of the prepara- tions made with it. It is a solvent for resins, volatile oils, alka- loids, and neutral principles, while it does not take up such inert principles as starch and gummy matter. Glycerin.—The solvent properties of this lie between that of alcohol and water, and when added to either of these, it insures greater stability of the finished preparation. It dissolves tannin, starch, many inorganic salts, pepsin, organic acids, etc. (See Glycerites.) Ether dissolves principally fixed and volatile oils, fats, resins, and most alkaloids (not their salts). Chloroform, possesses about the same solvent properties as ether, but it has the advantage that it is not inflammable. Acids.—Acetic acid in a diluted form, is employed as a solvent in the preparation of the official vinegars. Glacial acetic acid and hydrochloric acid are solvents of many organic compounds. Oils are employed as solvents of gums and resins in the pre- paration of liniments. Effect of Temperature on Solubility.—Rise of temperature usually increases the solubility of a solid. In some cases, we find that the- solubility increases in a definite ratio with the temperature of the- solvent, for example, potassium chloride, barium chloride, or magnesium sulphate. In another class (the majority), we find the ratio of solubility to the temperature irregular. In a small num- ber of cases we find that the solubility steadily diminishes as the temperature rises, that is, the substance is more soluble in cold, than in hot water. As examples of this we have calcium hydrate, sodium chloride, strontium sulphate, calcium citrate, and paral- dehyde. The relationship of temperature to solubility is most clearly shown by the table of curves,* Fig. 205, where the lower line of figures express the degree of temperature, and the side figures, the quantity dissolved by 100 parts of the solvent. * Ostwald, “Outlines of Inorganic Chemistry,” p. 150. 130 HANDBOOK OF PHARMACY. In cooling a hot saturated solution, a portion of the dissolved body separates out in a solid (usually crystalline) form, while the remainder, according to its coefficient* of solubility for the given temperature, remains in solution. When bodies of differ- ent degrees of solubility are dissolved, the less soluble separate out first, while the more soluble remain in solution. The Presence of Dissolved Bodies in a solution often affects the solubility of other substances in this menstruum. Here we may distinguish several different cases:— 1st. The presence of one salt may increase the solubility of another. For instance, the presence of an alkaline chloride, such as sodium or ammonium chloride, increases the solubility of mer- curic chloride in water. Iodine is practically insoluble in water, but by the use of an alkaline iodide, we can cause water to take up large amounts of it (ex- ample, Lugol’s Solution). This is an example where it is pos- sible for us to form a saturated solution (KI), which is capable of taking up a further quantity of a second substance (I). 2d. The presence of one salt may diminish the solubil- ity of another. For example, we cannot dissolve potassium sulphate in a solution of am- monium sulphate, or potassium nitrate in a solution of ammo- nium nitrate. Potassium car- bonate is a very soluble salt, but it is insoluble in concen- trated water of ammonia. 3d. An alteration in the nature of the solvent may alter the solubility of the salt. The addition of alcohol to many saline solutions will cause the salt to be precipitated. For ex- ample, on adding alcohol to a saturated solution of ferrous sul- phate, the iron salt will be precipitated as a granular powder Condition of Contact of the Body with the Solvent.— We may facilitate the solution of solids by triturating or agitat ing them in powder form with the solvent; this facilitates the contact of the two, by continually exposing the surfaces of the particles of the powder to the contact of fresh portions of the solvent. This same principle is involved, when air or carbonic acid gas is passed rapidly through a mixture of the solid and fluid, for the purpose of producing brisk agitation. Circulatory Solution.—When the quantity of matter to be dissolved is large, and the time permits, we may suspend the Fig. 205. Table of Curves of Solubility for Nitrates. * Coefficient is a number, expressing a certain arithmetical ratio. “ Coefficient of solubility ” is the number expressing either how many parts of a salt, etc , are soluble in 100 parts of a solvent, or how many parts of a solvent are required to dissolve 1 part of a salt. SOLUTION. 131 substance, placed in a porous diaphragm (perforated funnel, sieve or muslin bag), just below the surface of the liquid solvent. A more or less saturated solution (resulting from the immediate contact of the solvent with particles of the solid), owing to its density, sinks to the bottom of the vessel, and its place is taken by fresh portions of the solvent displaced. This circulation con- tinues until the liquid becomes saturated. This same procedure applied to the extraction of soluble matter from vegetable drugs Fig. 206. Apparatus for Generation, Washing, and Solution of Gases. is known as “Circulatory Displacement,” and is employed in the preparation of infusions, tinctures (by maceration), etc. Supersaturated Solutions.—A hot saturated solution of Glauber’s salt (Na2SO4 + 10II2O), when proper care is taken to protect it from jarring and dust, may be cooled, and still remain liquid, notwithstanding the solution contains a larger amount of the salt than the coefficient of solubility for the lower tempera- ture allows. The slightest jar, or bringing it in contact with a solid body, causes its solidification at once. Such a solution is called “ supersaturated ” Solution of Gases.—Gases are usually more soluble in alcohol 132 HANDBOOK OF PHARMACY. than in water. The most easily condensible gases are the most soluble. The method of solution is the reverse of that usually employed in dissolving solids, that.is, the solvent is kept as cool as possible. Under like conditions of pressure and temperature, one and the same liquid does not absorb equal quantities of different gases. At a temperature of 0° C., and a pressure of 760 Mm., one volume of water dissolves the following volumes of gas Carbonic acid (carbon dioxide, CO2), 1.8 Sulphuretted hydrogen (H2S), 4.3 Sulphurous acid (sulphurous anhydride, SO2), 79.8 Hydrochloric acid (HC1), 503.0 Ammonia (NHS), 1050.0 Solutions of such gases as chlorine, sulphuretted hydrogen, sulphurous acid or ammonia, are often prepared by the apothe- cary. For the preparation of such solutions, the apparatus as shown in Fig. 206 may be employed. The gas is generated in the flask a, which is provided with a safety tuber; the gas passes out through d into the wash-bottle /, which contains a little water, for the purpose of retaining impurities; then it passes on through the tube i into the water contained in flask g. The tube dips just a little below the surface of the water which half fills the bottle, which is placed in a bath, A, of cold water. The neck of the bottle is loosely plugged with cotton to pre- vent the escape of gas. At short intervals the bottle is removed, its mouth closed with the ball of the thumb, or palm of the hand, and agitated until the unabsorbed gas is d issol ved. Th is proced ure is con- tinued until, after shaking, pressure on the hand is observed from escap- ing gas. A better method for the preparation of chlorine water is that of Liebig (Fig. 207), in which the current of gas (as soon as the air is removed from the apparatus), is passed into an inverted retort filled with water. As soon as some gas has collected over the surface of the water, it is shaken until dissolved; this is con- tinued until the water is saturated. This avoids the escape of odors into the room. The operation of shaking the excess of gas with the water or solvent, is not necessary in the case of such soluble gases as ammonia and sulphurous acid. In preparing solutions of these in water, care should be taken to keep up a steady current of gas, and when the operation is over, the receiver should be at once disconnected at the rubber joint e, before the lamp is removed from under the sand-bath />, because the vacuum created by the cessation of hot vapors would cause the contents Fig. 207. Preparation of Chlorine Water. SOLUTION. 133 of the wash bottle (/) and receiver (<?), to be separated back into the flask. Density of Solutions.—On bringing a salt or gas into solu- tion in a solvent, the specific gravity (density) of the liquid is generally increased. In most instances, this increase is in definite ratio to the amount of the body dissolved. The specific gravity of water being 1.000, if we dissolve five parts by weight of caustic soda in it, we will find the specific gravity to have risen to 1.059; if ten parts, to 1.115, etc. If we dissolve 31.9 parts of hydrochloric acid in water, the specific gravity will be 1.163. On the other hand, if we make a solution of ten per cent, of ammonia gas in water, we will find the specific gravity to be 0.960; and if one of 28 per cent., 0.901. The specific gravity of a solution, is a ready and fairly accurate means of determining the amount of dissolved salt or gas, when only one substance is present. Change in Volume by Solution.—Most salts, when dissolving in water cause contraction; where water of crystallization is taken up by the salt, the contraction is greater than in the case of salts having combined water. On diluting a concentrated solution, contraction takes place. Expansion of volume takes place when the dissolved solid contains a large amount of water of crystal- lization, or a decided rise of temperature takes place. For example, when we dissolve ferri sulphas exsiccatus or alumen exsiccatum in a measured volume of water, we find that a con- traction of volume results, since these salts have withdrawn respectively 7 or 24 molecules of water; on the other hand, if we dissolve the crystalline salts, we find an increase in volume, due to the throwing off of 7 or 24 molecules of water. On mix- ing absolute alcohol and water, a contraction of from three to four per cent, takes place, according to the proportions of the two ; it being greatest when 49.836 volumes of water are mixed with 53.939 volumes of absolute alcohol; at 15° C. the mixture meas- ures exactly 100 volumes, instead of 103.775. Freezing Mixtures.—The passage of bodies from the solid to the liquid state (or, of the solid or liquid to the gaseous), produces a consumption of energy, which is accompanied by a lowering of the temperature; hence in dissolving salts, particularly those which dissolve rapidly, a cold mixture results.* * FREEZING MIXTURES. If the liquids employed be first cooled, a greater diminution of temperature will take place. The Temperature is Lowered. On Mixing:— From To 8 pts. powd. Glauber’s Salt and 5 pts. Hydrochloric Acid, + 10° — 17° C. 1 pt. each of Ammonium Chloride, Potassium Nitrate and Water, . + 10° — 25° C. 1 pt. each of Ammonium Nitrate and Water, + 10° — 12° C. 2 pts. Snow and 1 pt. Salt, ..... 0° — 21° C. 9 pts. Sodium Phosphate and 4 pts. Dil. Nitric Acid, + 10° — 29° C. 1 pt. Snow and 1 pt. Dil. Sulphuric Acid, — 7° — 50° C. 7 pts. Snow and 10 pts. cryst. Calcium Chloride, 0° — 55° C. A mixture of Ether and solidified Carbon Dioxide, — 110° C. Pictet’s Fluid (liquefied mixture of SO2 and CO2), — 200° C. 134 HANDBOOK OF PHARMACY. Elevation of Temperature Due to Chemical Action.— In the process of solution, we find many instances where a con- siderable amount of heat is generated, as when dissolving anhy- drous caustic soda or potash or calcium chloride in water. From these solutions we can obtain the crystalline salts NaOH + 7H2O; KOH -|- 2H2O; CaCl2 + 6H2O. The enormous rise of temperature produced by the addition of sulphuric acid to water is also attribu- table to the fact, that chemical action has taken place, with the absorption of water of hydration. The mixing of 30 parts by weight of absolute alcohol with 70 parts of water causes a rise of temperature of 9.14 degrees, producing probably the hydrate C2H5OH.3H2O. In order to ascertain the solubility of a body, we have recourse to either one of two methods: 1st. Method of Digestion.—When we expose an excess of the powdered substance to the action of the solvent, during a period of from several hours to a day, at the desired temperature. We place the mixture of the two in a small flask or test-tube, which is placed in a bath kept at the desired temperature, and shaken at frequent intervals. After digestion has been continued sufficiently long, the entire mass (liquid and undissolved powder), is quickly drained on a small dry filter. The filtrate is collected in a tared beaker and weighed, then evaporated to dryness, cooled in a desic- cator, and again weighed. 2d. The Method of Cooling.—We heat the mixture of the solvent and substance, until a concentrated solution has been obtained at a temperature higher than that at which the determina- tion is to be made. This solution is then cooled to the desired temperature, and maintained at this point for some time, under addition of some crystals of the salt, and agitation. It is then filtered and treated as directed above. In applying either of the above methods to the determination of the solubility of a solid, in a volatile menstruum, it is best to employ a small flask with an inverted condenser (Fig. 151) to avoid loss of solvent. Then a sufficient quantity is filtered quickly into a stoppered weighing flask (Fig. 208), this is closed, allowed to cool and weighed. The volatile liquid is then evaporated off, and the weight of the dry residue determined. Care must be taken, that the proper temperature (at which the solubility is to be determined) is maintained for at least an hour before filtration. In carrying out the above, for crystalline salts, the evaporated solution must be dried at a temperature sufficiently high to drive off all water of crystalliza- tion, and the residue then weighed as anhydrous salt, but calculated back to crystalline when the results are estimated. DETERMINATION OF THE SOLUBILITY OF SUBSTANCES. Fig. 208. Weighing Bottle. SOLUTION. 135 Example: A saturated solution of potassium chlorate at 12° C., weighed 10.98 Gm.; when evaporated to dryness it gave 0.7025 Gm. residue. What was the amount dissolved? Let the weight of the saturated solution be taken as W, and the weight of the substance found therein dissolved, be w; then W — w will equal the weight of the water; we make the propor- tion (W — w) : w : : 100 : x or x = Substituting figures (W = 10.98; w = 0.7025) we have: W —w = 10.2775 the weight of water in the solution. Weight of water, Dry residue, rppen 10.2775 : 0.7025 : : 100 : X X = 6.83 That is 100 parts of water had dissolved 6.83 parts of potassium chlorate at 12° C. For convenience, solubilities are sometimes expressed by stating the amount of solvent required to dissolve one part of the solid. Then in this case it would be— Dry Weight of residue, solvent, as 6.83 : 100 : : 1 : X X = 14.64. That is, 14.64 parts of water held 1 part of potassium chlorate in solution at 12° C. AN APPARATUS (“LYSIMETER”) FOR DETERMINING SOLUBILITIES. In determining the solubility of a substance in some liquid at a given temperature, there is usually but little difficulty encoun- tered, when the solvent is not very volatile and the temperature at which the determination is to be made is not high. With a highly volatile solvent, and a high temperature, however, certain difficulties present themselves which are liable to lead to error. The main difficulty is encountered in the endeavor to separate from the original solution, which usually contains an excess of the substance in suspension, a filtered portion at the same tem- perature as that of the solution. The higher this temperature is, the more difficult becomes the removal of a portion without the introduction of errors by the ordinary methods of filtration. It appears, therefore, that it is only necessary to modify the method of filtration in such a way as to maintain the temperature of the original solution unchanged in order to eliminate these errors. This may be easily accomplished by upward filtration into a tube placed in the original solution, and so constructed that it will enable the operator to control the act of filtration, as well as accurately to determine the amount of solvent and dissolved material. For this purpose the little apparatus here described has been found very serviceable. 136 HANDBOOK OF PHARMACY. The apparatus consists of a glass tube, a, 15 centimeters long, and one centimeter in external diameter, provided at one end with a well-ground stopper, c, while the other end is cup-shaped, there being a contracted neck between the cup and the main tube. Into this cup is made to fit a carefully ground glass bell, e, having a small perfora- tion in its bottom (as shown in /). There is also a stopper, b, which is carefully ground to fit into the cup, and which is inserted after the glass bell, e, has been removed. The several stoppers, etc., are all numbered, to show where they belong. To show how the apparatus is used, it will be best to quote a practical example. Let us assume that the solubility of mor- phine in boiling alcohol is to be determined. It will be necessary to provide for such an amount of liquid that at least one-half of the glass tube, a, may be immersed in the liquid. In the case of comparatively cheap solvents and substances to be dissolved, beaker glasses may be used; for more expensive materials test-tubes of such a size that there will be no great waste of material are preferable. The glass tube is made ready by inserting the stopper, c, and introducing into the cup- shaped end the glass bell, e, containing a pellet of purified cotton and prevented from dropping out by a thin platinum wire fast- ened around the contracted neck and crossed over the mouth of the bell. A sufficient amount of alcohol having been introduced into a beaker or test-tube, heat is applied and morphine added, until, after the boiling has been kept up some time, a portion of the alkaloid remains undissolved. The prepared glass tube is now inserted in the liquid. As long as the stopper, c, closes the mouth of the tube, no liquid will be able to filter upwards. When the tube has acquired the temperature of the boiling liquid the stopper, c, is removed, whereupon the liquid will begin to filter through the pellet of cotton and rise in the tube as far as the quantity of liquid will permit. In order to insure perfect uniformity of the liquid within and without the tube, it is best to allow the filtered portion to flow back through Fig. 209, The Lysimeter.* *This apparatus was devised by Dr. Charles Rice of New York City. The description as given was published in the Journal of Amer. Chem. Society, Oct., 1894. SOLUTION. 137 the pellet of cotton once or several times. The stopper, c, having then been inserted, the tube is withdrawn, turned upside down, the glass ball removed, and the stopper, d, inserted. The tube is now carefully cleaned with alcohol, and laid aside until cold. Its tare having previously been determined, the increase in weight represents the weight of the solution contained therein. On transferring or washing the contents into a fared beaker or capsule, and evaporating, the weight of the dissolved morphine will be found. PERCENTAGE SOLUTIONS. It must be distinctly understood, that percentage by weight means that all ingredients must be weighed, and percentage by volume, that all ingredients must be measured. A 1 per cent, solution of cocaine hydrochlorate contains 1 part by weight of the salt, and 99 parts by weight of water; a 2 per cent, solution con- tains 2 parts by weight of salt, and 98 parts by weight of water. The word part may stand for a grain, or gramme, or ounce, or any unit. To make a fluidounce of a 1 per cent, solution we first need to know the weight of a fluidounce of w’ater, at the temperature at which we desire to make our solution. We find that a fluidounce (of 480 minims) of water at 15.5° C. weighs 455.7 grains, hence 1 per cent, of this would be 4.55 + grains. Subtracting this from 455.7, we obtain 451.2 + grains. Consequently, we dissolve 4.5 grains of cocaine hydrochlorate, in 451.2 grains of water at this temperature.. If we desire to make one fluidounce of an alcoholic solution of cocaine hydrochlorate, we must first find the weight of 1 fluidounce of alcohol. If we use U. S. P. alcohol of specific gravity 0.820, then 455.7 times 0.820 gives us 373.6 -j-,the weight of 1 fluidounce of this alcohol, in grains; then we proceed as above. To prepare a pint of a 1 in 1000 solution of cocaine hydrochlorate, divide 7,291 (grains in 1 pint of water) by 1000; this gives the number of grains (7.29) of the salt per pint, and sufficient water must be added to make the product weigh 7,291 grains. In these calculations, 1 grain of the salt was assumed to occupy the same space as 1 minim of water, which is not exactly the case,* hence a solution prepared as above, will measure two or three minims less than a fiuidounce. For all practical purposes how- ever, this is near enough, but when an exact volume (say exactly 1 fluidounce) is desired, it is best to make a quantity, a little in excess, and then to throw away what is not needed or to dispose of it otherwise. Many physicians in prescribing solutions under- stand percentage by measure, i. e., grains of a solid to the flui- drachm or fluidounce, or milligrammes to the cubic centimeter; this is weight for measure and not percentage. For convenience * Jour. Chem. Soc., 1892, page 766. 138 HANDBOOK OF PHARMACY. in dispensing, the table of Puckner or that of Loudenbeck are useful.* RULES AND EXAMPLES FOR DILUTION AND FORTIFICATION. In applying these rules, percentage by volume or weight may be used; the two must not be confounded or mixed in carrying out the calculations. Alcohol is selected as illustration; but in place of this, such liquids as ammonia water, hydrochloric or acetic acid, or any others may be selected. For further study of this subject the reader is referred to Oldberg’s “ Pharmaceutical Problems and Exercises,” from which these examples are selected. Rule I.—To find the quantity of water required to be added to alcohol of any given percentage strength, to dilute it to any other percentage strength desired :—Divide the per cent, strength of the al- cohol to be diluted (a) by the percentage desired (b\ and subtract 1 from the quotient; the remainder is the number of parts of water (z) to be added to each part of the alcohol used to produce the result desired. a i — 1 — x. b Example.—We have a 90 per cent, alcohol to be diluted to 60 per cent.:— 90 — = 1.50; and 1.50—1 = 0.50. 60 ’ Therefore: f pound of water is to be added to 1 pound of the 90 per cent, alcohol to reduce it to 60 per cent. Rule II.—To make a definite quantity, by weight, of alcohol of any given percentage strength from any stronger alcohol:— Multiply the required quantity (a) by the desired per cent. (6) and di- vide by the per cent, strength of the stronger alcohol used (c); the quotient is the weight of stronger alcohol required (d) to be diluted with water; and the difference between that weight (d) and the weight of the diluted alcohol desired (a), is the weight of water (e) necessary for the dilution. a = d; and a — d = e. c For each fluidounce of water take of the salt— For each fluidounce of water take of the salt— To make: Grains: To make: Grains: 1 per cent., 4.597 1 in 1000, . . 0.456 2 per cent., 9.289 1 in 500, . . 0.912 3 per cent., 14.078 1 in 400, . . 1.141 4 per cent., 18.906 1 in 300, . . 1.522 5 per cent., 23.957 1 in 200, . . 2.290 10 per cent., 50.576 1 in 100, . . 4.597 15 per cent., 80.327 1 in 50, . . 9 289 20 per cent., 113.797 1 in 25, . . 18.966 25 per cent., 151.730 1 in 20, . 50.576 40 per cent., 303.460 1 in 5, . . —The 113.797 Apothecary, Feb. 1892,10-13. *Using pure water at 22° C. (71.6° F.), 1 fluidounce weighing 455.19 grains. SOLUTION. 139 Example.—6 pounds of 60 per cent, alcohol is to be made from an alcohol of 90 per cent, strength :— 6X60 . , o o —— = 4 ; and 6 — 4 =2. 90 ALLIGATION. Rule I.—To find the value of any mixture of known quanti- ties of ingredients, each of known value:—Multiply the quantity of each ingredient by its value and add the several products; divide the sum by the sum of the quantities of the several ingredients ; the quo- tient is the value of the whole mixture. Example.—We mix 3 pounds of 80 per cent, alcohol, 8 pounds of 91 per cent, alcohol, 5 pounds of 45.5 per cent, alcohol, 6 pounds of 40 per cent, alcohol, and 8 pounds of water; what will be the alcoholic percentage strength of the mixture ? 3 x 80 = 240. 8 X 91 = 728. 5 X 45.5 = 227.5 6 X 40 = 240. 8X 0 30 1435.5 and 1-4j%5- = 47.85 per cent. Rule II.—To find the proportional quantities of ingredients of known value required to produce a given mean value :—JJrite the numbers expressing the units of value of the respective ingredients in a column to the right, and the mean sought, to the left; link together the numbers expressing the respective values of any two ingredients, one of which is above and the other below the mean value sought; take the difference between the mean and the value of each ingredient, and placethat difference opposite the value of the other ingredient to which it is linked; the differences are the proportions required of the ingre- dients opposite whose values they are placed. Thus:— Example.—Five substances of different value are to be mixed so as to yield a product of the mean value of 14. The value of the several substances are: 9, 12, 13, 16, and 18. How much of each substance will have to be taken ? r 9 2 =18 12. 4 =48 14 131 2 =26 l16J 14-5 =96 18 J 2 =36 11 4- 5 = 16) 224 ( 14 16 64 64 The first ingredient, having a value of 9 (which is a value below 14), is linked to the fourth ingredient, having the value of 16 (which 140 HANDBOOK OF PHARMACY. is above 14). The second ingredient, with the value of 12, is linked to the fifth, with the value of 18; and the third ingredient, having a value of 13, is linked to the fourth in the same manner. As the difference between 13 and 14 is 1, we place the number 1 opposite 16, to which the 13 is linked ; and as the difference between 14 and 16 is 2, we place the number 2 opposite the 13 to which the 16 is linked. Then taking another pair, we put the number 4 opposite 12, because 12 is linked to 18, and the difference between 14 and 18 is 4; and opposite 18, which is linked to the 12, we put the number 2, which is the difference between 14 and 12. One more pair now remains, viz.: that of 9 and 16. Opposite 9 we put the number 2, because 2 is the difference between 14 and 16, to which 9 is linked; and opposite 16 we put the number 5 (in addition to the number 1 already placed opposite 16), because 5 is the difference between 14 and 9. Now we add together the numbers set opposite the ingredients, which are 11 + 5, making the total 16 parts. In other words, we must use 2 parts of the ingredient represented by 9; 4 parts of the ingredient having the value of 12 ; 2 parts of the third ingredient; 1 + 5, or 6 parts of the fourth ingredient, and 2 parts of the fifth, making 16 parts in all, and we will find that this mixture will have a mean value of 14. CHAPTER XI. DIFFUSION-DIALYSIS. Diffusion is the mutual permeating of two or more liquids or gases, or an intermixture of the molecules of liquids of different density ; it is of the same nature as solution. As to their diffusive powers through water, liquids differ widely; fixed oils do not, volatile oils slightly, while syrups, glycerin, alcohol, crystalline salts, etc., readily diffuse in every proportion. If water is poured carefully upon a layer of sulphuric acid, the two form distinct layers, but, on standing they gradually intermix, that is, they diffuse into one another. The same may be said of saline solu- tions and various other liquids. They all differ from one another, however, in the rapidity with which they diffuse; solutions of such substances as starch, dextrin, gum, albumen, glue, etc., dif- fuse exceedingly slowly, if at all. Graham, considering gelatin as a type of this latter class, has proposed to call them colloids (xoUtj, glue), to distinguish them from the far more easily diffu- sible crystalloid substances. Graham proposed a method of separating bodies based on their unequal diffusibility, which he called dialysis. Dialysis is the diffusion between liquids modified by the inter- position of an animal or vegetable membrane. It is the process of separation of crystalline from non-crystalline or colloidal sub- stances by the interposition of a membrane. This membrane, whether of bladder or parchment-paper, possesses an infinite number of minute pores (capillary tubes), by means of which the liquids are brought in contact with each other and “ diffuse.” This is called osmosis. A dialyser consists of a ring of hard rubber or other suitable material, over one end of which was stretched, while wet, a sheet of parchment paper or a piece of bladder, thus forming a vessel about two inches deep and about ten inches in diameter. Into this vessel is poured the mixed solution to be dialysed, and the whole floated in another vessel containing water (Fig. 210). Glass vessels may be used in making the dialyser, as shown in Fig. 211, but because of its weight, the dialyser should be supported to the proper depth in the water. The mixture in the dialyser should not be over one-half of an inch deep on the diaphragm. A bladder filled to about two-thirds with the mixture and suspended in a jar of distilled water, answers just as well. If the mixture placed in the dialyser (floating vessel), consists of crystalloid and colloid matter, it will be found, after a period of from several hours to a day or so, that only the colloids remain in the dialyser, while the crystalloids have diffused through the membrane into the dis- tilled wrater of the outer vessel. This solution is called the diffusate. 141 142 HANDBOOK OF PHARMACY. The process of dialysis is employed by the chemist as well as the pharmacist. The toxicologist separates such poisons as arsenic, antimony, lead, alkaloids, etc., from the contents of a stomach, by placing the material in the dialyser, which is suspended in acid- ulated distilled water; these poisons, being crystalloids, readily Fig. 210. Dialyser. diffuse through the membrane and are identified in the diffusate. The pharmacist may purify salicylic acid by a process of dialysis, or may separate many crystalline organic bodies from their impu- rities. We can remove in this manner the crystalline active constituents from the prepara- tions of such drugs as opium, aconite, belladonna, etc. B. F. McIntyre of New York intro- duced a class of preparations called Dialysates, based on this idea, whereby the active con- stituents were removed from the inert matter in the various drugs. Thus far we have learned that the diffusate contains the material we seek, while that left on the dialyser is discarded. In the case of Dialysed Iron, how- ever, it is just the reverse, the colloid matter left on the dia- lyser being the material aimed at, while the crystalloids (am- monium chloride and ferric chloride) with any free acid pass into the diffusate, and are thrown away. Fig. 211. Dialyser. CHAPTER XII. CRYSTALLIZATION. Generally speaking, bodies,' in passing from the liquid or vaporous condition to the solid state, assume regular geometric forms. Such regular forms, bounded by plane faces and definite angles, are called crystals. The phenomenon of formation is called crystallizing. We define bodies which are capable of assuming this form, as crystallizable (as quartz, alum, etc.), and those which have assumed it, as crystalline. Such bodies as do not conform to the above, that is, do not crystallize, are called amor- phous (as chalk, glue, etc.). When a body is freshly broken, we often observe the fractured surfaces to exhibit a crystalline struc- ture. This is sometimes called “ crystalline fracture ” (as marble, alabaster, etc.). The plane surfaces which bound a crystal are called faces or planes. The intersection of two adjacent faces (planes) forms an edge. When two or more lines or planes intersect, their edges form an angle. In order to classify and compare the various forms of crystals, we must have some simple method of expressing the relative position and inclination of their planes. This is done by referring them to certain systems of axes. These axes (Figs. 212, 218, 222, etc.), are called crystallographic axes; they are imaginary lines, which, if drawn through, would intersect at the centre of the crystal. The position of the different faces (planes) of the crystal are fixed by, and expressed in, the relative lengths of their intercepts on these axes. For the purpose of comparing the different crystal planes, systems of symbols have been devised, which aim to locate the position of each plane, with reference to its relation to the crystallographic axes.* Since every crystalline body has its own peculiar crystal form, it will be readily seen that we have an immense number of these in all possible varieties. However, in the face of this, according to their greater or less degree of symmetry, they are divided into six different classes or systems. Each one of these systems has its imaginary crystallographic axis to which the different planes (faces) bear a fixed symmetrical position. According to the relative position, number and size of these different planes, we distinguish the following six different systems. 1. Regular system. 2. Tetragonal system. 3. Hexagonal system. *For different systems see Williams’ “ Elements of Crystallography.” 143 144 HANDBOOK OF PHARMACY. 4. Rhombic system. 5. Monoclinic system. 6. Triclinic system. 1st. The Regular (monometric, isometric, tesseral) System. All forms have three. axes of equal length, which intersect at angles of 90° (Fig. 212). The fundamental form of this system, from which all others are most easily de- rived, is the regular octahedron (or octohedron) (Fig. 213), with eight equilateral faces (crystal form of the alums). If the six octahedral angles be truncated, we have the crystal form of potassium chloride (Fig. 214). Imagine square truncations on the octahedral angles ; then we have the six-sided hexahedron (cube), the crystal form of potassium iodide and sodium chloride (Fig. 215). By the truncation of the twelve octahedral angles, we obtain, according to the size of the new faces, the form (Fig. 216), and the rhombic dodecahedron (Fig. 217), the crystal form of phosphorus, boracite, etc. In a similar manner, the various other forms of this system are ob- tained. 2d. The Tetragonal (dimetric, quadratic, pyramidal) System has <Aree axes, which Fig. 212. Fig. 213. Fig. 214. Fig. 215. Fig. 216. Fig. 217. Regular or Isometric System. intersect at angles of 90°, two of these (lateral) being of equal length, the other (prin- cipal axis), being either longer or shorter. The fundamental form of this system is the tetragonal pyramid (Figs. 219, 221). By truncating the horizontal angles, we obtain the square pyramid (Figs. 223, 224), the crystal form of tin stone. By the truncation of the upper and lower angles of the tetragonal pyramid, we obtain the crystal form of potassium ferrocyanide (Fig. 220). 3d. The Hexagonal (rhombohedric) System has four axes. The number of equal axes (lateral) are three, intersecting the principal axis at angles of 90°, and each other, at angles of 60°. The fourth or principal axis is of greater or lesser length (Fig. 222). The fundamental form, is the double hexagonal pyramid (Fig. 225), bounded by twelve similar scalene triangles, from which, the forms of the hexagonal prism, closed by the basal pinacoid (Fig. 227), or by a pyramid (Fig. 226), are derived. In this system we find quartz, iceland-spar, arsenic, bismuth, antimony, sodium nitrate, etc. 4th. The Rhombic (orthorhombic, prismatic, trimetric) System has three axes of unequal length, all intersecting at right angles (Fig. 228). The fundamental form is the rhombic octahedron (Fig. 229), bounded by eight congruent scalene triangles. CJR YSTA LLIZA TION. 145 To this series belong sulphur, saltpeter, magnesia, zinc sulphate, tartar-emetic, citric acid, etc. Fig. 218. Fig. 221. Fig. 223. Fig. 224. Fig. 219. Fig. 222. Fig. 225. Fig. 220. Tetragonal and Hexagonal Systems. 5th. The Monoclinic (oblique, monosymmetric, prismatic) System has three axes of unequal length, two of which intersect at an oblique angle, being perpendicular to Fig. 226. Fig. 227. Fig. 228. Fig. 229. Rhombic or Ortho-rhombic System. the third (Fig. 230). The fundamental form of this is the monoclinic octahedron (Fig. 231), bounded by eight scalene triangles of two different forms ; one set of 146 HANDBOOK OF PHARMACY. which has a degree of inclination toward the axes different from that of the other. The most frequent and characteristic form of this system is the monoclinic prism Fig. 230. Fig. 231. Fig. 232. Monoclinic System. (Fig. 232). To this system belongs sulphur (fused), sodium sulphate, ferrous sulphate, cane sugar, oxalic acid, tartaric acid, etc. 6th. The Triclinic (asymmetric) System has three axes of unequal length, all oblique to one another (Fig. 233). The most common form is the triclinic octahedron, all of the upper or lower faces of which have a different degree of inclina- tion toward the three axes. To this system belong copper sulphate, potassium bichromate, etc. When a body crystallizes in two or more forms, belonging to different sys- tems, it is said to be polymorphous. When of two forms it is called dimor- for example ; sulphur crystal- lizes in the rhombic and monoclinic systems. When the body crystallizes in three forms, belonging to different systems, it is said to be trimorphous, for example, titanic acid is found in three forms, as rutile, brookite and anatas. Different bodies having the same crystal form are designated as isomorphous. Chemically analogous compounds, which have the same crystal form, have the power of crystallizing in variable proportion with one another, also to exchange their constituents. In the case of ordinary alum (A12(SO4)3 + K2SO4 + 24H2O) the bases may be replaced by Fe, - Cr, - Mn, - or K, - NH4, - Rb, - Cs, respectively, without a change in their crystal form. A crystal of ordinary alum, when suspended in a solution of chrome- alum, grows as though it were in its own solution. This is explained by the similar atomic and molecular structure of the isomorphous bodies. The terms prismatic and acicular are often applied to long pointed crystals, and tabular to those crystallizing in flat plates. Although not used in crystallography, these three terms are very common and convenient, since they describe the general outward appearance of the crystal, without complicating matters with Fig. 233. Fig. 234. Triclinic System. CR YSTA L LIZA TION. 147 technical terms. The determination of the crystalline form, that is of the system and stereometric form, to which a crystal may belong, is often a very difficult matter, involving a knowledge of cleavage, the use of the polarizer, refractometer, goniometer, etc.; hence the reader is referred to the various text-books on Miner- alogy and Crystallography.* The different conditions under which crystallization takes place are the following:— 1st. Crystallization through the cooling of vapors; that is subli- mation, which happens only in the case of volatile solids, such as calomel, benzoic acid, iodine, corrosive sublimate,etc. 2d. Crystallization through the cooling of fused masses. Exam- ples are sulphur, antimony or bismuth ; the beautiful crystalline sulphides of nature, as those of iron, antimony, etc. 3d. Crystallization through deposition from solutions. This may take place under either of the two following condi- tions : a, By the spontaneous evaporation of concentrated solu- tions at a uniform temperature, b, By the slow cooling of a hot supersaturated solution. 4th. By precipitation, as the result of chemical interaction or alteration of menstruum. 1st. Crystallization through Sublimation (see Sublimation). 2d. Crystallization through Fusion and Partial Cooling.—To obtain these substances in a crystalline form, they should be fused in a deep vessel (Hessian crucible), and when sufficiently cooled, the crust which forms over the surface is pierced and the melted material drained off; on examining the interior, the sides will be found covered with crystals. 3d. Crystallization through Deposition from Solutions.—The object of crystallization is that of purification, for when we obtain a body in well-defined crystals, this is a proof that it is practically pure. This method of purification is now sometimes applied to the purification of such liquids as chloroform, acetic ether, glycerin, phenol, etc.; these, on being exposed to an extremely low temperature, crystallize, thus enabling us to separate the non- crystallizable impurities (Pictet’s patent). (a) In order to carry on crystallization successfully, we must observe certain precautions: First, that the solution be perfectly clear and free from mechanical impurities. Second, that it be brought to the proper degree of concentration,for upon this depends the size and character of the crystals. In order to obtain large and well-defined crystals, i t is best to subject the solution to slow “ spon- taneous evaporation.” This is employed particularly in cases where the salt is very soluble, as in potassium bromide and iodide; here the solution, after being brought to the proper degree of con- centration, is set aside in a dry place of uniform temperature. ♦Williams’ “Elements of Crystallography,” Tsehermack's, also Dana’s “ Mineralogy,” etc. 148 HANDBOOK OF PHARMACY. Should variations of temperature take place, a portion of the salt, having crystallized out at a lower, would be again dissolved at a higher temperature. The proper degree of concentration, requires a consideration of the nature and solubility of the substance. If it is very soluble,a boiling saturated solution should not be made, otherwise we would obtain a granular mass. The proper degree of concentration is always determined beforehand by experiment on smaller quanti- ties. When the body is not very soluble, the solution is evapor- ated until a pellicle or crust forms over the surface, and then set aside. Manufacturers are guided by the density and quantity of the solution, in conjunction with the temperature of the air. It must not be forgotten that the quantity of the solution determines largely the size of the crystals. (6) The method of crystallizing by slowly cooling hot supersaturated solutions, is employed largely in the crystallization of organic bodies. In dissolving these, we employ besides water, such solvents as alcohol, ether, chloroform, benzol, benzin, petroleum, hydrochloric and acetic acids. Each solvent has its own peculiari- ties and applications. When we employ this method, we dissolve the body in the hot solvent, so as to produce as concentrated a solution as possible. This is best accomplished by adding the solvent by degrees to the dry substance, until just enough has been added to dissolve it at a boiling temperature. The solution is then set aside and allowed to cool slowly so that crystals may deposit. The slower the rate of cooling, the larger and better defined are the crystals. For this reason, we often allow the vessel to cool in a bath of hot water. The evaporation of saline solutions is carried on in shallow vessels. Volatile solutions are placed in deep vessels; these are then set aside in a warm place and left undisturbed. The slight- est jarring hinders the formation of large crystals. For this reason, the hot saturated solution of Epsom salt is stirred while cooling. This prevents the formation of large rhombic prisms, and produces in their stead, small needles. Sometimes these saturated solutions refuse to crystallize. This is overcome by the introduction of rough or angular bodies, or by rubbing the sides of the vessel with the stirring rod, or by introducing a few crystals of the substance which is in solution. Strings or thin sticks of wood are often placed in the crystallizing vats, which, by their rough surfaces, offer points of adhesion, attracting the nuclei and facilitating the deposition of crystals around them; this accounts for the long cylindrical masses, in which we receive milk sugar, rock candy, tartar emetic, prussiate of potash, copper sulphate, etc. The liquid remaining after crystallization is called the “ mother liquor.” This, on further concentration, yields another crop of crystals called the “ second crystallization,” which are, however, CR YSTA LLIZA TION. 149 not as pure as the first. Thus, cane-sugar crystallizes from its first solution in pure white crystals ; the mother liquor on further concentration yields a second crop of a yellowish cast; still further, we obtain crystals of a brown color. That this brown color is simply due to mechanical impurities, is shown by the fact that, by repeated crystallizations {recrystallization), the body can be obtained of a pure white color. If more than one body be present in a solution, ami their solu- bilities differ, they may be readily separated; for the least soluble crystallizes out first, and so on in the order of their solubility, the most soluble last. This method of separation is called “fractional crystallization.” Some substances are insoluble in the usual solvents; hence saline solutions must be employed. Thus, mercuric iodide may be obtained in beautiful prisms by crystallizing it from a solution of common salt; this is called “intermediate crystallization.” Fig. 235. Fig. 236. Growing Crystals. Every crystal has a hypothetical center point; around this, the formation takes place with development of the different faces and planes. It is rare to find all the faces of a crystal fully developed. Crystals with deficient faces may be developed by “growing” that is, by suspending them by a thread in a concentrated solu- tion of the salt, or laying them on the bottom of the vessel, with the deficient face up (Figs. 235, 236). Certain substances do not crystallize, but when concentrated and spread out on glass in thin layers they dry, forming thin transparent scales. These are often mistaken for crystals. As examples of these scale compounds we have pepsin, citrate or tartrate of iron, etc. 4th. Formation of Crystals by Precipitation or Chemical Inter- action.—This can scarcely be considered, from the standpoint of inorganic chemistry, as a method of crystallization, inasmuch as the product obtained is thrown out of solution by mechanical or chemical means, usually yielding precipitates of a granular nature (see Precipitation, Granulation). In crystallizing many organic 150 HANDBOOK OF PHARMACY. compounds, it is necessary to alter the menstruum after solution has been effected. For instance, let us assume that we have an organic body which is extremely soluble in alcohol, and only partly soluble or insoluble in ether. Now in order to facilitate crystallization, we may add a little ether to the alcoholic solution, thus producing a sufficient alteration in the solvent power of the menstruum, to facilitate the formation and deposition of crystals. Crystallization, as the result of chemical interaction, is often brought about by bringing together solutions of different sub- stances. For example, on bringing together two inorganic bodies, we have the following:— 2NH4C1 ,+ Ptci4 = (NH4)2PtCl4 Ammonium Chloride. Platinic Chloride. Ammonium Platino- Chloride. On bringing together an organic and inorganic body we have the following:— CSHJ + KSCN = CS = N —C3H5 + KI Allyl Iodide. Potassium Allyl-Sulphocyanate Potassium Sulphocyanate. (Oil of Mustard). Iodide. When it is desired to crystallize small amounts of substances, from an aqueous solution, it is best to place the crystallizing Fig. 237. Fig. 238. Draining Crystals. Crystallizing Vessel, vessel in a desiccator, which facilitates the spontaneous evapora- tion of the solvent. After crystallization has taken place, the vessel is inclined, to facilitate the draining off of the mother liquor (Fig. 237). After this, the crystals are thrown into a funnel (stopped with cotton or glass wool) and the remaining mother liquor allowed to drain off. This draining may sometimes be facilitated by pouring over the mass some liquid in which the crystals are not soluble. We occasionally use alcohol for this purpose, in the case of certain inorganic salts. The crystals are finally dried by laying them between the folds of filter paper or on porous tiling. When the crystals are small, forming a granular mass, they are best freed from mother liquor by throwing the entire mass on a perforated porcelain plate, in a funnel, and draining off by suction (see page 182). Large quantities of crystals are drained by placing CJi YSTA LLIZA TION. 151 them in the centrifugal machine (see page 214). Since no pres- sure is here employed, the structure of the finest crystalline mass is not injured. EFFECT OF THE SOLVENT ON CRYSTALLIZATION. Here we must distinguish between several cases: 1st. The solvent takes no part, either physically or chemically, in the crystallization. Thus ammonium chloride, potassium iodide, and potassium sulphate crystallize from their aqueous solutions free from water of crystallization. 2d. The solvent takes part in the formation of the crystals, in furnishing crystal water. Thus in the formation of ferrous or cupric sulphate, or of sodium carbonate, water of crystallization is withdrawn from the water present. We have examples of such salts which crystallize with different proportions of water. Sodium carbonate is capable of crystallizing with one, five, eight or ten molecules of water. Glauber’s salt crystallizes with ten molecules of water of crystallization from a cold solution, and from hot water with seven molecules, or in an anhydrous condition, accord- ing to the temperature. Again such organic substances as alka- loids and glucosides, may crystallize out from different solvents, in crystals of different form, each form being characteristic of the solvent. Such salts give up their water of crystallization readily; and many, such as sodium carbonate, ferrous sulphate, etc., give up a portion of their wrater on exposure to the air (see Efflorescence). 3d. The solvent plays a chemical and physical part in the crystallization. When water enters into the chemical consti- tution of the crystal, it is called “ water of constitution,” while, when it merely serves for the formation of the crystal it is called “water of crystallization.” The water of constitution is not lost by mere efflorescence, but only after subjecting the salt to pro- longed high temperature. In many crystals, particularly those of the tesseral system, water is mechanically enclosed during the formation of the crystal, and is called “ interstitial water.” Such crystals, on heating, decre- pitate, from the explosive force of the minute water sacs, as they rupture the crystal. As examples of these we have potassium chlorate and nitrate. CHAPTER XIII. GRANULATION. Granulation is disturbed crystallization. We resort to this pro- cess to obtain many salts in a convenient form for dispensing. It also often adds to their general elegant appearance. For many salts this is a process of purification. The solutions of very soluble salts, such as potassium carbonate or citrate, or sodium salicylate, are rapidly concentrated, and then slowly evaporated to dryness on a water bath with constant stirring, which causes the salt to separate in a granular form. Ammonium chloride is thus granulated, having first undergone purification by the addi- tion of water of ammonia to its boiling solution, and subsequent filtration. When evaporating a solution to dryness for the pur- pose of obtaining a granular salt, care must be taken, that the powder does not cake on the bottom of the dish. Potassium chlo- rate and ferrous sulphate are granulated by constantly stirring their supersaturated solutions, while rapidly cooling. The former is soluble in 1.7 parts, and the latter in 0.3 parts of boiling water, while in cold water, the former is soluble in 16.7 parts while the latter is soluble in 1.8 parts. Ferrous sulphate, because of its greater solubility in cold water, is more conveniently granulated by filtering its concentrated solution into alcohol, in which it is insoluble. These granulated or granular salts should be thoroughly dried before being introduced in bottles. GRANULAR EFFERVESCENT SALTS. These are prepared by thoroughly mixing dry medicated pow- ders with dry tartaric acid and sodium bicarbonate, then moist- ening the mixture with alcohol (or any menstruum which is not a solvent of the constituents), to form an adherent mass. This is then forced through a sieve and the granules dried quickly in a current of dry hot air, or placed in a hot drying closet. It may then be sorted into different sized granules by sifting. These products should be kept in hermetically sealed bottles. 152 CHAPTER XIV. EXSICCATION. Exsiccation consists in depriving crystalline salts of their water of crystallization. Such salts as contain a large amount of crystal water, as potassium alum (45.5 per cent.), sodium carbonate (62.9 per cent.) and ferrous sulphate (38.8 per cent.) are exsiccated for the purpose of reducing their bulk, thereby increasing their com- parative strength. This is particularly evident in preparing pills which may contain any of the above, for, by using the dried salts we reduce the difficulty of making, as well as the size of the pills. In preparing these exsiccated salts, we should first allow them to effloresce in a warm place, after which, they are subjected to a strong heat under constant stirring (they melt in their own crystal water), until free from water; when cold, the mass is powdered and placed in dry bottles. These anhydrous salts, when dissolved in water, may be made, by evaporating their solutions, to assume their original crystalline condition. 153 CHAPTER XV. DELIQUESCENCE AND EFFLORESCENCE. Deliquescence is the property, possessed by many salts, of ab- sorbing moisture from the air. Such substances should be kept in well closed bottles in a dry place. Efflorescence is the property possessed by many salts when they are exposed to the air, of gradually giving up their water of crystallization and becoming dry and powdery on the surface. DELIQUESCENT SALTS OR SUBSTANCES. Acidum Chromicum. Ammonii lodidum. “ Nitras. “ Valerianas. Aurii et Sodii Chloridum. Caffeina Citrata. Calcii Bromidum. “ Chloridum. Chloral. Ferri Chloridum. “ et Quininae Citras. Hyoscyaminae Hydrobromas. ‘ • Sulphas. Lithii Bromidum. “ Citras. “ Sal icy las. Magnesii Citras Granulatus. Pepsinum. Pilocarpiuae Hydrochloras. Physostigminae Sulphas. Potassa. ‘ ‘ cum Calce. Potassii Acetas. “ Carbonas. “ Citras. “ Cyanidum. “ Hypophosphis. “ Sulphis. Soda. Sodii Hypophosphis. ‘ ‘ lodidum. “ Nitris. Sparteinae Sulphas. Stroutii Bromidum. “ lodidum. Zinci Bromidum. “ Chloridum. “ lodidum. All granular effervescent salts. EFFLORESCENT SALTS. Aciduni Citricum. Cadmii Sulphas. Codeina. Cupri Acetas. “ Sulphas. Ferri et Ammonii Sulphas. Ferri Sulphas. Magnesii Sulphas. Plumbi Acetas. Potassii Ferrocyanidum. Quinine Salts. Sodii Arsenas. ‘ ‘ Acetas. “ Benzoas. “ Boras “ Hyposulphis. ‘ ‘ Carbonas. “ Phosphas “ Sulphas. Strychnine Salts. Zinci Acetas. “ Sulphas. Acidum Hydrocyanicum undergoes decomposition, depositing a black precipitate which may be prevented by the addition of a little hydrochloric acid. EFFECTS OF THE EXPOSURE OF CHEMICALS TO LIGHT AND AIR. 154 DELIQUESCENCE AND EFFLORESCENCE. 155 Acidum Nitrohydrochloricum decomposes, losing chlornitrous acid ; it should be kept only in small quantity, in partly filled bottles in a dark place. Acidum Sulphuricum rapidly absorbs moisture. Acidum Sulphurosum oxidizes to sulphuric acid. Ammonii Carbonas loses NH3 and C02, and becomes bicar- bonate. Apomorphinae Hydrochloras turns green, indicating partial de- composition. Aqua Chlori decomposes with formation of hydrochloric acid and oxygen. Calx Chlorata loses chlorine, absorbing CO2. Calx Sulphurata loses sulphuretted hydrogen, changing to sulphate. Chloral as well as Camphor are slowly volatilized. Iodides or bromides of arsenic, ammonium, iron, mercury (ous and ic), sodium, strontium, sulphur, and zinc, lose iodine or bromine, respectively. Magnesia (calcined) absorbs CO2 and becomes carbonate. Magnesii Sulphis oxidizes to sulphate. Morphinse Acetas loses acetic acid. Napthalinum slowly volatilizes. Oleatum Hydrargyri, u. s. p., deposits metallic mercury. Physostigmine salts turn red. Potassa Sulphurata forms carbonate, hyposulphite, and sulphate. Resorcin becomes colored. Silver salts are all decomposed by light in presence of organic matter. Sodii Bisulphis loses sulphurous acid. Santoninum turns yellow on exposure to light. Zinci Acetas loses water and acetic acid. Zinci Phosphidum oxidizes, losing phosphorus. CHAPTER XVI. PRECIPITATION. Precipitation is a process, by which one or more substances which have previously been in a state of solution, are caused to separate out in an insoluble form. The substance which sepa- rates out is called the “precipitate-” the clear liquid above, the “ supernatant ” liquid; the substance added, the “precipitant-” and the process, “ precipitation.” Most precipitates fall to the bottom of the vessel, because they have a higher specific gravity than the remaining liquid. Those which are light, rise (for instance, Pepsin), and some may remain suspended throughout the liquid for a long time. The various causes which bring about precipitation, are :— 1st. Change of Temperature.—By boiling a solution of albumen or lime water, we cause precipitation (see pages 129, 184). If we cool a hot saturated solution of potassium chlorate, a precipitation or separation of a portion of the salt takes place. Changes of tem- perature often cause precipitation to take place in Fluid Extracts (see page 269). 2d. Change in Menstruum.—Any substance in solution is pre- cipitated on the addition of a miscible fluid in which it may be insoluble. Such inorganic salts as ferric and cupric sulphate are precipitated from their aqueous solutions on the addition of alcohol. Alcoholic solutions of resinous substances, on addition of water, separate their resin. Ether precipitates sugar from alco- holic solution. Chlorides of sodium and barium are precipitated from their concentrated aqueous solutions, upon the addition of concentrated hydrochloric acid. 3d. Chemical Interchange.—When the precipitant added pro- duces a chemical change among the substances in solution, the result depends on the insolubility of a new compound formed, as when sulphuric acid is added to a solution of barium chloride, which causes the production of insoluble barium sulphate. The addition of soluble potassium iodide to a solution of lead acetate, produces insoluble lead iodide. If the solutions are cold, the pre- cipitate is amorphous; if hot, crystalline. This form of precipitation is applied in analytical operations, as well as in the manufacture of many chemicals. 4th. Light.—This causes precipitation in the solutions of many silver compounds in the presence of organic matter etc., also to some extent in some pharmaceutical preparations, as in some Fluid Extracts, etc. 156 PRECIPITATION. 157 Precipitation may have for its object: 1st. To obtain the substance in as fine a powder as possible. Examples: Precipitated chalk or magnesium carbonate. 2d. To remove impurities. Iron is removed from calcium chloride by precipitation with calcium hydrate; from zinc chlo- ride solution by precipitation with zinc oxide. An impure sodium acetate is freed from sulphuric acid by the careful addi- tion of barium acetate, etc. 3d. To obtain new chemical compounds; for instance lead iodide and mercuric iodide, ammoniated mercury, bismuth sub- carbonate and subnitrate, etc. 4th. The qualitative and quantitative determination of sub- stances. In analytical chemistry, we identify and separate the various groups by means of different precipitating reagents. We also ascertain the quantitative composition of different bodies, by the precipitation and subsequent weighing of the various con- stituents. As to their appearance, precipitates are designated as: Crystalline — produced, for instance, by the cooling of hot satur- ated solutions of salts. Amorphous — produced, for instance, by precipitation of ferric chloride by alkalies. Granular — produced, for instance, by addition of alcohol to a concentrated aqueous solution of ferrous sulphate. Curdy — produced, for instance, by addition of hydro- chloric acid to a solution of silver nitrate. Flocculent — produced, for instance, by precipitation of albu- men with alcohol. Gelatinous — produced, for instance, by addition of collodion to carbolic acid. Magma —is a pasty mass resulting from the straining or fil- tering of an amorphous precipitate retaining water mechanically. Examples, ferric hy- drate, aluminum hydrate. Hot, dense solutions, yield dense precipitates. Cold, dilute solutions, yield light (diffusible) and often crystal- line precipitates. Dense precipitates are more easily washed, for they subside readily and admit of being washed by decantation. Crystalline Precipitates.—In many operations, we aim to obtain the precipitated body in a so-called crystalline condition, for the purpose of facilitating its separation and subsequent purification. For example, we cause calcium carbonate (precipitated chalk) and barium sulphate to be precipitated from hot solutions. This causes these compounds to form dense and crystalline precipitates, which are then easily removed and purified. 158 HANDBOOK OF PHARMACY. On mixing cold solutions, the precipitate formed will usually be crystalline and of greater purity; the solutions should be mixed slowly and with constant stirring. The precipitate will be denser, if it is allowed to stand at least twenty-four hours in the liquid. Example: On adding cold “ magnesia mixture ” to a cold, weak solution of a phosphate, a crystalline precipitate will gradu- ally form, consisting of the double salt ammonium-magnesium phosphate. Light magnesia (MgO) is made from the light car- bonate, which is made by reaction between cold solutions of sodium carbonate and magnesium sulphate. Heavy magnesia is made from the heavy parbonate, which is made by reaction between hot solutions of sodium carbonate and magnesium sulphate. Amorphous Precipitates.—Amorphous precipitates (for instance, hydroxides or sulphides of the metals), are denser and separate more rapidly from saline solutions; for instance, when ammonium sulphydrate produces in solutions of ferrous salts only a green color of ferrous sulphide, the addition of ammonium chloride causes its immediate separation. In order to obtain the hydroxides of aluminum (A12(OH)6) and iron (Fe2(OH)6), the precipitation must take place in the cold, and in very dilute solutions, in order to insure a finely subdivided pre- cipitate. Amorphous precipitates are much more easily washed in this finely subdivided condition. Moreover, in the case of the two examples quoted, precipitation must be effected in the cold, in order to obtain the precipitates in the hydrated condition and not as oxyhydrates (hot solutions). Upon these two conditions de- pends the solubility of ferric hydrate in solutions of the organic acids (preparation of scale salts). In quantitative analysis many precipitates (metallic sulphides, hydroxides, etc.) are thrown down from boiling solutions, in order to render them as dense as possible. This will also cause them to settle rapidly, so that they may be washed by decantation; also this facilitates the solution of the soluble salt (impurity) formed by the reaction, which must afterward be removed by washing. The order in which these solutions are added to one another, de- termines largely the purity of the product, and the ease with which it is afterwards washed. Hence, we should add the solution of ferric chloride to the diluted ammonia water, otherwise oxy- chlorides may be formed. In preparing yellow oxide of mercury, we pour the solution of mercuric chloride into the solution of potassa, for if the operation is reversed we obtain red oxychloride of mercury. In analytical operations we should add, for instance, the barium solution to the solution of the sulphate or sulphuric acid, other- wise some of the barium salt may be carried down with the pre- cipitated barium sulphate. The nature of the precipitate depends on the conditions under which the two solutions come in contact, that is, which of the two PRECIPITATION. 159 remains longest in excess. If we pour a solution of mercuric chloride into a solution of potassium iodide, so that the latter remains in excess, the solution remains clear, because as long as the latter remains in excess the mercuric iodide is dissolved as fast as formed. If wre reverse the order, having the mercuric chloride in excess, the mercuric iodide is likewise dissolved. It is only by a careful regulation of the proportions that success is obtained. Fractional Precipitation has for its object the purification of sub- stances by partial precipitation. For this purpose the precipitant is added only in small portions at a time, each precipitate being removed, before a further portion of the precipitant is added. In these different fractions, the substance may be found in different degrees of purity. Thus carbolic acid is separated from the empyreumatic resins which accompany it, by adding to its alka- line solution an acid, in small portions at a time, the first precipi- Fig. 239. Fig. 240. Precipitating Jar. Beaker Glasses (nest). tations consisting of these resinous impurities, while the later ones contain the acid in pure form. We may thus separate salicylic acid from its inert isomers by fractional precipitation with silver nitrate. In carrying on precipitation, it is necessary that the liquid be constantly stirred during the addition of the precipitant; this is for the purpose of facilitating the contact of the substances dis- solved in the liquids, also to prevent the precipitate from forming lumps, which might enclose particles of the substance yet unacted upon. With the exception of some operations in analytical chemistry, it is always advisable that both solutions be well diluted before mixing. In direct precipitation, the precipitant is added until no further precipitation takes place. This may be ascertained by allowing 160 HANDBOOK OF PHARMACY. the precipitate to settle away from near the surface and then add- ing to the clear supernatant liquid a drop or two of the precipi- tant, which should not produce any further turbidity. Precipitation is carried on, in small operations, in deep beaker glasses (Fig. 239), or in the so-called “ precipitating jar” (Fig. 240), the latter being a deep, heavy glass vessel, broad at the bottom and narrow at the top. This enables the precipitate to settle over a larger area of surface, thus assisting the operations of washing and decantation. On the large scale earthenware jars are usually employed, in which the supernatant liquid may be drawn off by means of spigots placed at different heights; wooden tanks are also constructed upon the same principle. CHAPTER XVII. DECANTATION. Decantation is the act of removing the supernatant liquid from a precipitate or sediment.* We usually resort to decantation in removing the clear supernatant liquid from a precipitate which may be deposited by tinctures or fluid extracts on standing. It is an expeditious and accurate method of separating soluble from insoluble matter, when conducted with due care. Decanta- tion is employed in the process of Elutriation, where the lighter are separated from the heavier particles of matter, the former being suspended in the upper layers of the mixture. By “ decantation with washing,” is understood the removal of soluble from insoluble matter in precipitates, by the repeated affusion and withdrawal of water. It is employed in those cases where a large quantity of a heavy, insoluble precipitate is to be washed, requiring, necessarily, a large amount of water. The precipitate is first allowed to settle; the supernatant liquid, after it lias become clear, is drawn off; then hot or cold water is poured upon the precipitate, with thorough stirring. It is again allowed to settle and treated as before; this oper- ation is continued, until all foreign soluble matter is removed. In decanting off the supernatant fluid, it is necessary to use the guid- ing rod (Fig. 241), other- wise, owing to adhesion, the liquid will run down the side of the vessel (Fig. 242). If due care is taken, not a drop of the liquid need be lost. When the form of the vessel, or the quantity of the liquid, admits pouring Fig. 241. Decantation with Guiding-rod. * A Sediment consists of solid matter, which is deposited by force of gravity, from solutions (in which it was suspended) on standing. A Precipitate consists of solid matter (amorphous or crystalline), which separates from a solution, as the immediate result of a reaction, be it heat, light or chemical influence. 161 162 HANDBOOK OF PHARMACY. off without a guiding rod, the outside of the lip or edge of the vessel should be slightly greased; this prevents the adhesion of the liquid, and its running down outside. Decantation may be more expeditiously and thor- oughly effected by means of the siphon (Figs. 244, 245). This is a glass tube, bent at an angle of about 60°, or bent at two right angles, having one of the limbs longer than the other. It is first started by filling it with fluid, while in- verted like a A; then the longer extremity being tightly closed with the finger, the shorter end is immersed in the liquid, with the longer arm extending outside, below the level of the liquid. On removing the finger, the flow of liquid commences. By lowering the inner, shorter arm, the liquid may be almost entirely drained off. Fig. 246 illustrates a form well adapted to siphoning off volatile or Fig. 242. Careless Decantation. Fig. 243. Decanting over Greased Rim. caustic liquids; the siphon a, b, is fitted tightly through the cork k, through which also a mouth-piece, c, extends to just below DECANTATION. 163 the cork. By blowing air in at c, the liquid is forced out through the siphon, which may be raised or lowered, according to the height of the precipitate. The same principle is applied in Fig. 244. Fig. 245. Decanting with Siphon. drawing off acids, in which the air may be forced in, by means of a rubber bulb. Fig. 247 illustrates another form of siphon which can be started by suction without danger or accident. The finger is Fig. 246. Fig. 247. Siphon Apparatus. Siphons with Suction Tubes, placed over the end of the long limb, or the stop-cock tem- porarily turned off, and suction applied at the mouth-piece of the curved lateral tube, until the current is started. 164 HANDBOOK OF PHARMACY. In analytical operations, we usually wash precipitates first by decantation, pouring the decanted liquid through the plain filter, to avoid any possible loss of substance, then by means of the tip of a feather (Fig. 248), or a small glass rod tipped with a small piece of rubber-tubing, any particles of the precipitate that may be adhering to the sides of the beaker, are brushed down, and the entire mass carefully trans- Fig. 248. Fig. 249. Rinsing Out Precipitates. ferred to the filter, the beaker being several times rinsed with boiling (or cold) water, the feather or tipped rod being used to remove any adhering particles. The precipitate is further washed, dried or ignited, and then weighed. Pipettes.—For removing small quanti- ties of a supernatant liquid from pre- cipitates, where the amount is not suffi- cient for siphoning, decantation is very difficult without entailing loss; hence we employ the pipette (Fig. 249). This consists of a long glass tube of small diameter, near the middle of which is usually blown a globular or elongated bulb, the lower tip being tapered out to a small opening. The tip of this is in- serted into the liquid to be drawn off, and by suction, it is drawn up into the bulb; when filled, the upper end is quickly closed with the finger, or if a rubber tube be used (Fig. 297), closed by pinching. Fig. 250, illustrates a suction ar- rangement which can be applied to any pipette; this consists of a glass tube (closed at one end), which fits closely, yet slides easily over the stem of the pipette; an air-tight joint is formed by a short piece of rubber tubing, which fits over the extremities of the outer tube and the stem of the pipette, then by raising or Pipettes, DECANTATION. 165 lowering this outer tube, the liquid may be drawn up into, or discharged from the pipette. Pipettes are also graduated for the purpose of draining off measured quantities of fluids. Wash Bottle or Spritz Bottle.—In the various operations of rins- ing and washing of precipitates, the “ wash or spritz flask ” is employed. This consists of a flat-bottomed flask (Fig. 251) fitted with a rubber stopper, having two holes, through which pass two glass tubes. The tube a, extending slightly below the cork, is the mouth-piece for forcing in the air, and this is tipped with a piece of rubber tubing. The tube b, d, is for the ejection of water. The tip b is drawn out to a point, to allow the passage of a fine stream of water; this tip is connected with the Fig. 250. Fig. 251. Suction Arrangement for Pipettes. Wash or Spritz Flask. main tube c, by means of a short piece of rubber tubing at /, which arrangement enables the operator to direct the stream of water in any direction, without altering the position of the flask. Around the neck at e is wound heavy cord, to enable the operator to handle the flask when hot. If a continuous stream of water is desired, the flow is started by blowing through the mouth-piece; then the latter is quickly closed by forcing the thumb against the end of the tube a. Automatic or Continuous Washing of Precipitates.—For this pur- pose there are a number of contrivances, answering also for the 166 HANDBOOK OF PHARMACY. continuous filtration of large quantities of liquids. Fig. 252 illustrates a convenient form, in which the flask containing the wash-water is inverted over the funnel. Through the perforated cork of the flask extend two bent tubes (Fig. 253). The end b must reach higher than cord; and d must extend farther than c. When placed over a funnel, the tip a should reach below the sur- face of liquid. As soon as the level falls below a, air enters at b, which admits a fresh supply of water until the end of the tube a is again immersed. Another form is that devised by Gay-Lussac (Fig. 254). Instead Fig. 252. Fig. 254. Fig. 253. Automatic Filtering and Washing Apparatus. of a bottle having two necks as illustrated, a single-necked bottle may be used as well. Through a tightly fitting cork two tubes are inserted, one of which is short and straight and serves as air tube, while the other (siphon) is bent so that one arm extends below the level of the bottom of the bottle, the tip (at a) being curved upward. Through c air is blown until the liquid rises in the funnel, above the mouth of the tube a. When the tube 6, a, is once filled, the siphon supplies the filter mechanically, for as DECANTATION. 167 soon as the level falls below a, air is admitted through the tube c and causes the funnel to fill again. An arrangement as shown in Fig. 255 answers well for the filtration of, or washing with, volatile liquids. In this, the bottle, Fig. 255. Automatic Filtration of Volatile Liquids. A, must be of such size as to fit well over the top of the funnel, the neck extending down some distance. The funnel, T, (with filter) is placed over the bottle, and then without separating the two, the funnel is placed into the neck of the receiving flask, B. The cord, /, serves to allow space for the escape of air. CHAPTER XVIII. COLATION. Colation or straining is the process of rapidly separating pre- cipitates and all kinds of suspended matter from fluids, by means of pouring them upon a cloth or other porous fabric. We employ this method, for the separation of mechanical impurities of all kinds, particularly in those cases where rapid filtration is required, and where the solid particles to be removed are not very finely divided, or the amount of precipitate is very large. For this purpose we employ as filtering media, felt, flannel, cotton flannel, muslin, gauze, etc. The felt strainer being made of wool, is in the form of seamless conical bags; it forms an excellent strainer for oils, melted fats, honey, etc. Inasmuch as they are difficult to cleanse they should always be em- ployed for straining the same mate- rial. In place of this, the woolen flannel strainer answers just as well; when over-seamed, they last a long time, and have the advantage that they are more easily cleansed; they are suspended from frames as shown in Fig. 256. While straining syrup or honey, the strainer should be hung in a warm place free from draughts. Canton or cotton flannel and muslin form the cheapest materials, and are most generally employed. Before Fig. 256. Fig. 257. Straining Bag. Strainer Frame. using them, they should be well washed in boiling water, to re- move any soluble matter that may have been used in calendering 168 COLATION. 169 These strainers are then suspended from the corners of the strainer frame (Fig. 257) which may be supported by a clamp, or placed directly over a vessel. After most of the liquid has drained through, and if the amount of precipitate is large, the strainer should be removed from the frame by gathering it in along the sides, as shown in Fig. 258, and then the retained liquid should be forced out by a twisting motion. When the amount of sus- Fig. 258. Fig. 259. Forcible Straining. pended matter is small, filtration through absorbent cotton an- swers all purposes. Each strainer or straining material should always be moistened before it is used. Should the fluid which first passes through not be perfectly clear, it should be returned to the strainer until the precipitate has filled the meshes of the cloth, when the liquid will flow through clear. If a clear liquid cannot be obtained in this manner, the strained liquid must subsequently be filtered through paper or other suitable medium. CHAPTER XIX. FILTRATION. Filtration is the process of depriving liquids of solid or sus- pended matter, by passing them through some porous medium, which allows only the passage of the fluid ; the clear, transparent liquid which flows through is called the “ filtrate.” For filtering purposes, we employ filter-paper, absorbent cotton, asbestos, spun and ground glass, charcoal, etc. When filtration is applied to viscous liquids, such as syrups, mucilage, honey, etc., for the pur- pose of removing mechanical impurities, it is called straining. When we separate a heavy precipitate from a fluid, with which it is mixed, by draining through muslin, we call the process eolation. Filter Paper.—This consists of unsized paper of loose texture, which is to be had either in square or circular sheets. It is an essential requisite, from a pharamaceutical point of view, that the filter paper used should be prepared from clean materials.* For this reason as well as another presently to be mentioned, the gray filter paper, which is the cheapest in the market, should not be used for filtering pharmaceutical preparations. This sort of paper almost always contains iron, lead, lime, starch and coloring matter, the presence of which at once precludes its use for filter- ing solutions of sensitive chemicals, such as iodide of iron, hydrio- dic acid, iodine, etc. Aside from the color imparted by gray paper to preparations which are filtered when hot (for instance, magnesium citrate solution), they also acquire a disagreeable taste, due to the presence of organic impurities contained in the paper. For all purposes, the white paper of the various standard brands f (German, Swedish, French) should be used. A thick paper of compact texture will be found to give the best satisfac- tion in most cases. The different makers prepare a great variety of filter-papers adapted to all kinds of work. There is filter- paper of a dense close texture for removing fine suspended matter; * According to Dr. Lardier, the gray filter paper usually employed, is made from cast-off rags of the filthiest sort, without any previous disinfection. It therefore contains enormous quantities of bac- teria, which are apt to pass into the filtrate, and are capable of converting medicinal preparations into “ culture fluids ” for myriads of these organisms. + The most suitable paper for general pharmaceutical purposes is Schleicher and Schiill’s Nos. 595, 597 and 598. The 595 is a light, while the 597 and 598 are heavy papers; the first of these is best adapted for filtering tinctures, spirits, etc., while the latter two are more suitable for the rapid and clear filtration of denser fluids. For filtering syrups, fruit-juices, oils of all kinds, etc., a paper of thick, loose texture is necessary ; this will be found in Nos. 584, 586 or 591 ; the larger sizes of these are sold with parchment ized points, so as not to break under the pressure of a heavy column of liquid. For quantitative purposes (£. e. quantitative analysis), Schleicher and Schiill’s 589, and 590, or Munk- tell’s No. 1 Swedish, or the Prat-Dumas French filter paper are the best. Messrs. Schleicher and Schull prepare a hardened filter paper (No. 575) which possesses even in a damp state, a hardness and durability which almost equals parchment. This is specially adapted for pressure filtration, also for the collection or removal of moist precipitates. 170 FILTRATION. 171 paper of loose texture for the rapid filtration and removal of coarser particles; then paper of such a texture as to admit the easy filtration of syrups and oils. A very useful toughened filter paper is to be had in the market, which is made by drawing ordinary white filter paper through nitric acid (sp. gr. 1.42), and then immediately washing with water. The paper shrinks somewhat and can be washed and rubbed, just like linen, without losing its filtering properties. Another form of filter paper is that in which linen threads are interwoven throughout, thus strengthening the tissue and pre- venting its rupture, which often occurs with the ordinary filter paper, when the operator pours a quantity of liquid too suddenly into the filter. For analytical purposes, it is necessary to select a paper that will not only retain the finest suspended matter, but which will also, when burned, yield the smallest possible amount of ash. In view of this, it is necessary that the paper be of a very close texture and yet not impede filtration; further, it is necessary that not more than traces of inorganic matter be present. These inorganic constituents (silica, alumina, oxides of iron and calcium) are always present in ordinary white filtering paper, but may be removed therefrom by washing with a diluted mixture of hydrochloric and hydrofluoric acids. Plain and Folded Filters.—In pharmaceutical and chemical operations we employ both the “plain ” and the “folded ” filter. Each form has its specific uses. The Plain Filter is employed in all operations where a precipi- tate is to be collected or subjected to washing. The filter is made by folding the square piece S (Fig. 260) along a-Z>, forming the triangle T (Fig. 261), which is again folded along the dotted line forming the triangle U (Fig. 262), this is rounded by cutting along cj-h (in round filter paper not necessary), it is then laid open in conical form as shown in Fig. 263. A still better method is to fold the sheet along a-b, as shown in Fig. 265, then along e-f (Fig. 266), forming thereby a square, as shown in Fig. 267, this is then rounded by cutting, as shown in Fig. 262. Then by holding it in position with the finger, it is well moistened with water or alcohol, according to the nature of the liquid to be filtered, and by gently patting with the finger, the filter is made to fit the sides of the funnel closely. This precaution must be observed, particularly in analytical operations, to avoid the risk of washing particles of the precipitate down between the sides of the filter and funnel. In some operations, a double filter is employed, in which case two plain filters are taken, one being placed inside of the other, so that there will be four folds to each side. For the economical use of expensive paper for analytical pur- poses, Edo Classen recommends cutting the filter in half and fold- ing as illustrated in the diagram (Fig. 264). It is obvious that 172 HANDBOOK OF PHARMACY. this will answer for pharmaceutical work in all cases which allow or require the use of a plain filter. When it is necessary to remove a precipitate from the filter after Fig. 260. Fig. 261. Fig. 263. Fig. 262. Folding Filters. drying, as in opium assay, a special paper with a hardened smooth surface, which can be had in the market, may be used for this purpose. Fig. 264. Folding Filter. The Plaited Filter.—For general pharmaceutical purposes, when the precipitate is not the desired object, for instance, in filtering tinctures, solutions, etc., the plaited filter is employed, because, FILTRATION. 173 owing to its numerous folds, it increases the rapidity of filtration. The filter paper (round or square) is folded along the line a-b (Fig. 265), and then along e-f (Fig. 266), resulting in the square (Fig. 267); this is then folded along c'-f, forming a triangle (Fig. 268); this triangle is folded along the lines g-f", forming an elongated short-based triangle (Fig. 269). This is opened to a Fig. 265. Fig. 266. Fig. 267. Fig. 268. Fig. 269. Fig. 271. Fig. 270 Folding Filters. rectangle (double) as shown in Fig. 270; or proceed thus: after folding to the form shown in Fig. 267, open out as showm in Fig. 266, then taking the lower corners of the edges d and e, fold them over so as to meet at e, thus forming a triangle, this is then laid open and each of the four triangles formed by the creasing, is again creased along the middle by bringing the sides together (inward) in the same manner; this wdien laid out presents the appearance of Fig. 270, the folds or creases all being bent the same direction, that is inward; then beginning at the triangle d-f-x, make a fold along the middle of each of the triangles (fi-fk-fl-fm, etc.), bending the paper back on itself in triangular form. When completed, it pre- 174 HANDBOOK OF PHARMACY. sents the appearance as in Fig. 271 (cut off at M); and when opened out, it appears as shown in Fig. 272. If, by means of a magnifying glass, we examine the structure of a piece of filter paper or filtering cloth, we will see that it is made up of fine hairs or fibres, loosely interlaced, with spaces of considerable size between. These holes are quite large, as compared with the size of the particles of the precipitates we attempt to remove from fluids. Hence in many operations it is necessary to return the first portions of the filtrate, until sufficient of the moist precipitate has collected on the skeleton of the paper or cloth to reduce the diameter of the pores or interstices, after which only the fluid portion will pass through. The paper or cloth simply forms a framework, on which the precipitate builds its own filter bed. Liquids containing mucilaginous or starchy matter which refuse to pass the filter, owing to the deposit thereon of mucilage, are Fig. 272. Plaited Filter. best managed by first straining through some coarse material, such as haircloth, which removes most of this matter, after which they may be filtered in the usual manner. MAXIMS TO BE OBSERVED IN FILTERING. In plaiting, care should be taken not to extend the folds entirely to the apex, but to leave about half an inch uncreased ; otherwise, through the creasing, the apex may become weakened. Before pouring the liquid upon the filter, the latter should be well moistened with water, alcohol, or diluted alcohol, as the case may be. The filter paper should never extend above, but should always end slightly below, the upper edge of the funnel. In filling a filter, the liquid should be poured in, in a slow stream, near the upper edge, where the force will be exhausted on FILTRA TION. 175 the side of the filter, and not be brought to bear on the apex (Figs. 273, 274). If the liquid contains a very fine precipitate, or is dense or hot, a double filter should be employed. Fig. 273. Fig. 274. Decanting Fluids on Filter. The tip of the stem of the funnel should touch the side of the beaker or dish in which the filtrate is to be received. This hastens the flow of the filtrate and avoids any splashing. Fig. 275 Fig. 276. Filtering Stands. When filtering into a bottle or flask, the funnel should be placed in the ring of a filter stand (Figs. 275, 276); or, when placed directly into the flask, sufficient space should be provided for the escape of air, which would otherwise be imprisoned, and 176 HANDBOOK OF PHARMACY. cause filtration to cease for a time. This may be provided for by hanging a short piece of a string or a folded strip of paper in the neck (Fig. 277), or by introducing a glass tube between the filter and funnel, reaching down into its neck. FIG 277. Fig. 278. Filtering into Bottle. Chemists’ Cover. In filtering volatile liquids, the funnel should always be covered, either with a well-fitting plate of glass, or, better, with a rubber cover (chemists’ cover), provided the liquid does not act on rubber. Funnels.—A funnel is a conical- shaped utensil, the apex of which is terminated by a long stem or tube. They are used to assist in pouring fluids into narrow-mouthed receptacles and for the purposes of filtration. In a properly shaped funnel, the sides should be so inclined, that, when meet- ing at the neck, they form an angle of 60° (Fig. 279). The outer lines at the junction of the sides and neck form an angle of 150°. The funnels d and e (Fig. 280) are poorly shaped ; in d, the angle of the sides is too sharp ; in e, the neck fails to form a sharp angle with the sides.* The end of the stem of the funnel should be cut off diagonally, which facilitates the discharge of the filtrate. Funnels are constructed of glass, porcelain, earthenware, so- called agate or granite ware, iron, tinned iron (“ tin ”), copper, Fig. 279. Rim. FBody. Neck. Stem. End or Tip of Stem. Properly Shaped Funnel. * For the general purposes of filtration, especially when the plaited filter is used, these require- ments are not necessary. The latter refer more particularly to plain filters used in analytical opera- tions, and that of rapid filtration, where it is absolutely necessary that the sides of the funnel should have the proper degree of inclination. FILTRATION. 177 hard rubber, etc.; each has its own particular application. Copper is employed for liquors and neutral liquids, tinned iron for oils, enameled ware or earthenware for hot caustic liquids. With Fig. 280. Proper and Faulty Shaped Funnels. usage, the enameling is apt to chip off and expose the iron surface, which rusts readily. The earthenware or porcelain funnels are objectionally clumsy and heavy. Tin wears off too readily and exposes the iron underneath to rust. Hard rubber funnels are very light and durable, but are objectionable because, by long use, the inner surface be- comes rough, and particles of matter find an easy lodging place and are very diffi- cult to remove, hence are liable to con- taminate subsequent filtrations. For gen- eral use, glass answers best, because of its transparency and cleanliness. Funnels grooved inside (so called “ fluted funnels ”) are also in the market for the purpose of facilitating filtration ; many of these are objectionable, because of the difficulty in thoroughly cleansing them; moreover, they do not filter more rapidly than a properly made plaited filter. The ribs, to be of any value, should be deeper and spirally arranged. Circu- lar, wire or wooden frames are also to be had for placing in a plain funnel, on which the filter is to be laid; but the wire will rust, thereby staining all preparations containing tannin; and wood will retain the odor and flavor of the different liquids filtered, thereby contaminating subsequent filtrations. For general purposes, such as the removal of coarse mechanic- ally suspended matter or impurities (eolation), a small pledget of Fig. 281. Ribbed or Fluted Funnel, 178 HANDBOOK OF PHARMACY. absorbent cotton placed in the neck of the funnel answers very well. It will not, however, remove finely divided suspended matter. For the filtration of acids, alkaline solutions, or corrosive liquids, spun glass or fibrous asbestos answers best. Granulated charcoal or ground glass are sometimes used for filtering large quantities of liquids. Upward Filtration.—For the filtration of oils and dense liquids, the filtering bag of felt has been in use for a very long time (Fig- 256). Besides this, animal charcoal, sand; sawdust, ground coke, etc., used to be employed, through which the oil or liquid was filtered. This method had the serious objection that the fluid either finds channels between the particles of the filtering medium, whereby it passes through without being filtered, or the filtration proceeds very slowly, or ceases entirely after a time, owing to the clogging of the filter from the sediment deposited. This slow and tedious method has been superseded by the method of “ upward filtrationbut this is only adapted to the filtration of larger quantities of material. For the filtration of oils, we find an early appli- cation of this principle in the oil filter* as shown in Fig. 282. This consists of two separate cylindrical vessels: a has a flange rim of lesser diameter, soldered on the bottom, so as to fit firmly into the open top of the vessel b. To one side of the bottom of a, is attached a tube and stopcock, c, which fits into another tube, d, at e. Near the bottom of the lower vessel is placed a felt filter, curved upward and fastened by thumb- screws passing through two rings and the felt. The stopcock c is closed, and the vessel a is filled with the oil or fluid; then c is opened, the fluid passes down into the space below, filtering upward through the felt into b, where it is drawn off at f. The felt is easily removed and the bottom cleansed. Fig. 283 illustrates an improved form of filtering apparatus upon the principle of which all others are constructed. The oil stored in the reservoir A flows down through the pipes, F, F, into the bottom, a, a, of the two filters, B, B. It is then forced upward, through a layer of felt, b, b, into the layer of sawdust (charcoal, coke), etc., c, c, which is covered with another layer of felt, on which a finely Fig. 282. Filter for “ Upward Filtration.” *This is sometimes called Warner’s Filter. FILTRATION. 179 perforated plate, e, rests, which can be raised or lowered by means of the screws, D, D, decreasing or increasing the pressure on the layer of sawdust. The filtered liquid is drawn out at E, E. Fig. 283. Apparatus for “ Upward ” Filtration of Oils. Fig. 284 illustrates a method of filtering in which the fluid passes through a perforated porcelain cone fitted into the neck of a funnel. Around this cone is wrapped a layer or two of filter paper (or muslin). Then, after inserting the covered cone in the neck of the funnel, the liquid is poured in. This passes through the layers of paper into the perforations, and is discharged below. The particles of precipitate, owing to their own gravity, collect around the bottom, thus avoiding the clogging up of the filter; there is also no danger of rupturing the paper by careless pouring. Upon this same principle Dr. Squibb has constructed a rapid filter for the filtration of large quantities of liquids, A rectangular wooden box is taken (dimen- sions about 30 X 18 X 6 inches), all the sides are pierced full of holes, leaving the bottom intact; one hole is bored in the top for admitting a siphon. Around the box are wrapped, alternately, layers of muslin and filter paper, the outside layer being muslin, secured by stitching. This box is then immersed in the vat of liquid to be filtered; the fluid filters rapidly through into the box, whence it is drawn off continuously by means of a glass siphon. The muslin sides of the filter may be brushed, should they show a tendency to clog from the collec- tion of the precipitate. Hot Filtration.—Dense liquids, such as syrups, oils, fats, gel- Fig. 284. Perforated Fil- tering Cone. 180 HANDBOOK OF PHARMACY. atin solutions, or such solutions as are prone to crystallize while Fig. 285. Fig. 286. Jacketed Funnel. Dieterich’s Jacketed Funnel (for Steam). cooling, are filtered while hot; this is conveniently accomplished by employing the jacketed funnel (Fig. 285), which is double-walled, made of tin or copper. It is filled through an opening in the top and heated at the projecting flange. Fig. 286 illustrates a form proposed by Diete- rich, which is heated by passing steam in at c, which circulates about the sides, b b, escaping through d. Another form * (Fig. 287) consists of a worm of lead or brass pipe, coiled in the form of a cone having an angle of 60°, so as to adapt itself closely to the sides of the funnel. The coil is intended to be charged with steam, to avoid the close proxi- mity of a flame, when inflam- mable liquids are to be filtered. The steam may be generated as shown in Fig. 153, the apparatus being placed some distance from the funnel if necessary. Rapid Filtration (Pressure Filtration).—To promote the rapidity of filtration, particularly in cases of dense or mucilagin- ous liquids, a partial vacuum may be produced and maintained beneath the filter paper. For this purpose various forms of filter pumps are used in the laboratory; in these pumps, water is ejected from a small tube having a pointed orifice, placed with- in another tube communicating with the vessel into which the funnel is fitted air-tight. The continuous, strong jet of water aspirates the air contained in the vessel, and thereby causes the Fig. 287. Liebreich’s Steam Coil Jacket for Hot Filtra- tion. g. Funnel, b. Pipe Coil. * Liebreich’s, made by Kaehler and Martini of Berlin. FILTRATION. 181 liquid to pass rapidly through the filter. The construction of these pumps is very simple, as may be seen in that made of glass, shown in Fig. 288. The water entering at b c, under pressure, is forced out at rapid rate through d, causing suction in e f; the rubber valve, g, regu- lates the pressure and prevents the back-flow of water through / into the apparatus. Fig. 289 illustrates such an apparatus in operation; it consists of a flask, D, into which is tightly fitted, by means of a rubber stopper, a funnel and an exit tube for the withdrawal of air, which is ac- complished by means of the vacuum pump; the water enters the pump at A, and is discharged through B with considerable force, withdrawing the air from the flask by suction through C. Then the pressure exerted by the atmosphere upon the surface of a liquid in the funnel, forces it rapidly through. The more expensive form of a pump with the indicator (indi- cating the pressure), may be replaced by the cheaper forms made of glass. Fig. 288. Water Pump. Fig. 289. Rapid Filtration. 182 HANDBOOK OF PHARMACY. The stopper should be of rubber and firmly fitted in the neck of the flask; to prevent the filter paper from being ruptured at the point, a perforated cone of thin metal (platinum) is first placed in the bottom of the funnel, and into this is placed the plain filter (preferably double) and moistened, care being taken that it fits the sides closely, so as not to admit air through furrows. It is next filled with the fluid, and the suction pump then started, slowly at first and gradually increasing. The cone of platinum may be replaced by a piece of muslin folded like a plain filter, or a so-called “toughened” or “hardened” filter may be used. During filtration, usually by the sudden removal of pressure, Fig. 292. Fig. 290. Fig. 291. Suction Flask for Rapid Filtration. c. Perforated cone. b. Side tube connected with pump. Funnel with Per- forated Disc. Improved Porous Filtering Plate. water may sometimes be drawn over into the filtrate (in the flask). This can be avoided by interposing an empty bottle by means of tightly fitting connections between the pump and filter- ing flask. Where a powerful suction is obtainable, rapid filtration may be effected by placing a Witt’s perforated porcelain disc (with ground slanting edge) in the funnel (Fig. 291); this is then covered with a piece of filtering paper cut slightly larger than the disc, the edges extending about one-fourth of an inch up the sides of the funnel. This is then moistened, the suction gently started, and the filtering paper closely pressed to the sides of the funnel, so that when the liquid is poured in, the sediment may not be drawn down behind the paper. This form of filtration is best FILTRATION. 183 adapted to the collection and washing of precipitates. Fig. 292 illustrates an improvement devised by Kaehler & Martini,* in which a rubber ring is stretched around the edge of the plate to obtain a more secure joint at c; the rod a is intended to assist in keeping the plate in position. Fig. 293 illustrates a convenient method where special appliances Fig. 293. Rapid Filtration (Improvised Apparatus). are wanting; the two aspirators, a, b, are connected by a rub- ber tube; a is filled with water and connected with the flask c, to which is fitted the funnel for filtering. The water is then allowed to flow down from a to b ; this causes the withdrawal of air from c; the higher a is above b, the greater the suction. When the bottle b is full, it is simply interchanged for a, and the flask containing the filter connected with b. * Berlin, Prussia. CHAPTER XX. CLARIFICATION. Many liquids contain finely divided suspended matter which interferes with their transparency, and which cannot be removed by filtration. In such cases we must resort to treatment with some insoluble substance which will attract or envelop these par- ticles. This operation is called Clarification. There is a kind of clarification which may be called “ spontane- ous clarification,” or “ clarification by subsidence,” which may be employed in many cases. It consists in allowing the liquid to stand in a quiet place for a sufficiently long time, until the suspended matter has settled to the bottom. When time is a consideration we resort to artificial clarification. This may be accomplished in several ways :— 1st. By the application of heat, which coagulates albuminous substances which may be present. If liquids containing albumen or albuminous matter are boiled, the albumen coagulates, enclos- ing thereby the particles of suspended matter mechanically, caus- ing them to rise to the surface as a scum. This is then removed by skimming or straining. In this manner we clarify fruit juices, also honey. 2d. By mechanical appliances, (a) Use of Albumen. When albumen is not already present in the liquid, it may be added. The white of an egg (one for each gallon), is first well diluted with a portion of the liquid, the mixture strained, and then added to the balance, which after being well shaken or mixed, is heated gradually to the boiling point, when the coagulated matter is skimmed off. Albumen should not be used for alcoholic liquids, or for solutions which contain substances that unite with albumen forming insoluble compounds, such as salts of mercury, lead, copper, or tannic acid, etc. (6) Use of Gelatin.—This is employed in removing suspended matter, due to the presence of tannin-like substances. It readily unites with these, forming an insoluble leather-like compound. To the cold liquid is added a solution of isinglass; the whole is well mixed, heated to boiling, and on cooling it is strained or filtered. Gelatin is not adapted to alcoholic liquids or solutions whose activity depends on tannic acid. (c) Use of Insoluble Bodies, as Calcium Phosphate or Magne- sium Carbonate or Talcum.—These answer admirably for clarify- ing neutral liquids ; in this case a small quantity is triturated to a paste with the fluid, the balance being added gradually, and the whole is then filtered through a plain or plaited filter. 184 CLARIFICATION. 185 Paper Pulp.—This acts mechanically like the preceding, but is not so satisfactory. The pulp is added to the liquid, the mixture well shaken and poured on the filter, the first portions of the fil- trate being returned to the filter, until the liquid runs through clear. The pulp may be prepared by pouring a hot solution of caustic soda over cut filter paper, reducing it to a pulp by means of a pestle, then washing thoroughly with hot water, until all traces of alkali have been removed; that is, until the wash water fails to turn red litmus blue, or phenolphtalein red. (cZ) Use of Alcohol.—This coagulates slimy and mucilaginous substances. Hence, when added to liquids containing these mat- ters, it causes a coagulum to separate which carries the suspended matter along with it. After filtration, the alcohol is driven off by heat. Alcohol plays the part of a clarifying agent, in the clarifi- cation of fruit juices, and, owing to the manner in which it is generated, the operation is designated as clarification by fermenta- tion. This method is based on the transformation of the fruit- sugar contained in the expressed juice into alcohol by means of saccharine fermentation. For this purpose, the expressed juice is placed in a room where the temperature varies from 20 to 25° C., until alcoholic fermentation is over; this requires about forty- eight hours, after which the liquid is heated to boiling and strained. * * A powder for clarifying wines, liquors, essences, etc., may be made by mixing 40 parts each of finely powdered egg albumen and milk-sugar with 20 parts of starch in fine powder. To each liter of the fluid, 5 grammes of this powder are added, and after thorough agitation, the mixture is set aside for several days and then filtered. CHAPTER XXL DECOLORATION. The process of depriving liquids of color by filtration through some substance capable of absorbing organic coloring matter. The object of decoloration is to remove the coloring matter and impurities accompanying vegetable principles such as alkaloids, glucosides, or bitter principles. It is resorted to particularly for decolorizing syrups in sugar refining, and cotton-seed oil; for the removal of color from petroleum residues, in the manufacture of petrolatum, and petroleum jellies. Formerly precipitated iron or aluminium hydrate were used to some extent as decolorizing agents. Animal charcoal is made by heating bones, in closed retorts, out of contact with air; the product is then reduced to a granular condition by grinding. The best qualities are made from dried blood. Powdered animal charcoal is often called bone-black. When of good quality, it should, upon being boiled with solution of potassa, not impart any color to the liquid. It consists of carbon (about 10 per cent.), calcium phosphate and carbonate, aluminum and iron hydroxides, and silica (about 90 per cent.). Its decolorizing powers were supposed to be due to the minute state of division of the carbon, or to its physical condition, as an aggregation of cellular spaces; however, recent investigations tend to show that the impurities in the animal charcoal play a large, if not the largest, part in the decolorizing power. In view of this, Stenhouse has prepared an aluminized charcoal,made by impregnat- ing finely powdered wood charcoal with 7| per cent, of alumina, drying, and igniting. He also prepared an artificial bone black by impregnating powdered charcoal with 7| per cent, of calcium phosphate. These prepared charcoals decolorize well, but can be used only for neutral solutions. After being once used, animal charcoal may be washed with dilute acids, re-burnt out of contact with air, and again used; in fact, it may be used many times over, although its decolorizing powers gradually become weaker. Solu- tions of plant principles which are to be decolorized are either digested with, or percolated through it. Since it has a tendency to retain such principles, the charcoal should afterward be boiled with some of the solvent, for instance, alcohol, which extracts the principle retained. 186 CHAPTER XXII. SEPARATION OF IMMISCIBLE LIQUIDS. The pharmacist occasionally has to separate immiscible liquids ; for instance, in the washing or purification of oils (volatile and fixed), which have become resinified or partially rancid. He has also occasion to separate immiscible volatile solvents (ether, chloroform, benzin, etc.), from aqueous solutions. In the first in- stance, after the oil has been thoroughly washed, by agitation in a closed flask with water (slightly alkaline), the mixture is poured into an open separating funnel (Fig. 294), allowed to stand until it has separated into two clear layers, then the underlying water or oil may be slowly and carefully drawn off. Fig. 295 illustrates a home-made separating funnel designed by C. 0. Cur- Fig. 295. Fig. 296. Fig. 291. Separating Funnel (stoppered). Separating Funnel (Currier). Separating Flask (pear-shape). rier. The liquid is drawn off by means of a glass tube, sliding through a cork. Near the closed end of this tube a hole is filed through, by means of a rat-tail file (moistened with oil of turpen- tine) ; then, by raising or lowering the tube, the respective liquids may be drawn off. For all kinds of operations, the so-called “ separator,” or sepa- rating flask provided with a glass stopper, is to be preferred (Fig. 296). This consists of a pear-shaped or cylindrical bulb provided with a well-ground, perforated stop-cock and a short exit-tube. This form is usually employed in the various opera- tions of shaking aqueous liquids with volatile solvents, which is necessary in the preparation of various pharmaceutical products and in the assay of alkaloidal drugs. When such separators are 187 188 HANDBOOK OF PHARMACY. not available, the agitation may be performed in a glass-stoppered bottle, and the fluids separated by means of a pipette, the point of which is drawn out to a capillary (Fig. 297). Over the top of these small pipettes an unperforated rubber nipple may be drawn, which may be used as a means of suction instead of the mouth.* In operating upon larger quantities of liquids, they may be separated readily and completely, by means of a siphon which is operated by forcing air into the flask. The arrangement in Fig. 298 is adapted for the withdrawal of the lower fluid, and in order that none be lost, the tube is bent so that it can be shoved into the edge of the bottom when the flask is inclined. For drawing off the upper fluid (Fig. 299) the siphon, which has a hook at the shorter extremity, is raised to the lower level of the floating fluid. Fig. 297. Separation of Fluids by Capil- lary Pipette. Fig. 298. Fig. 299. Separation of Immiscible Fluids by Siphon. * See Pipettes, page 164. CHAPTER XXIII. EXTRACTION. This term is applied to any process whereby the soluble matter of complex drugs, usually vegetable, are separated from the in- soluble portion by means of a solvent: when practically ac- complished, the drug is said to be exhausted. This is carried out in the operations of maceration or digestion, percolation, or a combination of both. MACERATION. Maceration consists in subjecting a drug, reduced to a coarse powder, to the solvent action of a selected liquid, called the menstruum, the length of time and temperature being an im- portant consideration. The temperature employed in different pharmacopoeias varies from 10° to 100° C., being accordingly designated as maceration, digestion, infusion, or decoction. When a moderate heat (30-40° C.) accompanies maceration, it is called digestion. Maceration for a short time, either in cold, lukewarm, hot, or boiling water, and subsequent straining, is called infusion. When the mixture of drug and water is‘boiled together, it is called decoction. The temperature of maceration, in the preparation of tinctures, wines, vinegars, etc., as directed by most pharmacopoeias is from 15° to 20° C. The length of time is from 1 to 36 hours, according to the nature of the drug and menstruum; where the process of percolation is not employed, the time of maceration is usually extended to the period of a week or more. In the manufacture of pharmaceutical preparations, when the drug is to be exhausted by a fluid menstruum, as in the prepa- ration of tinctures, extracts, wines, vinegars, etc., two methods of extraction are employed, either that of maceration, or that of percolation. The process of maceration is employed almost exclusively by the European apothecaries, wTho claim that it pos- sesses the following advantages over the method of percolation. By maceration, the drug is more evenly exhausted, and the products obtained are of like and uniform composition and are more stable. It affords excellent results every time a substance is to be ex- hausted and with the smallest possible quantity of menstruum. It is far less expensive, since the loss in alcohol is very slight, the chief opportunity for any loss being during the operation of expressing the residue. 189 190 HANDBOOK OF PHARMACY. Preparations made by percolation are less stable, being more liable to precipitate, and especially so if water is used for forcing out the last portions of alcoholic menstruum, for then a diffusion of the two cannot always be avoided. Maceration answers best for inexperienced hands, since the operation of percolation requires skill, with careful and constant supervision, in consequence of the wide variance in the nature and structure of different drugs. It does not necessitate the pulverization of the drug, thereby dispensing with previous desiccation and possible loss, by alter- ation or destruction, of volatile principles, as, for instance, in conium, lobelia, physostigma, etc. On the other hand, it is claimed that the process of maceration involves considerable loss. Yet, when the operation is carefully managed, the loss is not any greater than by the process of perco- lation.* For further references concerning the process of macera- tion, see Tincturse and Extracta Fluida. Percolation is not adapted to certain kinds of drugs, particularly those of a spongy nature, which tend to swell with aqueous or hydro-alcoholic menstrua, and render the passage of the fluid slow and difficult; as examples, arnica flowers and orange-peel may be cited. Percolation is well adapted to such drugs as aconite root, cin- chona bark, ergot, etc., but, wherever applied, the process demands care and skill. * Economic Percolation by Arny, “ Proceed. A. P. A., ’92,” p. 169. CHAPTER XXIV. PERCOLATION. Percolation, or displacement, is the process of extraction of a drug by the gradual descent of a solvent. It is called displace- ment because the solvent, after becoming charged with the solu- ble constituents of the drug, is displaced by fresh portions of the solvent liquid, and from its own gravity, and by the presence of the liquid above, minus capillary force, continues downward and is discharged below. Percolation, when properly carried out, is an effective and expeditious process of drug extraction. It yields at once, without further manipula- tion, a finished product. The product is called thepercolate, and the vessel in which the operation is carried on, the percolator, and the liquid sol- vent employed is called the menstruum. The earliest and simplest application of the process of percolation wasthat embraced in the old process of lixivia- tion, which consists in depriv- ing wood ashes of their solu- ble matter, by pouring water over them, when placed in a cylindrical or conical vessel. Count Rumford, in 1813, used percolation in making coffee decoction, but the first application of this process to the extraction of drugs was made by Count Real in 1815, who invented a so-called press (Fig. 300), which con- sisted of a metallic cylinder, tapered below to a narrow neck, which was provided with a stopcock. In the bot- tom of this cylinder was a perforated diaphragm, upon which the drug was to be packed, entirely filling the apparatus. The top Fig. 300. Real’s Press (Percolator). 191 192 HANDBOOK OF PHARMACY. is covered with a tightly fitting cap, connected with an upright tube, from 2| to meters long, enlarged to a cup-shaped opening above. This was employed in making infusions, in which the main difficulty experienced was, owing to the great pressure produced by the height of such a column of liquid, that the menstruum flowed through without completely exhausting the drug. Later (1817) it was used by Johnson in the extraction of cinchona, but to Boullay freres (1833) belongs the credit of fully demonstrating its practical value in pharmacy. While the process was making rapid progress in France, Messrs. Duhamel, Proctor, and Grahame were carrying on experiments in America, which finally led to its first introduction into the U. S. Pharmacopoeia of 1840, where it was made official as an alternative process. Since that time, great progress has been made in bringing this process to a greater state of perfection through the labors of Proctor, Squibb, Lloyd, and others. The process, while being employed exclusively in our own Pharmacopoeia in the preparation of its tinctures, fluid extracts, etc., has received until within recent years, comparatively little attention from the European pharmacopoeias, where the pro- cess of maceration is still employed almost exclusively. The U. S. Pharmacopoeia gives the following definition and description of the process:— “ The process of percolation, or displacement, directed in this Pharmacopoeia, consists in subjecting a substance or a mixture of substances, in powder, contained in a vessel called a percolator, to the solvent action of successive portions of a certain menstruum in such a manner that the liquid, as it traverses the powder in its descent to the receiver, shall be charged with the soluble portion of it, and pass from the percolator free from insoluble matter. “ When the process is successfully conducted, the first portion of the liquid, or percolate, passing through the percolator, will be nearly saturated with the soluble constituents of the substance treated; and if the quantity of menstruum be sufficient for its exhaustion, the last portion of the percolate will be nearly free from color, odor, and taste, other than those of the menstruum itself.” In order to be able to apply the process of percolation intelli- gently, so as to secure the object aimed at, viz., the extraction of the useful soluble constituents of a drug, the operator must have some knowledge of the structure and composition of the drug. In its natural, unpowdered condition, the drug (assuming it to be of organic origin) is usually made up of cells and vessels of various shapes and of interstitial spaces. When the drug is powdered, many of these cells and vessels, which usually contain the matters to be extracted, are broken up, and the interstitial spaces are thus largely increased in number. If the powdered mass is now to be extracted by a menstruum, not in repose, but slowly passing through the mass, it is necessary to adjust the current so that the menstruum has time to penetrate the solid PERCOLATION. 193 particles, to become charged with the soluble matters contained therein, and to be slowly displaced by fresh portions of the menstruum. If the current of the menstruum is so rapid that the latter has not sufficient time to penetrate and pass through the solid particles, there will be a deficiency in the product. The best plan of avoiding this is to give ample time to the menstruum, particularly in the beginning, to penetrate the solid substance and to render the cell-walls ready for the process of osmosis. Hence the first step, in percolation, is to moisten the powder and to wait until the liquid has thoroughly penetrated the solid particles themselves. In some drugs this is accompanied by a considerable swelling, or increase of volume, due to their spongy or muci- laginous nature. In these cases it is particularly necessary to wait for complete expansion, since, otherwise, the drug would so clog the percolator that no liquid would be able to pass. Fig. 303. Fig. 302. Fig. 301. Cylindrical Glass Percolator. Conical Glass Percolator. Metal Percolator. “ The percolator most suitable for the quantities contemplated by the Pharmacopoeia should be nearly cylindrical, or slightly conical, with a funnel-shaped termination at the smaller end. The neck of this funnel-end should be rather short, and should gradually and regularly become narrower toward the orifice, so that a perforated cork, bearing a short glass tube, may be tightly wedged into it from within until the end of the cork is flush with the outer edge of the orifice. The glass tube, which must not project above the inner surface of the cork, should extend from 3 to 4 Cm. beyond the outer surface of the cork, and should be pro- vided with a closely fitting rubber tube, at least one-fourth longer than the percolator itself, and ending in another short glass tube, whereby the rubber tube may be so suspended that its orifice shall be above the surface of the menstruum in the percolator, a rubber band holding it in position. 194 HANDBOOK OF PHARMACY. “ The shape of a percolator should be adapted to the nature of the drug to be operated upon. For drugs which are apt to swell, particularly when a feebly alcoholic or an aqueous menstruum is employed, a conical percolator is preferable. A cylindrical or only slightly tapering percolator may be used for drugs which are not liable to swell, and when the menstruum is strongly alcoholic, or when ether or some other volatile liquid is used for extraction. The size of the percolator selected should be in proportion to the quantity of drug extracted. When properly packed in the perco- lator, tiie drug should not occupy more than two-thirds of its height. The percolator is best constructed of glass or stone-ware, but, unless otherwise directed, may be made of any suitable material not affected by the drug or menstruum.” While not specifying dimensions, the Pharmacopoeia directs the employment of either one of two forms, the conical or cylindrical. In percolating such drugs as are liable to swell considerably, for instance, gentian, calumba, rhubarb, etc., or where the menstruum is more aqueous than alcoholic, the conical form is preferred; since, owing to the slanting of the sides, the drug has an oppor- tunity to expand upward. Also, since these drugs yield to aqueous menstruum a large amount of soluble and mucilaginous matter, it cannot as readily collect as a viscid liquid, and retard percolation, as is often the casein the cylindrical form. In all other cases the tall and narrow cylindrical percolator is preferred, which increases the height of the column of the drug and men- struum in proportion to their mass, thus insuring the thorough exhaustion of the drug with a moderate quantity of menstruum.* “ The percolator is prepared for percolation by gently pressing a small tuft of cotton into the neck above the cork, a thin layer of clean and dry sand being then poured upon the surface of the cotton to hold it in place.” * VARIOUS DIMENSIONS FOR THE DIFFERENT SIZES OF THE OLDBERG CYLINDRICAL PERCOLATOR. Numbers. Approximate Capacity. Length of Body. Internal Diameter at the Top. Internal Diameter of Body at the’ Shoulder. Depth of Shoul- der. Length of Stem (or Neck). Inter- nal Di- ameter of Stem at the Throat. Inter- nal Di- ameter of Stem at Mouth or Exit. Length of Rubber Tube. Numbers. r S J) oiS Millimeters. Inches. Millimeters. Inches. Millimeters. Inches. u SP Inches. Millimeters. Inches. Millimeters. Inches. Inches. -- Inches. 2 150 5 fl. oz. 180 7.09 36 1.417 30 1.181 6 .236 30 1.181 10 .394 12 .472 240 9.45 2 3 240 8 “ 210 8.27 42 1.654 35 1.378 8 .315 30 1.181 10 .394 12 .472 280 11.02 3 4 300 12 “ 240 9.45 48 1.890 40 1.575 10 .394 30 1.181 10 .394 12 .472 320 12.60 4 5 530 18 “ 270 10.63 54 2.126 45 1.772 12 .472 35 1.378 13 .512 15 .591 360 14.17 5 6 740 25 (i 300 11.81 60 2.362 50 1.968 14 .551 35 1.378 13 .512 15 .591 400 15.75 6 7 1,240 42 “ 360 14.17 72 2.835 60 2.362 16 .630 35 1.378 13 .512 15 .591 480 18.89 7 8 1,960 66 “ 420 16.53 84 3.307 70 2.756 18 .709 35 1.378 13 .512 15 .591 560 22.05 8 9 3,000 100 “ 480 18.89 96 3.780 80 3.150 20 .787 35 1.378 13 .512 15 .591 640 25.20 9 10 3,780 8 pts. 540 21.25 108 4.252 90 3.543 22 .866 35 1.378 13 .512 15 .591 720 28.35 10 11 5,700 12 “ 600 23.62 120 4.724 100 3.937 24 .945 35 1.378 13 .512 15 .591 800 31.50 11 12 7,600 16 “ 660 25.98 132 5.197 110 4.331 26 1.024 35 1.378 13 .512 15 .591 880 34.65 12 PERCOLATION. 195 In preparing the percolator, care should be taken not to press the wad of cotton too tightly. It should fit loosely into the upper portion of the neck, partly covering the bottom of the percolator; it is preferable to cover this with a disc of filter paper cut to fit the bottom of the percolator. This may be covered with a layer of clean sand, or pebbles. Some operators prefer to insert a cork, grooved all around, into the upper part of the neck, and to cover this directly with a disc of filter paper. Where obtainable, glass-wool will be found far better than cotton for this purpose, since it retains its spongy condition and does not fall together on becoming wet. In selecting the proper-sized percolator, we must be guided by the amount of drug; thus, if the percolator be large enough for 16 troy ounces, we should not use it for 8 or 10 ounces of drug, and, upon the other hand, the percolator must be amply large enough to accommodate a good supply of menstruum above the surface of the powder. “The powdered substance to be percolated (which must be uniformly of the fineness directed in the formula, and should be perfectly air-dry before it is weighed) is put into a basin, the specified quantity of menstruum is poured on, and it is thoroughly stirred with a spatula, or other suitable instrument, until it appears uniformly moistened. The moist powder is then passed through a coarse sieve—No. 40 powders, and those which are finer, requir- ing a No. 20 sieve, whilst No. 30 powders require a No. 15 sieve for this purpose. Powders of a less degree of fineness usually do not require this additional treatment after the moistening. The moist powder is now transferred to a sheet of thick paper and the whole quantity poured from this into the percolator. It is then shaken down lightly and allowed to remain in that condition for a period varying from fifteen minutes to several hours, unless otherwise directed ; after which the powder is pressed, by the aid of a plunger of suitable dimensions, more or less firmly in pro- portion to the character of the powdered substance and the alco- holic strength of the menstruum; strongly alcoholic menstrua, as a rule, permitting firmer packing of the powder than the weaker. The percolator is now placed in position for percolation, and, the rubber tube having been fastened at a suitable height, the surface of the powder is covered by an accurately fitting disc of filtering paper, or other suitable material, and a sufficient quantity of the menstruum poured on through a funnel reaching nearly to the surface of the paper. If these conditions be accurately observed, the menstruum will penetrate the powder equally until it has passed into the rubber tube and has reached, in this, a height corresponding to its level in the percolator, which is now closely covered to prevent evaporation. The apparatus is then allowed to stand at rest for the time specified in the formula. “To begin percolation, the rubber tube is lowered and its glass end introduced into the neck of a bottle previously marked for the quantity of liquid to be percolated, if the percolate is to be 196 HANDBOOK OF PHARMACY. measured, or of a fared bottle, if the percolate is to be weighed; and by raising or lowering this receiver the rapidity of percola- tion may be increased or decreased as may be desirable, care being taken, however, that the rate of percolation, unless the quantity of material be largely in excess of the pharma- copoeial quantity, shall not exceed the limit of ten to thirty drops in a minute.* A layer of menstruum must con- stantly be maintained above the powder, so as to prevent the access of air to its interstices, until all has been added, or the requisite quantity of percolate has been obtained. This is con- veniently accomplished, if the space above the Fig. 304. Fig. 305. Percolation.! Receiving Jar. powder will admit of it, by inverting a bottle containing the entire quantity of menstruum over the percolator in such a man- ner that its mouth may dip beneath the surface of the liquid, the bottle being of such shape that its shoulder will serve as a cover for the percolator.” Degree of Fineness of the Powdered Drug.—It is essential * The rate or speed of percolation may be increased in proportion to the amount of drug percolated. + Fig. 304 illustrates the official operation of percolation. It also illustrates the solvent action of the menstruum in its descent; the portion, c-d, containing the largest amount of extractive, is followed by the layer d-e, containing less, and e-f, the least amount of extractive. In actual opera- tion the lines of demarcation are not so sharp, but gradually blended from below upward. PERCOLATION. 197 that the drug be of a proper and uniform degree of fineness; when it is too coarse, complete exhaustion does not take place; when it is too fine, percolation ceases from agglutination, and when it is not of uniform fineness, percolation is hindered. The fineness of the powder must be in accordance with the nature of the drug and solvent. Drugs like rhubarb and gentian, which have an open, loose cellular structure, and whose constituents are readily soluble, are easily exhausted when in coarse powder. Such drugs as mix vomica and ignatia have a hard, horny structure, which is not easily penetrated by a solvent, hence they must be reduced to a fine powder. The finer the powder, the more intimate will be the contact with the solvent; hence, in the preparation of fluid extracts, we employ as fine a powder as is consistent with the nature of the drug, while in the case of tinctures, where the amount of menstruum is large in comparison to the drug, we em- ploy a coarser powder. Moistening and Packing.—A drug should be thoroughly moistened and permitted to expand before being packed, so that the dry cellular tissue may, from the absorption of liquid, swell to its ultimate condition, and that, after the drug is packed, the liquid may pass in an even current. If a drug is packed without having been moistened, or before it has ceased to swell, and men- struum then poured upon it, the passage of the latter would soon be obstructed by the swelling of the particles. After being moist- ened, the powder should be rubbed through a coarse sieve so as to secure uniformity of texture and to prevent any balling. After this, it may be either poured into the percolator, which is to be carefully covered so as to prevent the powder from drying out, or placed in a well-closed, wide-mouthed macerating jar. It is then allowed to stand for a period varying from fifteen minutes to several hours, according to the nature of the drug. The powder is now “ packed ” in the percolator, which is done by introducing it in portions, distributing it uniformly and evenly, and applying a more or less strong pressure, according to the directions, in such a way, however, that the pressure always diminishes toward the surface. The directions given by the Pharmacopoeia, viz., “to pour the powder into the percolator, to shake it down carefully so as to avoid the formation of furrows or cavities, and then to apply pressure on the surface,” are liable to produce difficulties during the percolation. The firmness with which a powder should be packed, depends entirely on the structure of the drug and on the menstruum employed. If the drug be porous and spongy and the menstruum aqueous, it should be packed loosely; if the menstruum be alcoholic, it should be packed firmly. As a rule, the more alcoholic the menstruum, the firmer should be the packing. After the powder has been properly packed, a circular piece of filter paper (nicked around the edges), slightly larger than the 198 HANDBOOK OF PHARMACY. diameter of the upper layer of powder, is laid upon the surface, and weighted with pebbles, broken glass, a funnel, or a glass tripod weight* made for this purpose. As much menstruum should be added at once as the percolator will hold, great care being always taken not to allow the menstruum to disappear below the surface of the powder; for should this take place, air will be drawn into the interstices of the drug and fissures will form by contraction of its mass; hence, when more menstruum is added, it will flow through those parts where it meets the least resistance, seeking the fissures which allow the passage of the menstruum through these channels, instead of percolating through the powder. When constant attention cannot be given to the operation, a flask may be inverted over the top of the percolator, as shown in Fig. 304, or the device illustrated in Fig. 252 may be employed, or else the process may be interrupted by stopping the flow of the percolate. After the menstruum has been added (if the drug has been properly packed), it will permeate the powder and descend at a uniform rate throughout the mass. Should it descend more rapidly on one side than on the other, this would be due to irregular packing, indicating that too little pressure has been used on one side as compared with the other, and then a portion of the powder will not be as thoroughly exhausted as that more loosely packed, owing to the rapidity with which the menstruum passes through the more porous portion. Under proper conditions, after the menstruum has penetrated the entire powrder, and passed into the rubber tube, the mouth of the percolator is to be covered to prevent evaporation, and allowed to stand at rest for the time specified by the formula. The length of this period of maceration depends on the nature of the drug and the amount of menstruum. Should the amount of menstruum be small, as in the preparation of fluid extracts, a greater length of time is necessary than in the making of weaker preparations, such as tinctures, wines, etc., for with these the length of maceration may be short, since we have a large amount of fluid with which to exhaust a small amount of drug. Proper Menstruum.—A knowledge of the constituents of a drug, and of their properties, is absolutely necessary before the proper menstruum for percolation can be selected. The menstruum must be so chosen as to extract the active principles, and yet take up as little as possible of the inert matter. The menstruum must also be capable of holding the extractive matter permanently in solution. Such drugs as contain alkaloids, resins, etc., require a more strongly alcoholic menstruum. Such as licorice require a slightly alkaline hydro-alcoholic menstruum. Such as ergot, sanguinaria, conium, etc., are better exhausted with an alcoholic menstruum slightly acidified. In many cases glycerin is added, since it has intermediate solvent properties between that of alcohol * Made by Messrs. Whitall, Tatum & Co. PERCOLA TION. 199 and water, and dissolves all principles soluble in either alone. In the case of gentian, scoparius, and quassia, just enough alcohol is employed to prevent fermentation of the finished preparation. Exhaustion.—The Pharmacopoeia directs that displacement be continued until the drug is exhausted. The exhaustion of a drug cannot be insured with a given amount of menstruum, for that depends entirely upon the skill of the operator. In this case, we must be guided by the nature or peculiarities of the drug operated upon. When the active principles possess a bitter taste, as in nux-vomica, cinchona, or quassia, exhaustion is indicated by the disappearance of a prominent bitterness. In the case of resinous drugs, such as podophyllum or jalap, the percolation is to be con- tinued until the percolate ceases to produce cloudiness when dropped into water. With astringent drugs, such as catechu or krameria, we judge the drug to be exhausted by the disappearance of an astringent taste. The exhaustion of alkaloidal drugs is best observed by directly testing a fraction of the percolate for the presence of alkaloids by means of Mayer’s reagent. The color is but rarely a criterion of strength or exhaustion, for percolates may continue to pass through highly colored, and yet the drug may have long been devoid of activity; an exception to this is cochineal, whose virtues reside in its color only. Hence, to carry on the process of percolation intelligently, we must understand the nature and constituents of the drug operated upon. After the drug has been exhausted, varying amounts of the menstruum are retained in the drug residue (marc). The recovery of this is quite important where larger quantities are operated upon. It is best then to throw the entire mass directly into a still, into the bottom of which live steam is passed and the distil- late then condensed. VARIOUS FORMS OF PERCOLATING APPARATUS. For the use of the apothecary, in operating with smaller quan- tities of drugs, the glass percolator is the best, since by its use we are enabled to observe the various stages of the operation. It is also adapted to all kinds of drugs. Glass percolators of a larger size than five gallons are not safe, since, owing to their great size and weight, they are liable to crack. The larger sizes should be supported upon frames covered with some soft material like rub- ber or cork. Next to glass, stoneware jars (Squibb’s Siphon Percolator) are to be preferred. These may be used for quantities up to 200 pounds. Most manufacturers employ tinned copper percolators which permit the carrying on of operations involving 300 to 500 pounds of drugs. Fig. 306 illustrates the Christ-Dieterich Percolator, which is made of tinned copper or earthenware, the sizes varying from one to 10 liter capacity. It is fed automatically from the flask, A, 200 HANDBOOK OF PHARMACY. through the tube, e, which may be made of any length desired so as to reach further down, should the percolator not be filled. The drug rests on the sieve bottoms, a and b, between which a layer of cotton may be laid. The flow of percolate is regulated by the stop-cock, c. Fig. 307 illustrates a handsome percolator, constructed of glass, intended for operating with smaller amounts ; these are also con- structed of copper or enameled iron for larger quantities. The Fig. 307. Fig. 306. Christ-Dieterich Percolator. Percolator (Warmbrunn, Quilitz). operation is essentially the same as that shown in the preceding illustration. The drug rests on a perforated porcelain disc, b. In actual practice, it is a very difficult matter to regulate the flow of the percolate, to any degree of uniformity, with a stopcock. More- over, a stopcock is also very easily clogged by small particles of solid matter. Dr. Squibb has overcome this difficulty by using the siphon, as is shown in the following:— PERCOLA TION. 201 Siphon Percolator*—This form of percolator was designed by Dr. Squibb, who claims for it the following merits: it combines maceration with percolation, enabling the operator to vary the amount of maceration easily during the process; it controls the rate of percolation perfectly, and renders the percolation uniform throughout the mass of substance, independent of the packing, hence it requires less skill and experience in packing to obtain a given success in result; it is economical on the material, and as nearly automatic and self-controlling as a piece of apparatus can well be, and therefore requires the least time and attention ; it suc- cessfully exhausts substances in coarse powder better than the usual forms, hence it is better adapted for the use of the apothecary than the usual form, which requires a great deal of care and skilful manipulation. Fig. 308 illustrates one form of this percolator best adapted for handling smaller quantities of the drug. The description given by Dr. Squibb in his paper before the American Pharmaceutical Association in 1872 is as follows:— “ The percolator, a, is of the form of the modern glass percolator, somewhat funnel shaped, to allow substances to swell with- out becoming impacted, having no outlet at the bottom ; the delivery tube being converted into a solid stem, and this ter- minating in an ordinary circular foot upon which the percolator is supported. The total height is 15j to 16 inches, or about 40 centimeters, of which about 4 inches, or 10 centimeters, is foot and stem. The interior dimensions, to accommodate con- veniently an official portion of 16 troy ounces of any powder, however light, and a good portion of menstruum above it, is 111 inches, or 26 centimeters, deep, 51 inches, or 14 centimeters, across the top, and 2 inches, or 5 centimeters, across the bottom, which should be flat, as shown in the drawing, and not cup-shaped, as the glass blowers are apt to leave it. A rim of glass is made upon the upper edge or lip to thicken it, and this lip is ground off so that the cover may fit accurately to prevent loss by evaporation. “ A disc of flannel or blanket, b, is cut so as to lie flat upon the bottom, which it entirely covers. “ Another disc of the same material, but a little larger, c, is made with a crucial incision in the center, so that it may be stretched over the end of the well tube. “The central or well tube, e, is a simple piece of glass tube about 12 inches, or 30 centimeters, long by | to J of an inch, or 1J to 2 centimeters, internal diameter. Over one end of this w'ell-tube the upper disc of blanket is stretched, the end being pushed through the crucial cut so that the disc fits tightly on the tube, the four corners made by the crucial cut being reflected up against the sides of the tube. Fig. 308. Siphon Percolator. * Sometimes called “ Well-tube Percolator.” 202 HANDBOOK OF PHARMACY. The disc is then slipped up to the other end of the well-tube, and is tied firmly on to the tube by small twine or thread wrapped around the corners of the disc where they are reflected up against the tube. “A disc of filtering-paper, d, larger than the blanket, with a crucial cut in the center, is cut in toward the center around the edge so as to lie flat against the sides of the percolator where reflected up against them. This disc of paper is pushed down upon the upper blanket. “ If now a piece of paper be twisted around the upper end of the well tube, or a cork be temporarily stuck into it, the percolator is ready to receive its charge, which is packed in around the well-tube and upon the discs of paper and blanket so as to occupy the lower part of the body of the percolator, h. “When the charge, having been properly moistened, rubbed, and sifted, is packed in around the well-tube, its surface is covered by a disc of muslin, i, of proper size, and this is held in place conveniently by some fragments of broken glass thrown in upon it. The percolator is then ready to receive the menstruum or weak percolate, and enough of this should be poured on at once to fully saturate the entire sub- stance. The liquid then passes down like a piston, forcing the interstitial air out through the blankets into the well tube, whence it escapes freely. “ A snugly fitting cover, j, is the next requisite, to prevent unnecessary loss by evaporation. This is very conveniently made from sheet rubber, | to f inch, or | to 1 centimeter, in thickness. A disc 7 inches, or 18 centimeters, in diameter has a hole cut in its center, by means of a wet cork borer, of such a size as to slip easily over the upper end of the well-tube. As it is troublesome to raise this cover every time the percolator is to be supplied with liquid, it may be, by means of a sharp knife, kept wet and directed by a ruler, cut nearly through, so that the uncut part of the thickness serves at once as a hinge and a spring, and permits a part, say one-third, of the cover to be raised without raising the remainder, as shown in the drawing. “The percolator is now charged and in readiness to start the percolation. The menstruum will have passed down through the whole of the substance and will have arisen in the well-tube to nearly the same level as that of the liquid on top, and the entire mass will be saturated and in maceration ; and the whole arrange- ment will represent a well dug in the soil of the wet substance. Now, to pump out that well at a rate no faster, but just as fast, as the saturated liquid passes into it through the porous strata at the bottom, is the final step of the process. “This is most conveniently done by a siphon,/, which can be easily raised or lowered through the whole depth of the well. This siphon is made of glass tubing of about | inch, or 3 millimeters, bore, bent twice at right angles, the two legs about 12j inches, or 31 centimeters, long, and 41 inches, or 11 centimeters, apart. The outer leg is a little longer than the inner one, and turned up upon itself for about f inch, or 2 centimeters, as shown in the drawing. The legs should have only such a differ- ence in length that the inner one should reach the bottom of the well when required, and when measured upon the outer one should reach to about half the length of the short turned-up portion. This arrangement prevents the entrance of air into the siphon, and thus prevents it from emptying itself, for when the liquid is drawn over by the siphon until the surface falls to the level of the turned-up point at the outer end, the columns of liquid will be of equal length and will counterbalance each other, and the flow will cease. But as soon as the outer level is raised by the addi- tion of fresh liquid the flow will recommence at a rate proportionate to the difference of level. It is this automatic and constant self-regulating action of the siphon that enables the design of this percolator to be carried out in practice, and the facility with which the siphon is raised or lowered in the well gives the operator perfect control over the process. “ One or more short pieces of concentric india-rubber tubing, y, stretched tightly upon the inner end of the siphon, but fitting loosely in the well-tube, serve to guide the lower end of the siphon and keep it near the center of the well-tube. “Other short pieces of rubber tubing of different sizes, one over the other, so as to form a soft stopper for the upper end of the well-tube, as shown at k. completes the guide by which the siphon is kept in proper position. The inner piece of tub- ing composing this stopper should be large enough to move freely and easily upon the siphon, while the outer piece should fit the well-tube snugly. Then when the siphon is raised to the desired position and this stopper pressed into the well-tube lightly, it pinches the siphon lightly, but sufficiently to hold it in the desired posi- tion and to enable the operator to change the position at will without deranging the apparatus PERCOLATION. 203 “A receiving flask or bottle, I, marked in the neck or at some convenient place to the measure of a pint, and some wooden blocks to support this receiver at various heights, completes the apparatus. When the mouth of the receiver is left upon the same level as the liquid in the percolator, of course the receiver can never run over, and this is the position to which the receiver should be blocked up when left for the night or fora longer time. The liquid will then accumulate in the receiver more and more slowly, immersing the end of the siphon, until the level approaches or reaches that of the liquid in the percolator, and will then remain at rest, but in readiness to start at any moment when the levels may be disturbed either by a fresh supply of liquid to the percolator or by lowering the receiver. Fig. 309. Siphon Percolator. “In order to save space at the top of the drawing, the siphon is represented at nearly its lowest position, a position rarely required except at the end of a percola- tion when the very last portions of liquid are to be drained off. The position of the siphon is to be regulated by the rate of flow, and the position regulates the rate of flow. Therefore this rate must be arbitrarily adopted in view of the fact that the slower the rate the more effective is the percolation. The rate, upon this scale, should never exceed twenty to thirty drops per minute, or two to four fluidounces per hour. “ When the percolation is ready to be started, that is, after the substance is fully 204 HANDBOOK OF PHARMACY. saturated and a stratum of liquid lies above it unabsorbed, the liquid in the well will be found to have arisen nearly to the level of the liquid outside the well-tube. It never rises quite as high within, because this liquid is more dense than the outer liquid, and the column is therefore heavier. “The siphon is then introduced and fixed by the stopper in such a position that the inner end is immersed in the liquid of the well to the extent of two or three inches. The siphon is now ready to be started. The starting is perhaps best done by means of a short piece of small rubber tubing on the end of a longer piece of glass tubing. The rubber tubing should fit snugly over the turned-up end of the siphon, and then by suction with the mouth through the glass tube the siphon is carefully filled from the well. Before slipping off the rubber end of the suction tube from the end of the siphon, the receiver is to be put in place, so that the first drops from the siphon, as well as those which may have passed into the suction-tube, will fall into the receiver. The rate of flow may be very rapid for a few moments, but will soon diminish to uniformity as the levels become adjusted to the uniformity of the rate of flow. If this rate be more than twenty drops per minute the siphon is to be raised carefully, and a little at a time, so as not to expose the end above the liquid in the well, and thus allow the air to enter the siphon, until the required rate is attained. As the rate varies with the varying density of the percolate dur- ing the process the siphon is to be from time to time raised or lowered so as to restore it to the desired standard. When exhaustion is practically effected, the siphon is pushed down to the bottom of the well and all the liquid drained off. The exhausted substance may, by care, be then removed, and replaced by a fresh portion, without disturbing the well tube or discs of blanket and paper, which is a considerable advantage in repercolation, where the same drug is used in successive portions. “The difference in drugs and their menstrua, and difference in the fineness of the powders used, requires a difference in the position of the siphon for every percola- tion in order to attain a uniform rate. In a few drugs in fine powder, and packed pretty firmly, the siphon requires to be kept down at the bottom of the well, par- ticularly in repercolations when dense weak percolates are used on top, from the very first start, and even then the rate will often be far below the standard of twenty drops per minute. But such percolations are always very successful, and very economical except in the time required. When the powder is very coarse and the menstruum thin and light, the siphon is kept very high.” A larger form, is that illustrated in Fig. 309, which represents a stoneware pot of about 2 gallons (about 7.6 liters) capacity, 10 inches (24 Cm.) high, 10 inches across the top, by about 6 inches (14.4 Cm.) across the bottom, inside, holding about 5 to 6 pounds (2 to 3 kilos). These pots should be well glazed inside; they are made of all sizes, adapted to quantities up to 200 or 300 pounds. The manner of filling and the subsequent operations are the same as those mentioned under the preceding. Pressure Percolation.—For the purpose of hastening the oper- ation of percolation, two methods have been proposed: one by creat- ing a vacuum below the drug in the percolator, thereby increasing the pressure above, and the other, by means of hydrostatic pressure caused by a column of menstruum supplied from a reservoir at a height of from 5 to 10 feet. This latter is the embodiment of the principle of the old Real’s pressure apparatus (page 191). There are a number of different forms of this pressure per- colator, among which are those of Stearns, Rosenwasser, Suits, Berry, Anderson, and Lentz. They all differ slightly in various points of construction, but the principle of all is the same, namely, the rapid percolation of drugs by forcing the menstruum at a greater rate of speed than ordinarily attained. PERCOLATION. 205 These instruments may be used with advantage in some cases, for instance, for squills or calumba, which swell considerably, and allow the percolate to pass only slowly. However, the opera- tion should not be hurried, otherwise the particles of the drug are liable to be simply washed with the menstruum. In order that percolation may be successful, time must be given to the menstruum to penetrate the cells of the drug, and to take up the soluble matter, otherwise a satisfactory exhaustion cannot be ex- Fig. 310. Fig. 311. Lentz’s Pressure Percolator. pected. The apparatus devised by Lentz (Figs. 310, 311) will illus- trate the application of the principle. The percolator, h, is made of tinned copper, provided below with a light cover, having a stop- cock, in, as outlet for the percolate; this cover is made air-tight by a rubber ring being laid between the flat edges, held in position by means of clamps. The powdered drug rests upon the per- forated bottom, g, being held in position by the adjustable porous diaphragm, i, which is pressed down on the surface of the powder. The menstruum is supplied from the reservoir, b, which can be 206 HANDBOOK OF PHARMACY. raised to any height desired. The Suits Pressure Percolator is made of glass, so that the entire operation can be seen; this is also provided with a rubber bulb air-pump for producing air pressure when hydrostatic pressure is no longer available. Vacuum Percolation.—This method of percolation was pro- posed by Duffield in 1869. This consists in introducing the powdered moistened drug into a tight cylinder and exhausting as much as possible of the air by means of a pump. Thus by the removal of the air enclosed in the interstices of the drug, the menstruum is enabled to penetrate the drug more rapidly and thoroughly, thereby facilitating maceration and subsequent ex- haustion. An apparatus (devised by W. M. Thomson), based on Fig. 312. Percolator with Air Pump. this principle, is shown in Fig. 312. The following description is that given by R. F. Fairthorne.* “ The shape of the percolator differs somewhat from the usual form, being to some extent egg-shaped, whereby free percolation is insured. The cover (B), which is hemispherical in shape,is fastened upon the body (A) by means of clamps, with india-rubber rings between to render the joint air-tight. The drug to be operated on, having been sufficiently moistened with the menstruum and packed, is next exhausted of as much air as possible by a vacuum being produced through the upper part of the vessel by means of * Amer. Jour. Phar., 1882, p. 237. PERCOLA TION. 207 an air-pump (G), which is connected with it by means of the tube (F). The stop-cock (H) is next closed and (M) opened, connecting with the tube (E), the end of which dips into the liquid to be employed as menstruum, and thereby a sufficient quantity of it is allowed to be drawn into the displacer to cover the drug. The stopcock (M) is then closed and the materials allowed to macerate for several days. To start the percolation the receiver (C) is exhausted of air and the tap (I) having been opened the saturated fluid will begin to drop, and continue to do so so long as the force of the vacuum in the receiver is equal or greater than that in the upper vessel. When it begins to stop, air is admitted above the drug, which is drawn through the material, carrying with it much of the remaining liquid. To finish the operation air is forced into the percolator by means of the pump.” Hot Extraction.—For the exhaustion of a drug by means of a hot menstruum various forms of ap- paratus have been offered; very few, however, are adapted for the use of the apothecary for extracting from one to five pounds of drug. One of the most convenient forms for pharmaceutical operations is Lewin’s Extraction Ap- paratus (Fig. 313). This is adapted for (1) continuous extraction with hot menstrua, (2) continuous extraction with cooled menstrua, (3) recovery of the menstrua from the finished extract by direct distillation. The apparatus is composed of three easily separable prin- cipal parts: C, the tinned copper still, B, the copper percolator, which is pro- vided with three movable sieve bottoms for the reception of the substance to be extracted. A is the condenser. For the Continuous Extraction with Hot Solvents, the vapors pass from the still, C, in the tube 1, and enter through the tri-faucet I, when in position a, through tube 4, into the percolator, B, penetrate the substance to be extracted, and condense. The per- colate passes into the receiver and from this flows through thetri-faucet III, in its position a, through the tube 7, again into the still, to repeat this course as long as may be necessary or desirable. To pre- vent pressure in the apparatus, the tube 2 is removed during this operation, and the tri-faucet II is placed in position a. This admits the vapor into the cooling worm, A, which thus forms a safety valve. For the Continuous Extraction with Cooled Solvents, the vapors pass from the still, C, into the tube 1, and enter through the tri-faucet I, in its position b, through tube 2, into the cooling worm, J, from this as liquid through the tri-faucet II, in its position Fig. 313. Lewin’s Extraction Apparatus. 208 HANDBOOK OF PHARMACY. a, into the percolator, and so through the substance to be extracted into the still as before. For the Recovery of the Solvent from the Extract by Direct Distillation, the vapors pass from the still, C, through tube 1, through the tri-faucet 7, in its position b, through tube 2, into the cooler, A, through the tri-faucet II, in its position b, into the exit tube 3, which latter may be lengthened at pleasure. Portions of the percolate may be removed from the receiver at pleasure through the tri-faucet III, in its position c, by the tubes 2 and 3. All of the tubes are connected or disconnected by good screw-joints. Fig. 314 illustrates the extraction apparatus of C. 0. Currier, which recommends itself for simplicity and cheapness. It consists of a glass flask, O ; glass percolator, K : and a condenser, R. The condenser is the only part that will have to be made ; the other parts of the apparatus are to be found in almost every laboratory. The condenser is a modification of the Liebig condenser, consisting of a number of tubes instead of one, thereby increasing the condensing surface and distributing the condensed liquid evenly over the sur- face of the drug. The condenser is made in the following manner : A tube of tinned copper is made one inch less in diameter than the top of the percolator to be used, and about two or three times as long as its diameter. A cap of tinned copper (tinned side out) is fitted to each end of the tube. The tube is traversed by tin tubes (made by cutting off block- tin pipe to the proper length) that project three-fourths of an inch below the lower cap, and are cut off obliquely to facilitate the dropping of the condensed liquid. One of the tubes, A, is in the center, and passes through the upper cap about six inches, to which a bent safety tube may be attached to prevent undue pressure to the apparatus. The other tubes, G, H, C, D, are closed at the top and pass into the condensing tube to within one-half inch of the top, and are arranged in a circle around the central one. Their number can be increased or diminished according to the size of the apparatus, four or five being sufficient for a pint percolator. Holes for these tubes should be made through the lower cap just the size of the tubes, and the tubes soldered to the cap 2, on the inside before the cap is soldered to the condensing tube. A small brass tube, F, is inserted in the condenser near the bottom and one near the top, B, for the entrance of cold water and exit of warm water. A cork is chosen that will fit tightly into the top of the percolator, and a circular piece cut out of it, just the size of the condenser, R, and is put upon the lower part of it at E. The cork can be kept in place and prevented from slipping up the tube when press- ing into the percolator by soldering a collar of tin to the condenser at a distance from the bottom equal to the thick- ness of the cork. The apparatus is used in the following manner : A cork, N, with longitudinal channels cut in its surface, is inserted in the neck of the percolator, K ; through the center of the cork, a glass-tube, L, is passed to within two inches of the top of the percolator. The tube should be bent over at the top, to prevent its being clogged up by the drug while pack- ing it into the percolator. A little cotton is placed in the percolator and pressed down upon the cork, and the drug packed in the usual manner. The percolator is then fitted into the neck of the flask, O, by means of a perforated cork, M, the liquid to be used as a menstruum having been previously put in the flask. The condenser is then connected firmly with the top of the percolator. The joints are luted with ground flax-seed mixed Fig. 314. Currier’s Extraction Apparatus. PERCOLATION. 209 into a stiff paste with water. The tube F is connected with a supply of cold water by means of a rubber pipe, and the tube B with a sink, or waste-pipe. The apparatus thus put together is placed in a water-bath and the heat applied. The flask should be immersed in the water to the point marked S on the neck. After the drug is exhausted the percolator is removed from the flask and the flask is con- nected by means of a bent tube with a Liebig’s condenser, and the liquid recovered. For apparatus adapted to the extraction of smaller amounts of substances, see Oleoresins, page 290. CHAPTER XXV. EXPRESSION. Expression is forcible straining. The separation of fluid from solid matter is effected in small operations by hand, the straining cloth being used (Fig. 256). On the larger scale, as in the removal of the last portions of fluid from drug residues, it is accomplished by means of presses or the centrifugal machine. Expression is a necessary part of the process of Maceration ; it is also required in the operations of Percolation, for the removal of menstruum adhering to the dregs or “marc.” In some instances, the mass is thrown directly into the press or centrifugal machine; in others, it is first enveloped in a strainer of press cloth, before being sub- jected to pressure. For the purpose of enclosing the material which is to be subjected to pressure, we employ the press-cloth or bag; this must be made of a material sufficiently strong to withstand great pressure with- out rupture. For this purpose strong canvas may be used, or, better, the so-called press-cloth, which is specially made for this purpose. In conducting the process of expression, pressure should be applied very slowly, otherwise, should the substance contain much fluid, the cloth will be ruptured. After the greater part of the liquid has been pressed out and the pulp has become firm, the pressure may be gradually increased to the full power of the press. The compression should be carried on in stages, the press being allowed to rest a few moments after each increase of pressure, thus allowing a new portion of the fluid an opportunity to drain off, and at the same time affording the particles of the mass an oppor- tunity to assume their new positions in closer contact. Each sub- sequent increase of pressure will require a comparatively smaller effort. Screw Presses.—Fig. 315 illustrates the more common form, which consists of a vertical screw operated by a lever, the lower end of this screw fitting into a cavity in the top of tbe plunger, which is free to move about in the limited space of the cylinder. The body of the press consists of an outer metallic casing, which serves to receive the fluid when forced through the perforated sides of the inner cylinder. All the parts of the press, which come in contact with the drug or fluid, should be well tinned, to pre- vent rusting, also to avoid discoloration or injury to the product should it contain tannin-like principles or acids. The drug to be expressed should be first carefully enveloped in a moistened press- cloth (if straining has not been performed), care being taken to fold over the corners, so as to form a square, compact pack. For 210 EXPRESSION. 211 this purpose, the cloth should be sufficiently large, so that there may be no danger of the drug being forced out. The pack, or Fig. 316. Fig. 315. Tincture Press. Differential-Arm Screw Press. the loose drug, if it should require no press-cloth, should be placed uniformly in the cylin- der, so that it may re- ceive equal pressure on all sides. Fig. 316 illustrates the Differential-arm Screw Press, in which the arm is moved back and for- ward in a half-circle, whereby the screw is forced downward. This is the most powerful hand screw press made. Fig. 317 illustrates an elegant screw press designed by Prof. Witt, which is specially adapted for expressing strongly acid or alkaline liquids from masses. It recommends itself for all purposes, since the press-block and all the parts with which the fluid comes in contact are made of the strongest porcelain. Fig. 317. Witt’s Pharmaceutical Press. 212 HANDBOOK OF PHARMACY. A very convenient form of press, which can be operated with- out the use of the press cloth, is the Enterprise Screw Press (Fig. 318). This consists of a horizontal conical cylinder having a hop- per on the upper side of the larger end. A tapering screw fits closely to the inner surface of the case, on the under side of which Fig. 318. Enterprise Screw Press. is a narrow channel, into which slides a perforated brass strip, which permits the escape of the expressed fluid below. The sub- stance is fed into the hopper, where, by means of the revolving screw, it is carried forward and forced into a smaller and smaller space, undergoing thereby a gradually increased pressure, being finally dis- charged, in a dry condition, through a small opening in the end of the cylin- der. This opening may be regulated by means of a thumb-screw, which controls the amount of pressure to which the material is subjected. This screw press is employed largely for the recovery of juices from berries and fruits. The Wedge and Double Screw Presses are somewhat antiquated, and are not now employed in Pharmacy, since, owing to their construction, they are cumber- some and entail considerable loss of fluid. For pressing larger amounts, a very good form is the Knee-lever Press (Fig. 319), which consists of a horizontal screw, operated by means of either a spoked wheel or ratchet bar, causing the knee to be raised or lowered. Hydrostatic, or Hydraulic Press.—This is the most power- ful of all the various presses employed. Its action depends on Fig. 319. Knee-Lever Press. EXPRESSION. 213 the well-known law of equality of pressure, namely, that a “pres- sure exerted anywhere upon a mass of liquid, is transmitted un- diminished in all directions, and acts with the same force on all equal surfaces, and in a direction at right angles to those surfaces.” There are various forms of presses depending on this principle, a more familiar form being illustrated in Fig. 320. It consists of a heavy steel cylinder, B, in which a cast-iron ram, P, works, supporting the plate on which the material to be pressed is placed. Four strong columns support and fix Q. By means of the force- pump, A, which works by means of a lever, M, water is driven into the cylinder through the tube, K, forcing the ram, P, upward. If the area of P is ten times greater than that of p, then a pres- sure of one hundred pounds transmitted through the lever, M, will exert an upward pressure of one thousand pounds on P. Fig. 320. Hydraulic Press. The Centrifugal Machine (or Centrifuge).—As a means for the thorough and rapid separation of fluids from solids, the cen- trifugal machine forms an invaluable part of the outfit of many industries. It is used to separate the syrup (mother-liquor) from sugar crystals; also in the preparation of ammonia-soda in the Solvay process; in the removal of water from heavy precipitates; for removing the water retained by masses of cotton in the manu- facture of absorbent cotton, etc., etc. The centrifugal machine is employed by the chemist in separating crystalline masses from the mother liquor; in the separation of fats from milk; the rapid separation of precipitates in analytical operations, etc. The cen- trifugal machine is also useful to the pharmacist for the separa- tion of fruit-juices from their pulp, also, for the removal of fluid 214 HANDBOOK OF PHARMACY. matter from drug residues. While it does not remove the fluid as completely as a powerful press, yet it is exceedingly useful in Fig. 321. Fig. 322. “Under-Driven Type,” Centrifugal Machines, “Over-Driven Type.” many such operations. The machine consists essentially of a perforated cylindrical cage, fixed to a central shaft, and surrounded by a case. The inner cage revolving at a high rate of speed (up to several thou- sand revolutions per minute), anything contained in it is driven to the circum- ference, and if it be of a sufficiently fluid nature, it passes out through the perforations in the cage, and flies off tangentially. If we desire to free crys- tals from their mother-liquor, or to separate the adhering menstruum from a drug, we place them in the centrifugal machine, whereupon the mother-liquor, or fluid, escapes through the perfora- tions in the cage, while the crystals, or drug, are left behind. Figs. 321 and 322 illustrate small machines, such as are intended for the laboratory. The one intended to be driven by hand belongs to the so-called “over-driven type,” the other, to be oper- ated by a water-motor, is of the “under-driven type.” Fig. 323 Fig. 323. Laboratory Centrifugal Machine. EXPRESSION. 215 illustrates an apparatus adapted for minor operations in the micro- scopical and pharmaceutical laboratory. As shown in the cut, the tubes containing the liquids are placed on the conical bed attached to the pivoted stem, and are held securely in place by leather straps and by depressing the cover lid, which is fastened by means of a slot. The apparatus is set in motion by means of a cord, preferably gut, which is wound around the axis, the action being, of course, to and fro, as in the case of the school-boy’s buzzer. The appar- atus must always be evenly and symmetrically ballasted, so as to insure even action. Among the objects frequently subjected to centrifugal action, for the purpose of separating solids from the liquid, or for caus- ing the heavier suspended solids to settle at the bottom, and the lighter suspended solids to collect at the top of the liquid, may be mentioned milk, cream, urine, sputum, fermenting liquids, etc. PART II. CLASSIFICATION OF PHARMACEUTICAL PREPARATIONS. The various classes of preparations employed in pharmacy may be classed according to their physical and pharmaceutical characteristics:— LIQUIDS. I. SOLUTIONS. Aqueous. Aquae—(Injectiones Hypoderniicae). Liquores. Infusa. Decocta. Mucilagines. Acetous. Aceta. Alcoholic, or Hydroalcoholic. Spiritus. Vina Medicata. Tincturae. Tincturae Herbarum Recentium. Succi. Extracta Fluida. Saccharine. Syrupi. Mellita. Elixiria. Glycerin. Glycerita. Oleic Acid. Oleata. Ethereal. Oleoresinae. Collodia. II. MIXTURES. Linimenta. Misturae. Emulsa (or Emulsiones). SOLIDS. I. For Internal Use. Pulveres (P. Compositi). Triturationes. Oleosacchara (or Elaeosacchara). Massae. Confectiones. Trochisci. Pilulae. Tablettae. Extracta (also, Abstracta). Resinae. II. For External Use. Unguenta. Cerata. Emplastra. Chartae. Suppositoria. 216 CHAPTER XXVI. AQUEOUS SOLUTIONS. AQU2E MEDIC AT.E. Aquce Destillatce; Medicated or Distilled Waters. Eaux distillers, Hydrolats, Fr. ; Destillirte Wasser, Germ. Under the title of Aquae is understood an aqueous solution in which distilled water is quantitatively the main constituent; the solutions being clear, free from undissolved solid matter, and, with few exceptions (Aqua Chlori, Picis, etc.), colorless. As understood by the U. S. Pharmacopoeia, Medicated Waters are simple solutions in which water has been impregnated with volatile substances. Foreign pharmacopoeias recognize under this title aqueous solutions of certain non-volatile,* as well as volatile substances. Many of the aromatic waters are employed as vehicles for the administration of remedies, others are employed internally as medicines, while a third class is used in chemical operations and the arts. According to their method of preparation, they may be divided into three classes; those made by 1st. Direct Solution. 2d. Intermediate Solution. 3d. Distillation. Direct Solution.—In those instances, where the substance is readily soluble in the given excess of cold water, solution is brought about by simple agitation, as in the official examples of Aqua Amygdalae Am arse, Aqua Chloroformi, and Aqua Creosoti. We may prepare many of the medicated waters by simple solution through agitation of the volatile oil with hot water (at about 50° C.), in a flask, allowing to cool, and then siphoning off the dear solution, or removing the undissolved oil from the surface of the solution by means of a wad of absorbent cotton. This method is based on the fact that volatile oils are more soluble in hot than in cold water; hence, by preparing a supersaturated solution, and then cooling it, a saturated solution will result. To this class belong those medicated waters, or more properly chemical solutions, which are obtained by dissolving gases in cold water. For their method of preparation see page 131. The official examples are Aqua Am- monite, Aqua Ammonite Fortior, Aqua Chlori, and Aqua Hydro- * Aqua Calcis. 217 218 HANDBOOK OF PHARMACY. genii Dioxidi.* These solutions should be kept in glass-stoppered bottles in a cool and dark place. Intermediate Solution.—This method of preparation is by far the most satisfactory and convenient. It consists in saturating the distilled water by bringing it in contact with the volatile sub- stance brought to a very finely subdivided condition by means of some intermediate agent. There are various ways of accomplish- ing this. Among the poorest was the method of the U. S. P. of 1880, in which the volatile oil or alcoholic solution of the volatile substance was dropped on absorbent cotton; this was directed to be picked, so as to distribute the material as much as possible; then the cotton was inserted in the neck of a funnel, distilled water poured over it, and the filtrate returned to the funnel until it was saturated. The main objections to this process were that the cot- ton not only permitted oily particles to pass through into the finished preparation, but also that the water was not as thoroughly saturated as that obtained by other methods; since it is impossible to bring about as thorough a state of subdivision of the volatile body by means of cotton as by the method of trituration. This latter method consists in thoroughly triturating the volatile sub- stance, ora solution of it, with some insoluble, inert powder; then adding distilled water sufficient to form a smooth paste, after which the balance of the water is slowly added under trituration. This milky or turbid solution is poured upon a plain wetted filter, and the solution returned until it passes through clear. Various insoluble powders have been proposed, such as mag- nesium carbonate, kaolin, talcum, calcium phosphate, silica, powdered pumice-stone, precipitated chalk, etc. The most satis- factory of these is the precipitated calcium phosphate, which, owing to its insolubility and freedom from soluble impurities, is adapted to all classes of these preparations. Magnesium carbonate 4(MgCO3).Mg(OH')2.5H2O) should not be employed for this purpose, since there is sufficient amount of magnesium hydroxide (Mg(0H)2) present, which goes into solu- tion, to interfere with its use for many purposes. Waters prepared with this will cause the precipitation of many alkaloids; react with some oils; blacken calomel when shaken with them; also cause the decomposition of many sensitive chemicals, such as silver nitrate, gold chloride, mercuric chloride etc. The official waters directed to be prepared by intermediate solution are: Aqua Anisi, Camphorse, Cinnamomi, Foeniculi, Menthse Piperita?, and Menthse Viridis. The medicated waters belonging to this class should be prepared from the very best grades of the volatile oil obtainable. Old resinified oils are worthless. These waters may also be prepared by the following method of distillation: Distillation.—This method, though applicable only to those * Although HoOo is not a gas in the usual sense of the term, the solution is classed here for sake of convenience. AQUEOUS SOLUTIONS. 219 waters whose aromatic properties arc due to the presence of vola- tile oils, yields the finest quality of aromatic waters. In the pre- paration of these, a copper retort, tinned inside, is usually employed. The plant parts (leaves, seeds, crushed bark, etc.) are placed in a wire basket or cage,* which is suspended in the upper part of the body of the still, so that only the steam arising from the boiling wTater may pass upward through the material and over into the condenser. The drug should not come in contact with the boiling water nor touch the heated sides of the retort. It is much better to generate the steam in a separate vessel, and to blow it through the drug contained in the retort as shown in Fig. 153 (or 324). When prepared in this way, aromatic waters keep much longer and better, and are far more fragrant, because by the old method of boiling the plant parts and water together, the boiling Fig. 324. Apparatus for the Distillation of Volatile Oils. e. Boiler, r. Steam Pipe. a. Perforated bottom upon which plant parts rest. k. Condenser. water took up all the extractive and mucilaginous matter of the drug, the presence of which not only injured the aroma of the distillate, but caused matters to be carried over which interfered with its keeping qualities. Before each operation, the still or retort should be thoroughly cleansed by blowing steam through it; if proper cleanliness is observed, the distilled water will be entirely free from foreign (retort) or empyreumatic odor, and will keep longer and better. This cleansing should take place im- mediately after each operation, otherwise, through resinification of particles of oil remaining in the retort, it will be found almost impossible to remove all odor. Most pharmacopoeias direct that the leaves, flowers, crushed or * See Pharmaceutical Stills. 220 HANDBOOK OF PHARMACY. cut root or bark, etc., be macerated in water from 10 to 12 hours before distillation. For each 100 parts of distillate required, it is best to employ from 10 to 20 parts of the dry seed or fruit, and 10 parts of the dry or from 30 to 50 parts of the fresh leaves or bark.* For strong aromatics, such as angelica, juniper berries, cascarilla, etc., 25 parts of the drug are sufficient. Some prefer not to remove any volatile oil that may have separated in the distillate, but to transfer the entire liquid to a stock vessel and to set it aside after thorough agitation. The presence of the excess of oil tends to keep the water constantly saturated, and preserves it from fermenting. When the turbid water is to be dispensed, it should be passed through a wetted filter, which serves to retain the separated oil. The U. S. P. recognizes two waters (concentrated) made by dis- tillation, viz., Aqua Aurantii Florum Fortior, and Aqua Rosa? Fortior, which are known in commerce as “ triple,” and are used in preparing the weaker Aqua Aurantii Florum and Aqua Rosse, by dilution with one volume of distilled water. Only distilled water should be employed in preparing the offi- cial solutions, as well as in carrying out tests. Ordinary hydrant water often causes decomposition of such sensitive salts as silver nitrate, potassium permanganate, etc.; it is likewise irritating when used in preparing eye-washes. When we consider the low cost and the convenience with which pharmaceutical stills may be run, there is no excuse for any apothecary in substituting hydrant water for distilled. It is not within the province of the pharmacist to prepare these concentrated (triple) fragrant waters; hence they are usually imported from southern France and Italy, or other countries where the orange tree and rose are specially cultivated. Among the best known distillers of fragrant waters are Bertrand Bros., Lautier, Chiris, and Tombarell Bros. These concentrated waters retain their fragrance longer than the weaker, hence their use enables the pharmacist always to dispense a fragrant preparation. These stronger waters are best preserved in glass vessels, in which the stopper is covered with either parchment paper or a piece of bladder. Orange flower water should not be made from the oil (Neroli). Rose water can be made directly from the oil by the method of the German Pharmacopoeia, in which from 3 to 5 drops of the oil are agitated with the liter of hot distilled water. Preservation.—Medicated waters rapidly deteriorate, hence they should not be made in larger quantities than are likely to be consumed before they spoil. Unless a layer of oil covers the surface of the water, they will soon deposit flocculent matter or * The proportion depends upon the richness of the plant-part in volatile oil, these figures being general. AQUEOUS SOLUTIONS. 221 become ropy and lose their odor entirely. This is caused by a microscopic vegetable growth, which renders the preparation unsightly and unfit to dispense. In order to avoid this, the freshly prepared water should be put into clean glass-stoppered vials, of appropriate size, the bottles being entirely filled and well sealed to exclude air. In this condition, they may be preserved for an indefinite length of time. Preservative agents, such as alcohol, glycerin, boric acid, etc., have been proposed, buttheir use is not advisable. The presence of small amounts of alcohol gives rise to acetic fermentation ; larger amounts, as well as the presence of any other agents, inter- fere seriously with the various uses of these waters. EXPLANATORY. Aqua Amygdalae Amar.e (Bitter Almond Water; Bitter- mandelwasser, Germ.).—This contains 0.1 per cent, of the oil of bitter almond. The preparation is of variable strength, varying according to the source and quality of the oil of almond. When the artificial oil (benzaldehyde) is used, the product is free from hydrocyanic acid (HCN). If the true oil of bitter almond (con- taining from one to six per cent. HCN) is employed we find vari- able amounts present; should the oil contain six per cent, of absolute HCN, the water would contain about one drop of the official acid in each half ounce. It is employed in this country as a vehicle or flavoring agent. Aqua Amygdalarum Amararum.—Under this title, we find a preparation official in various European pharmacopoeias, which is prepared by distilling bitter almonds with water; this is far stronger than ours, being standardized to a definite percentage of hydrocyanic acid. It should be administered with great caution. In dispensing this preparation, care should be observed that it be of the exact strength required by the pharmacopoeia which the physician employs. The strength in hydrocyanic acid as recog- nized in various pharmacopoeias is as follows:— PharmacopcBia. HCN in 1000 Parts. Austrian, 1 Belgian, 1 Danish, contains alcohol, . . . . 1.4 German, contains alcohol, . . . 1 Netherlands 1 Russian, contains alcohol, . . . 1 Spanish, 0.86 Swedish, contains alcohol, . . . 1.3-1.4 Swiss, 1 A substitute for this may be made by dissolving 6.46 grammes of chloral cyanhydrate in 1000 Cc. of distilled water. Each 6.46 grammes of this salt contains 1 gramme of HCN. The above is used as a sedative in doses of from 10 to 15 drops. 222 HANDBOOK OF PHARMACY. Under the title of Aqua Laurocerasi (Cherry Laurel Water), a preparation of similar nature is official in several pharmacopoeias. It is made by distilling a mixture of bruised fresh laurel leaves and water. This preparation is likewise standardized to a definite percentage of hydrocyanic acid. Pharmacopceia. HCN in 1000 Parts. Belgian, 0.5 Netherlands, 0.839 British, 1 French, 0.5 The Spanish, German, Greek, and Swiss pharmacopoeias sub- stitute the above-mentioned bitter almond water for cherry laurel water. The German Pharmacopoeia prepares a diluted bitter almond water (Aqua Cerasorum or Kirschwasser), by mixing 1 part of the stronger with 19 parts of water. This preparation, containing 0.005 per cent, of hydrocyanic acid, should not be confounded with either of the above containing 0.1 per cent, of the acid. Aqua Chloroformi.—Chloroform is added in sufficient quan- tity to distilled water, so that, after agitation, it remains in slight excess; the supernatant saturated solution is decanted off as required. When exposed to sunlight, the chloroform readily undergoes decomposition, particularly so in the presence of water. Hence this preparation should be kept in a dark amber-colored bottle. It is employed as a solvent for many remedies, owing to its preservative properties; also, as an adjunct to anodyne mixtures. Aqua Creosoti.—This preparation contains 1 per cent, of wood creosote. It is employed principally as a gargle, or lotion. In ordering creosote, care should be taken to specify “true wood creosote,” or “ beech-wood tar creosote,” for under the term “ com- mercial creosote ” carbolic acid is usually understood. Under the class of Aquas, solutions of gases are included, viz.:— Aqua Ammonite.—(Specific gravity 0.960, containing 10 per cent, by weight of gaseous ammonia (NH3).) It is known among the continental pharmacopoeias under the title of “ Liquor Ammoniae,” being generally recognized to be of 10 per cent, strength (Fr. and Sp., 20 per cent.) This is commercially known as 16° BaumS; the so-called Aqua Ammoniae f.f.f., being 20° B., or about 17 per cent, by weight of NH3. Aqua Ammonee Fortior (sp. gr. 0.901, containing 28 per cent, by weight of gas), is only recognized by the U. S. and British Pharmacopoeias, that of the latter, however, being of 32.5 per cent, strength. For rules for dilution, see page 138. Ammonia Water is incompatible with acids and most metallic AQUEOUS SOLUTIONS. 223 salts; it should be preserved in well stoppered bottles in a cool place. Its strength is ascertained by means of its specific gravity, or by titration with a standard acid solution.* 2NH3 + H2SO4 = (NH4)2SO4. Ammonia. Sulphuric Acid. Ammonium Sulphate. 2 X 17 Pts. = 97.82 pts. 17 pts. = 48.91 pts. 0.017 pt. = 0.0489 pt. Since 1 Cc. of decinormal sulphuric acid solution (containing 0.0489 Gm. H2SO4) neutralizes 0.017 Gm. of ammonia gas (NH3), 20 Cc. of the acid solution will be equivalent to 20 X 0.017 = 0.34 Gm. of NH3. If 3.4 Gm. of Aqua Ammonia were taken for the assay, it would then, according to the above, contain 10 per cent, of ammonia gas. Aqua Chlori.—A clear, greenish-yellow liquid, containing at least 0.4 per cent, of chlorine gas, U. S. P. This preparation is official in all pharmacopoeias, and contains from 0.3 to 0.6 per cent, of chlorine gas. It should be freshly prepared when required for use, since it rapidly undergoes decomposition; thus, 2C1 + H2O = 2HC1 + O. As a ready means of ascertaining whether this decomposition has begun, or not, the pharmacopoeia directs agi- tation of the sample with mercury, which unites with the free chlorine, leaving any hydrochloric acid which may be present free to be detected by litmus paper. Chlorine water is employed in medicine as an antiseptic. It is incompatible with alkalies, silver and lead salts, tannin, infu- sions, emulsions, and tinctures, and liberates iodine and bromine from their salts. When prescribed in mixtures it should be added last. The chlorine strength of this preparation is ascertained in- directly by volumetric estimation.t This is based on the fact that chlorine displaces an equivalent amount of iodine from potassium iodide, according to the equation:— 2KI + 2C1 = 2KC1 + 21. Potassium Iodide. Chlorine. Potassium Chloride. Iodine. 2 X 35.3 2 X 126.5 The liberated iodine is held in solution by the excess of po- tassium iodide. In order to ascertain the amount of liberated iodine, decinormal solution of sodium hyposulphite is run into this dark-colored solution until it is decolorized, according to the following equation:— 21 + 2(Na2S2O3 + 5H2O) = Na2S4O6 + 2NaI + 10H2O. Iodine. Sodium Hyposulphite. Sodium Tetrathionate. Sodium Iodide. Water. 2 X 126.5 pts. 2 X 247.6 pts. 126.5 pts. 247.6 pts. 0.01265 pt. 0.0247 pt. * See Volumetric Solutions. t Ibid. 224 HANDBOOK OF PHARMACY. Since 1 Cc. of decinormal solution of sodium hyposulphite containing 0.0247 Gm. of the salt, is equivalent to 0.01265 Gm. of iodine, therefore 20 Cc. of the hyposulphite solution will be equivalent to 20 X 0.01265 = 0.253 Gm. of iodine. Hence if one molecule of iodine is equivalent to one molecule of chlorine, 0.253 Gm. of iodine will be equivalent to x grammes of chlorine. That is, i ci i ci 253 : 70.6 : : 0.253 : x. x = 0.070 -f- Gm. of Chlorine. If 17.7 Gm. of Aqua Chlori, after having been subjected to the above test, yield 0.070 Gm. of chlorine, it would then contain of the gas 17.7 : 0.07 : : 100 : x; x = 0.4 per cent, (approximately). Aqua Hydrogenii Dioxidi.—This solution should contain 3 per cent, by weight of the pure Dioxide (H2O2), corresponding to about 10 volumes of available oxygen. The dioxide itself may be obtained in a very pure condition* by agitating barium peroxide with diluted hydrochloric acid and ether, the latter absorbing the H2O2; upon shaking the ethereal solution with distilled water, slightly acidulated, it gives up most of its hydrogen peroxide. The great facility with which this solution gives up its oxygen renders it a powerful oxidizer. It bleaches organic colors, like- wise hair; converts sulphides and sulphites into sulphates, ferrous into ferric compounds; liberates chlorine from hydrochloric acid, iodine from hydriodic acid, and iodide of iron; it reacts very slowly in a neutral solution of potassium iodide, thus differing from ozone and chlorine. It is stated that the addition of one part of H2O2 to 1000 parts of impure drinking water will, after a short time, effectually destroy any disease germs that may be present. It is employed in medicine as a powerful antiseptic, and deodorant. The presence of a little acid (even as little as one drop of HC1 to the pint), is essential to prevent its too rapid decomposition. The commercial solution scarcely ever contains over three per cent by weight of absolute peroxide, and the ten and fifteen volume solutions often fall short of the strength claimed for them; hence it behooves the apothecary to assay each lot which he may purchase. The strength of this solution is sometimes indicated by volume. Thus a 20 volume solution is one which, when decomposed into water and oxygen, will yield 20 times its volume of oxygen. It does not matter, in this case, whether the whole of the liberated oxygen comes from the H2O2, or whether a part of this comes from the reagent added. If the H2O2 is decomposed by potassium per- manganate, only one-half of the oxygen given off comes from the H2O2. The strength of the solution is estimated by means of decinormal * Cresiner, “ Proceed. A. P. A.,” 1892, p. 845. AQUEOUS SOLUTIONS. 225 solution of potassium permanganate * according to the following equation:— K2Mn2O8 + 5H2O2 + 3H2SO4 = 5O2 + 8H2O + K2SO4 + 2MnSO4 Potassium Hydrogen Sulphuric Oxygen. Water. Potassium Manganese Permanganate. Peroxide. Acid. " Sulphate. Sulphate. 315.3 169.6 The permanganate solution is added slowly, until the pink color no longer disappears. The presence of the sulphuric acid serves the purpose of dissolving the manganic hydroxide f as fast as formed, otherwise the brown oxide diffused through the liquid w7ould render the end of the reaction difficult to distinguish. Now, according to the above equation, 1 mol. of K2Mn2O8 (315.3 p.) cor- responds to 5H2O2 (169.6 p.); or 0.003153 Gm. of potassium per- manganate (1 Cc. of the decinormal solution), corresponds to 0.001696 Gm. of absolute hydrogen peroxide. Where it is desira- ble to express the strength in volumes of available oxygen, we multiply the number of cubic centimeters of the solution of per- manganate, decolorized by 1 Cc. of the solution, by 0.56. This latter factor is explained thus:— Since one-half of the liberated oxygen is supplied by the potassium permanganate (K2Mn2O8), one molecule of Kq£u;2°8 liberates 5 of 8Q,vgen from the hydrogen peroxide (H2O2); hence, 63 Gm. of K2Mn2O8 (one-fifth of 315.3) will liberate 16 Gm. of oxygen (one-fifth of 80), which at normal temperature measures 11,188 Cc. If 63 Gm. of potassium permanganate liberate 11,188 Cc. of oxygen, 0.00315 Gm. of permanganate (1 Cc.) will liberate 0.56 Cc. of oxygen. AQIDE, U. S. P. Title. Constituents.X Use. Direct Solution. Aqua Amygdalae Am- arae,. Aqua Creosoti, .... “ Chloroform!, . . 0.1% Oil of Bitter Almond. 1% of Creosote. Saturated aqueous solution of Chloroform. Vehicle. Antiseptic. Antiseptic, Anodyne. Gaseous Solutions. Aqua Ammoniae, . . . “ Ammoniae Fortior, “ Chlori, Aqua Hydrogenii Di- oxidi, 10% of Gaseous Ammonia, wt. 28% “ “ “ “ 0.4%“ Chlorine, “ 3% “ Hydrogen Dioxide, “ Stimulant, Caustic. 14 44 Antiseptic. Antiseptic, Deodorant. *See Decinormal Solution of Potassium Permanganate. f The substance precipitated (from alkaline solution) is manganous hydroxide, which rapidly turns to brown manganic hydroxide J In this and subsequent tables $ (per cent.) is employed merely as an expression of convenience. In the case of anise water and others of this class, it means 2 (7c. of the oil in 1000 Cc. of water. In the case of camphor water it means 8 Gm. of Camphor in 1000 Cc. See “ Percentage Solutions,” page 137. 226 HANDBOOK OF PHARMACY. Solutions of Volatile C Title. >ILS. Constituents. Use. Aqua Anisi, “ Campho rae, . , . 0.2% of Oil of Anise. Vehicle. 0.8% of Camphor. Antispasmodic. Cinnamomi, . . 0.2% of Oil of Cinnamon. Vehicle. “ Foeniculi, .... 0.2% of Oil of Fennel. u ‘ ‘ Menthae Piperitae, 0.2% of Oil of Peppermint. u “ Menthae Virid is, . 0.2% of Oil of Spearmint. k k Distillation Aqua Aurantii Florum Fortior, Triple Orange-flower Water. Aqua Aurantii Floruni, Equal parts of the above and distilled water. Vehicle. “ Rosae Fortior, . . Triple Rose Water. ‘ ‘ Rosae, Equal parts of the above and distilled water. Vehicle. INJECTIONES HYPODERMICS—{Hypodermic Injections). When remedies are to be used hypodermically, it is absolutely necessary that these solutions be as neutral as possible and steril- ized. As antiseptic vehicles, for the administration of these remedies, various solutions have been proposed, such as solutions of camphor, thymol, or corrosive sublimate, and chloroform water; however, when these solutions have been exposed to the air, they are not fit to be dispensed. When it is necessary to prepare such a solution, the test-tube in which it is prepared and the receiving- vessel, should be first sterilized by rinsing them with boiling water, and then dried in an oven at a temperature of about 200° C. Only thoroughly boiled distilled water should be used as solvent. In Germany and Austria, these solutions are now often prepared and sealed in small, elongated glass pearls (sterilized at 200° C.) of 1 Cc. capacity. Thus sealed, these solutions may be preserved indefinitely and can be readily carried about. The sterilized hypodermic tablets, in which exsiccated neutral sodium sulphate forms the inert diluent, have become very popular, because of their convenience in use, and the accuracy of their dosage. These tablets should always be dispensed in their tubes and never handled with the fingers. The hypodermic dose of a remedy is | or less than the dose by the mouth. 227 AQUEOUS SOLUTIONS. LIQUORES—(ZtQwors).—SOLUTIONES— Liquors are aqueous solutions of chemical substances. There are twenty-four of these official in the U. S. P., 1890. Liquor Acidi Arsenosi (Liquor Arsenici Chloridi, U. S. P., 1880).—This is simply a solution of arsenous acid in hydrochloric acid and water, and not a definite compound. It is about twice as strong as Valangin’s solution, which contains about 0.4 per cent., while the official product contains 1 per cent, of arsenous acid. Its properties are much the same as Fowler’s solution, but its action is not reliable. Dose 0.12 to 0.6 Cc. (2 to 10 minims). For assay, see Liquor Potassii Arsenitis. Liquor Ammonii Acetatis (Spirit of Mindererus).—If the pharmacopoeial directions are strictly followed, a preparation of an acid reaction will be obtained. This is essentially necessary, otherwise, when it is added to solutions containing alkaloids or metallic salts, these would be likely to be precipitated from their combinations. Should such be the case, the addition of a little acetic acid, sufficient to clear up the solution, is necessary. The reaction between the ammonium carbonate (a mixture of ammonium acid carbonate and carbamate) and acetic acid is as follows :— NH4HCO3.NH4NH2CO2 + 3CH3COOH = 3CH3COONH4 + H2O + 2CO2 Ammonium Carbonate. Acetic Acid. Ammonium Water. Carbonic 156.7 3X 59-86 Acetate. Acid Gas. When freshly prepared, it contains free carbonic acid. The German and Swiss Pharmacopoeias prepare this from ammonia water instead of from ammonium carbonate. Exercise.—How much official ammonium carbonate will be required to neutralize 100 Cc. of diluted acid, U. S. P. ?—100 Cc. of the diluted acid weigh (100 X 1.008) 100.8 Gm.; 6 per cent, of this is absolute acid = 6.048 Gm., then: Acetic Ammon. Acetic Ammon. Acid. Carb. Acid. Carb. 179.5 : 156.7 : : 6.048 : x x = 5.27 + hence, 5.27 + Gm. of official ammonium carbonate are required to neutralize 100 Cc. of official diluted acetic acid. Liquor Arseni et Hydrargyri Iodidi (Donovan’s Solution). —This is best made from the precipitated Iodide of Arsenic (Bam- berger), as it is far more soluble than the commercial, made by EXPLANATORY. 228 HANDBOOK OF PHARMACY. fusion. The solution should be kept in a dark place, as the action of light causes a partial separation of iodine with change to yellow color. When in this condition it should not be dispensed. This solution contains one per cent, of each of the iodides. It is incompatible with alkaline solutions, since they cause the precipitation of the mercury; it is also incompatible with solutions of silver salts, owing to the precipitation of the silver as insoluble iodide; also with weak alcoholic or aqueous solutions containing alkaloids, since it forms with them insoluble double salts. Liquor Calcis (Lime Water).—When water is added to cal- cium oxide (burnt lime), considerable heat is generated, with formation of calcium hydroxide Ca(OH)2; this is soluble in 780 parts of cold water, but only in 1650 parts of boiling water. Each fluidounce of lime water would then contain about three-quarters of a grain of calcium hydroxide. Liquor Calcis should be pre- pared from a calcium oxide, which is made from marble, a very pure form of calcium carbonate. When the calcium oxide is made from ordinary limestone, it will be contaminated with alka- lies, which dissolve readily in water; hence the Pharmacopoeia directs, that the slaked lime should be first treated with a small portion of water, which removes these impurities. Lime water should not be added to salts of alkaloids or of metals, nor to acid solutions. When added to calomel (1 drachm to the pint) it forms the so-called Black Wash (Lotio Nigra). When added to corrosive sublimate (one-half drachm to the pint), it forms the Yellow Wash (Lotio Flava, or Aqua Phagedamica). In the latter case, care should be taken that no free corrosive sublimate remains in the solution, which may arise from deficiency of strength of the lime water. This solution should be kept in a well-stoppered bottle, away from access of the air, otherwise all of the calcium hydrate would soon be converted into and precipitated as carbonate. Liquor Ferri Acetatis.—This solution contains about 31 per cent, of anhydrous ferric acetate It is prepared by dissolving ferric hydroxide in glacial acetic acid. The former is made by pouring a diluted solution of ferric sul- phate, under brisk stirring, into ammonia water, whereby ferric hydroxide is precipitated. This precipitate is collected and well washed to remove adhering ammonium chloride. Fe2(SO4)3 + 6NH3 + 6H2O = Fe2(OH)6 + 6NH4C1 Ferric Ammonia Ferric Ammonium Sulphate. Water. Hvdrate. Chloride. 2 X 55.8 Fe. 6 X 17 FejfOH), + 6CH3CO2H = Fe2(C2H3O2)6 + 6H2O Ferric Hvdrate. Acetic Acid. Ferric Acetate. Water. 2 X 55;8 Fe. 464.9 AQUEOUS SOLUTIONS. 229 The preparation, if made from acetic acid of proper strength, will keep readily ; should a weaker acid be used, the prepara- tion is liable to precipitate a basic ferric acetate (probably Fe2(OH)4(CH3CO2)2). Assay.—The U. S. Pharmacopoeia directs to add to 1.117 Gm. of the liquor, diluted with water, 2 Cc. of hydrochloric acid; this liberates the acetic acid with formation of ferric chloride; then on adding the potassium iodide, iodine is liberated, with reduc- tion of the ferric to ferrous chloride and the formation of potassium chloride; thus: — Fe2Cl6 + 2KI = 2FeCl2 + 2KC1 + 21. Ferric Chloride. Potassium Ferrous Potassium Iodine. 2 X 55.8 Fe. Iodide. Chloride. Chloride. 2 X 126.5 One atom of iron (55.8 pt.) is equivalent to one atom of iodine (126.5 pt.). The amount of iodine liberated is ascertained by means of decinormal solution of sodium hyposulphite,* which is added until the blue color (iodide of starch) disappears; thus, I2 + 2(Na2S2O3.5H2O) = 2NaI + Na2S4O6 + 10H2O. Iodine. Sodium Hyposulphite. Sodium Iodide. Sodium 2 X 126.5 2 X 247.6 Tetrathionate. One molecule of sodium hyposulphite (247.6 pt.) is equivalent to one atom of iodine (126.5 pt.). 1 molecule of ferric acetate = 1 molecule of ferric chloride; 1 molecule of ferric chloride, containing 2 atoms of iron, liber- ates 2 atoms of iodine, which correspond to 2 molecules of sodium hyposulphite. 1 molecule Sodium Hypo- 1 atom Iron. 1 atom Iodine. sulphite. 55.8 Gm. = 126.5 Gm. = 247.6 Gm. 0.00558 Gm. = 0.01265 Gm. = 0.02476 Gm. Or 1 Cc. V. S. or 0.02476 Gm. of Sodium Hyposulphite = 0.00558 Gm. of iron. 15 Cc. of the Sodium Hyposulphite V. S. = 15 X 0.00558 = 0.0837 Gm. iron. Since we took 1.117 Gm. of the liquor and 7.5 per cent, of this should be metallic iron, we find it to be 0.0837 + Gm.,f thus proving our answer. Exercise.—What percentage of anhydrous ferric acetate is con- tained in the official Liquor Ferri Acetatis? According to the equation, page 228,111.7 parts of metallic iron (contained in Fe2(SO4)3) are necessary to the formation of one molecule of ferric acetate (Fe2(C2H3O2)6 = 464.9). * See Decinormal Solution of Sodium Hyposulphite. t A plus (+) sign after a decimal fraction means that the last decimal is slightly smaller than the true value. A minus (—) sign placed in the same manner means that the last decimal is slightly greater than the true value. 230 HANDBOOK OF PHARMACY. 1000 grammes of the solution of ferric sulphate taken contain 80 grammes of metallic iron (8 per cent, of 1000); then, as 2 Iron.* Ferric Acetate. Iron. Ferric Acetate. 111.7 : 464.9 : : 80 : x x = 333 + Gm. ferric acetate. Since the solution is made to weigh 1000 Gm., and contains 333 Gm. of the salt, 333 -s- 10 = 33.3 per cent. The solution should therefore contain 33.3 per cent, of the salt. This figure is not attained in actual practice. Liquor Ferri Chloridi (Liquor Ferri Sesquichloridi Ph. Germ., Liquor Ferri Perchloridi Ph. Br.).—This solution should contain, according to the U. S. Pharmacopoeia, 37.8 per cent, of anhydrous salt (Fe2Cl6). The reaction consists first in the formation of ferrous chloride: — (a) Fe + 2HC1 = FeCl2 + H2 Iron. Hvdrochloric Acid. Ferrous Chloride. Hydrogen. 55.8 ' 2 X 36.3 126.6 To convert this ferrous into ferric chloride, more hydrochloric acid is added to the solution, and this is poured into the necessary amount of nitric acid, which oxidizes the hydrogen of the hydro- chloric acid to water, undergoing itself reduction to nitrogen dioxide (N2O2 or NO), which with the oxygen of the air forms nitrogen tetroxide (N2O4 or NO2), and is evolved as such, while the chlorine liberated from the hydrochloric acid unites with the ferrous to form ferric chloride, thus: — (&) 6FeCl2 + 6HC1 + 2HNO3 — 3Fe2Cl6 + 4H2O + 2NO Ferrous Chloride. Hydrochloric Acid. Nitric Acid. Ferric Chloride. Water. Nitrogen 6 X 126.6 6 X 36.3 2 X 62.9 3 X 324 Dioxide. The solution is then further heated, to remove any excess of nitric acid or nitric oxide, then afterward tested for the presence of these by the addition of a crystal of ferrous sulphate to a few drops of the solution diluted with a little water, mixed with an equal volume of sulphuric acid, and allowed to cool. A dark- brownish zone (FeSO4.NO) forms around the crystal if any nitric acid be present. Should such be the case, it is necessary to heat the solution further. Care should be taken not to allow the liquid to become too concentrated, nor to employ too high a degree of heat (it should not boil), nor to heat too long, otherwise a portion of the iron will be converted into oxychloride, which separates on the addition of alcohol. The Pharmacopoeia directs that the solution be free from ferrous chloride. This is detected by adding a few drops of potassium ferricyanide T. S. to about the same quantity of the solution well diluted with water, when no blue coloration or precipitate should occur:— 3FeCl2 + 2(K3(FeCy6)) = Fe3(FeCy6)2 + 6KC1 Ferrous Potassium Ferrous Ferricyanide, Potassium Chloride. Chloride. Ferricyanide. Turnbull’s blue. *For sake of convenience and brevity, the various atomic and molecular weights are expressed only to the first decimal point; in some instances the nearest whole number is selected. AQUEOUS SOLUTIONS. 231 Assay.—The process is identical with that given under Liquor Ferri Acetatis. One Cc. of decinormal sodium hyposulphite V. S. (0.02476 Gm. of the salt) is equivalent to 0.00558 Gm. of iron, hence 26 Cc. = 26 X 0.00558 = 0.14508 Gm. of iron. Since, according to the Pharmacopoeia, the solution should contain 13 per cent, of metallic iron, and 1.12 Gm. were taken for assay, then this should contain 0.145 + Gm. of iron (13 per cent, of 1.12). Hence, according to the above, the solution is of proper strength. Exercise.—How much anhydrous ferric chloride can be made from 150 Gm. of pure* iron wire? According to the equation a (page 230), 55.8 parts of iron will yield 126.6 parts of ferrous chloride; hence 150 Gm. of iron will yield 340 + Gm. of ferrous chloride:— Fe FeCl2 Fe FeCl2 55.8 : 126.6 : : 150 : x x = 340 4- grammes of ferrous chloride. According to the equation b, 759.6 parts of anhydrous ferrous chloride, when oxidized, yield 972 parts of anhydrous ferric chloride; 340 + Gm. of ferrous will yield 435.4 Gm. of ferric chloride:— 6FeCl2 3Fe2Cl6 FeCl2 Fe2Cl6 759.6 : 972 : : 340 : x x = 435 +. Therefore, 435 + Gm. of ferric chloride can be obtained from 150 Gm. of iron if it be absolutely pure. Exercise.—How much iron is capable of being taken up by 540 Gm. of hydrochloric acid (U. S. P.) to form ferrous chloride. According to the equation a (page 230), 72.6 parts of absolute hydrochloric acid are able to combine with 55.8 parts of metallic iron. If the sample of acid be of U. S. Pharmacopoeia strength, it will contain 172.2 + Gm. of absolute acid (31.9 per cent, of 540). HCl Fe HCl Fe 72.6 : 55.8 : : 172.2 : : x x = 132.3 Gm. Fe. Therefore, 540 Gm. of hydrochloric acid (U. S. P.) will com- bine with 132.3 Gm. of pure iron to form FeCl2. AU Ferric Solutions are Incompatible with the Alkali Bromides or Iodides, since Free Bromine or Iodine is Liberated. Liquor Ferri Citratis.—The preparation of this solution depends on the fact that freshly precipitated ferric hydrate is soluble in the organic acids, in this instance citric acid. The ferric hydrate is prepared by pouring a diluted solution of ferric sulphate into wTell-diluted ammonia water, which must be in * The finest piano wire contains about 99 per cent, of pure iron, but in the above given calculations it is assumed to be absolutely pure (100 per cent.). 232 HANDBOOK OF PHARMACY. slight excess. The precipitated ferric hydrate is well washed, to free it from adhering ammonium sulphate:— Fe2(SO4)3 + 6NH3 + 6H2O = Fe2(OH)6 + 3(NH4)2SO4 Ferric Ammonia Water. Ferric Hydrate. Ammonium Sulphate. Sulphate. To be certain that all traces of ammonium sulphate have been removed, the wash-water acidulated with hydrochloric acid is tested with barium chloride T. S., which should not give a white cloud or precipitate (BaSO4). In the above case we employ di- luted cold solutions, in order to obtain a light flocculent precipi- tate, which is more readily dissolved by the citric acid:— Fe2(OH)6 + 2(H3C6H5O7 + H2O) = 2(Fe2(C6H5O7)2) + 8H2O Ferric Hydrate. Citric Acid. Ferric Citrate. Water. Care should be taken that the solution be not heated above 60° C., otherwise insoluble oxycitrates will form. When this solu- tion is employed in making scale salts, the operator should satisfy himself that the ferric sulphate solution is of full strength, other- wise the citric acid will not be sufficiently saturated and fail to “scale.” The solution is used in making the scale salts Ferri Citras and Ferri et Ammonii Citras. Assay.—On adding 1.117 Gm. of the solution to water and hydrochloric acid, the citric acid is liberated and ferric chloride is formed; thus :— Fe2(C6H5O7)2 + 6HC1 = Fe2Cl6 + 2H3C6H5O7 Ferric Citrate. Hydrochloric Ferric Citric Acid. 2 X 55.8 Fe. Acid. Chloride. 2 X 55.8 Fe. Then, on addition of the potassium iodide, iodine is liberated and ferrous chloride with potassium chloride are formed:— Fe2Cl6 + 2KI = 2FeCl2 + 2KC1 + I2 Ferric Chloride. Potassium Iodide. Ferrous Chloride. Potassium Chloride. Iodine. 2 X 55.8 Fe. 2 X 126.5. The liberated iodine is then estimated by dropping in decinor- mal solution of sodium hyposulphite in presence of starch, until the blue color disappears:— 2(Na2S2O3.5H,O) -f- I2 = 2NaI + Na2S4O6 + 10H2O Sodium Hyposulphite. Iodine. Sodium Iodide. Sodium Tetrathionate. Water. 2 X 247.6 2 X 126.5 One molecule of sodium hyposulphite (247.6 parts) unites with one atom of iodine (126.5 parts), this.being liberated by one atom of iron (55.8 parts). Therefore, one molecule of the hyposulphite (247.6 parts) corresponds to one atom of iron (56.8 parts). Then if 247.6 parts of hyposulphite = 55.8 parts of iron, (1000 Cc.) 24.76 “ “ = 5.58 “ (100 Cc.) 2.476 “ “ “ = 0.558 “ “ “ (10 Cc.) 0.2476 “ “ “ = 0.0558 “ “ “ (1 Cc.) 0.02476 “ “ “ = 0.00558 “ “ “ 15 Cc. of the decinormal solution = 15 X 0.00558 = 0.0837 Gm. metallic iron. AQUEOUS SOLUTIONS. 233 Having taken 1.117+ Gm. of the solution, this would indicate that it contains about 7.5 per cent. [(0.0837 -4- 1.117) X 100] of metallic iron; or, 7.5 per cent, of 1.117 Gm. — 0.0837 + Gm., the amount of metallic iron it should contain. Exercise.—How much of 10 per cent. Ammonia Water is neces- sary to completely precipitate 100 Gm. of solution of ferric sul- phate, U. S. P. ? The 100 Gm. of ferric sulphate solution contain 8 Gm. of iron (8 per cent.). 1 molecule of ferric sulphate con- tains 2 atoms of iron (2 X 55.8), which require 6 molecules (6 X 17) of ammonia for precipitation. Hence, one atom (55.8 parts) of iron will require 3 molecules (3 X 17 parts) of ammonia:— Fe 3NH3 Fe NH3 55.8 : 51 : : 8 : x x = 7.31 Gm. NH3 7.31 Gm. of ammonia gas correspond to 73.10 Gm. of 10 per cent, ammonia water. Hence, 73.10 Gm. of 10 per cent, ammonia water are necessary to precipitate 100 Gm. ferric sulphate solution, U. S. P. Liquor Ferri et Ammonii Acetatis (Basham’s Mixture).—On mixing the ferric chloride and ammonium acetate solutions an interchange of radicals takes place, with the formation of ferric acetate and ammonium chloride, a beautiful red-colored, clear solution resulting. When made according to our present Phar- macopoeia, it is stable and can be kept almost indefinitely; for- merly, difficulties arose from the use of an alkaline solution of ammonium acetate and an insufficient amount of acetic acid; hence, on mixing the two, a precipitate of basic ferric acetate occurred either at once, or very soon afterward. The preparation should be dispensed fresh. Liquor Ferri Nitratis.—This solution is made by dissolving ferric hydroxide in nitric acid: Fe2(OH)6 + 6HNO3 = Fe2(NO3)6 + 6ILO,—a safe and agreeable method, and preferable to the shorter process of the British Pharmacopoeia, in which the iron wire is dissolved in nitric acid. The last-mentioned reaction, being violent, requires great caution ; moreover, the fumes evolved are also annoying. This preparation is more astringent than the salts of iron with the organic acids. Liquor Ferri Subsulphatis (Monsel’s Solution).—This is an aqueous solution of basic ferric sulphate. It is sometimes called persulphate of iron solution, which is inaccurate, and liable to be confounded with the solution of tersulphate of iron. On adding the pulverized ferrous sulphate to the heated mixed acids, the solution becomes of a black color, due to the uniting of the nitric oxide with the ferrous sulphate (FeSO4.NO), which quickly dis- appears with evolution of red nitrous vapors. Should the solution remain of a dark (black) color, after all the ferrous sulphate has 234 HANDBOOK OF PHARMACY. been added, the addition of a few drops of nitric acid will be suffi- cient to cause the evolution of the nitric oxide, and the solution will then appear of a clear reddish-brown color. The tests for nitric acid and ferrous salt are the same as those given under Solution of Ferric Chloride. This solution contains a lesser amount of sul- phuric acid and more of ferrous sulphate than the tersulphate of iron, hence, instead of the normal ferric sulphate, a basic or oxy- sulphate (probably Fe4O(SO4)5) is obtained. On standing, this solution sometimes deposits a sediment; this may be redissolved by placing the bottle in hot water. This solution may be distin- guished from the tersulphate by adding one volume of sulphuric acid to two of the solution, when in the case of the subsulphate a white, heavy precipitate of basic or oxysulphate will be pro- duced. The dry persulphate (Monsel’s Powder) is obtained by evaporat- ing the solution to dryness and powdering. Both the solution and powder are used as local styptics in cases of hsemorrhage. Liquor Ferri Tersulphatis.—A solution of normal ferric sulphate, or solution of persulphate of iron. This solution is weaker in iron and contains more sulphuric acid than Monsel’s solution. It should contain about 28.7 per cent, of Fe2(SO4)3. On adding the ferrous sulphate (powdered), in portions, to the heated mixture of sulphuric and nitric acids, effervescence takes place, with evolution of vapors of nitric oxide (NO or N2O2). When all of the iron has been added, the solution should be clear and of a dark reddish-brown color. Should it be of a black color (FeSO4.NO), this indicates that there is not a sufficient amount of nitric acid present to oxidize all of the ferrous to ferric sulphate, hence nitric acid should be added drop by drop until effervescence ceases and the solution clears up. The reaction takes place as follows: — 6FeSO4+7H2O + 3H2SO4 + 2HNO3 = 3Fe2(SO4)3 + N2O2 + 11H2O Ferrous Sulphate. Sulphuric Nitric Acid. Ferric Sulphate. Nitric Oxide. Water. 6 X 277.4 Acid. 3 X 399.2 Assay.—The process of assay is identical with that given under solution of Ferric Acetate or Chloride. Exercise.—How many grammes of ferric sulphate (Fe2(SO4)3) can be prepared from 400 Gm. of ferrous sulphate, FeSO4-|-7H2O ? Since according to the equation given above, 1664.4 parts of ferrous sulphate yield 1197.6 parts of ferric sulphate, hence Ferrous Sulphate. Ferric Sulphate. 1664.4 : 1197.6 :: 400 : x Therefore x — 287 + grammes of ferric sulphate can be made from 400 grammes of ferrous sulphate. Now, if this solution is made up so as to weigh 1000 Gm. (U. S. P.) it would necessarily contain 28.7 per cent, of the salt. Liquor Hydrargyri Nitratis, or Solution of Mercuric Ni- A Q UJEOUS SOL ULLOA'S. 235 trate.—This solution is prepared by dissolving red mercuric oxide or metallic mercury in nitric acid:— HgO + 2HNO3 = Hg(NO3)2 4- H2O. Mercuric Oxide. Nitric Acid. Mercuric Nitrate. Water. 215.7 323.6 If 40 Gm. of mercuric oxide are taken, we would obtain about 60 Gm. of mercuric nitrate:— HgO Hg(NO3)2 HgO Hg(NO3)2 215.7 : 323 6 : : 40 : x x — 60 4~ Gm. If the solution be made up to the weight of 100 Gm. (U. S. P.), it would then contain about 60 per cent, of this mercuric nitrate. This solution is employed as a caustic. Liquor Iodi Compositus (Lugol’s Solution, or Compound Solu- tion of Iodine).—Free iodine is readily dissolved by an aqueous solution of potassium iodide. In the U. S. P. preparation we find 5 per cent, of iodine, and 10 per cent, of potassium iodide present. This is the best preparation adapted to the internal administra- tion of iodine, as it does not precipitate when added to water. This solution is a valuable reagent in testing for the presence of alkaloids in solution, since the latter unite with the iodine, forming insoluble double salts of a brown color. This fact should be remembered when Lugol’s solution is directed to be added to any preparation containing an alkaloid. Assay.—The amount of free iodine contained in this solution is estimated by titrating with decinormal solution of sodium hypo- sulphite in presence of starch ; the end of the reaction being known by the disappearance of the blue color (iodide of starch). The reaction that takes place is as follows:— (Na2S2O., + 5H2O) 4- 21 = 2NaI + Na2S4O6 4- 10H2O Sodium Hyposulphite. Iodine. Sodium Sodium Tetrathionate. Water. 2 X 247.6 2 X 126.6 Iodide. Sodium Hyposulphite. Iodine. 2 X 247.6 parts 2 X 126.6 parts. 247.6 “ 126.6 “ 1000 Cc. V. S. 24.76 Gm 12.66 Gm. 1. Cc. * V. S. 0.0248 Gm 0.01266 Gm. If 50 Cc. of the Hyposulphite solution were consumed in de- colorizing 12.66 Gm. of the Lugol’s Solution, then the amount of iodine present in the sample would be 50 X 0.01266 — 0.633 Gm., corresponding to 5 per cent [(0.633 -h 12.66) X 100]. Liquor Magnesii Citratis.—On bringing citric acid and magnesium carbonate in contact in presence of water, carbonic acid gas is given off, and magnesium citrate is formed; according to the proportions of the two, either the acid (MgHC6H5O7) or normal (Mg3C6H5O7) salt or a mixture of the two is formed. The first-mentioned is the more desirable, because of its solubility and the greater permanence of the solution. When the solution 236 HANDBOOK OF PHARMACY. contains less soluble normal salt, it will not keep well for any length of time. The pharmacopoeial preparation contains both the acid and normal salts, and is not calculated to keep long without precipitation. It would be well to increase the amount of citric acid by about 3 Gm. There should be sufficient citric acid pres- ent in this solution to combine with the magnesia, as well as to react with the potassium bicarbonate, so as to produce the neces- sary amount of carbonic acid, which is so desirable in this solu- tion. Boiled or distilled water only should be used in making this preparation.* Liquor Plumbi Subacetatis (Goulard’s Extract, Acetum plumbicum or saturninum). On boiling lead acetate and oxide with water, there are obtained, according to the relative propor- tions of the two, various basic lead acetates, that of the U.S. P. being Pb(C2H,O2)2 + 3H2O + PbO = Pb2O(C2H3O2)2 + 3H2O Lead Acetate. Litharge. Lead oxyacetate. Water. 378 222.36 546.4 If 170 Gm. of lead acetate are employed, 245.74 Gm. of sub- acetate (oxyacetate) are obtained :— Lead Acetate. Lead Oxyacetate. Lead Acetate. Lead Oxyacetate. 378 : 546.4 : : 170 : x x — 246 Gm. Subacetate of Lead. If the solution be made up to 1000 Gm., it will contain about 24.5 per cent, of the subacetate. This solution is not of constant strength, since it readily absorbs carbonic acid, which precipitates the lead as carbonate. It should be prepared in a flask, in order to avoid contact with air as much as possible; only boiled distilled water should be employed in order to avoid any decomposition of the lead acetate from carbonic acid that may be present. The litharge should be first tested for car- bonate by the addition of a little diluted nitric acid, and any sample which contains it should not be employed. Solution of lead subacetate is incompatible with hydrochloric or sulphuric acid or preparations containing these; also with the soluble iodides, bromides or chlorides, alkalies, mucilage of acacia, many organic acids, tannin, and vegetable solutions (in- fusions, fluid extracts, etc.), which contain much coloring matter. Exercise.—How much litharge should be taken to convert 170 Gm. of lead acetate into subacetate? Since 378 Gm. of lead acetate require 222.36 Gm. of litharge to form the official subacetate, 170 Gm. of lead acetate will require 100 Gm. of litharge:— Lead Acetate. Litharge. Lead Acetate. Litharge. 378 : 222.3 : : 170 : x x — 100 (practically). *It is also to be noted that the quantity of Syrup of Citric Acid should be reduced one-half (to 60 Gm.), the amount printed in the earlier issues of the U. S. P. (120 Gm.) being an error. AQUEOUS SOLUTIONS. 237 Assay.—The U. S. P. directs the assay of this solution by means of normal sulphuric acid, the reaction being as follows:— Pb2O(C2H3O2)2 + 2H2SO4 = 2PbSO4 + 2HC2H3O2 + H2O Lead Subacetate. Sulphuric Acid. Lead Sulphate. Acetic Acid. Water. 546.4 2 X 97.8 Two molecules of sulphuric acid (2 X 97.8) are equivalent to one molecule of lead subacetate (546.4), hence:— Sulphuric Acid—H.2SO4. Lead Subacetate—Pba0(C2H302)2. 1 molecule, 97.8 p, 273.2 p. (J of 546.4). 1000 Cc. V. S. = 48.9 Gm136.6 Gm. (J of 273.2). 1 Cc. V. S. = 0.489 Gm 0.1366 Gm. 25 Cc V. S. = 25 X 0.1366 = 3.415 Gm. of lead subacetate, and since 13.67 Gm. of solution of Lead Subacetate were taken, it would then contain about 25 per cent, of the salt [(3.415 h- 13.67) X 100] ; or 25 per cent, of 13.67 = 3.41 -f- Gm.). Liquor Plumbi Subacetatis Dilutus, (Lead Water; Aqua plumbica or saturnina).—This is prepared by simply diluting the preceding solution -with water, which should, however, be distilled and previously boiled; otherwise the solution will become turbid, and lose in strength, owing to a precipitation of a portion of the lead as carbonate. Liquor Potassje.— This is an aqueous solution containing about 5 per cent, of Potassium Hydrate (KOH). Besides the rapid method of dissolving the stick potassa in water, the Phar- macopoeia directs it to be prepared from potassium carbonate, which in turn is made from the bicarbonate by boiling the latter with water; through loss of carbonic acid it is converted into normal carbonate:— 2KHCO3 = K2CO3 + CO2 + h2o. 2 x 99.88 137.9 This solution is then boiled with slaked lime, CaO + H2O = Ca(OH)2, giving rise to potassium hydrate and calcium carbonate, thus:— Ca(OH)2 + K2CO3 = CaCO3 + 2KOH Calcium Potassium Calcium Potassium Hydrate. Carbonate. Carbonate. Hydrate. 137.9. 2 X 56. The solution is allowed to stand until clear, and decanted off from the precipitated calcium carbonate, or it may be directly filtered through spun glass or asbestos (fibrous). The commercial potassium carbonate (salt of tartar) contains silica and other impurities, hence the Pharmacopoeia prefers to employ the pure bicarbonate. When prepared from the ordinary stick potassa, the solution is liable to deposit a gelatinous precipitate of silica on standing. The purest form of potassa in the market is that which is purified by alcohol, made by treating the commercial product with alcohol, which leaves the silica, carbonates, chlor- ides, etc., undissolved. The solution should be preserved in rubber-stoppered vessels, or should glass stoppers be used, they 238 HANDBOOK OF PHARMACY. should be well greased with petrolatum. The solution readily absorbs carbonic acid from the air. It is incompatible with all solutions containing alkaloids, salts of metals, and also acids. Assay.—The strength of this solution is estimated by its neutraliz- ing power on normal sulphuric acid, according to the following equation:— H2SO4 + 2KOH = K2SO4 + 2H2O Sulphuric Potassium Potassium Water. Acid. Hvdrate. Sulphate. 97.8. 2'x 56. As two molecules of potassium hydrate neutralize one molecule of sulphuric acid, hence, one molecule of potassa will neutralize half a molecule of sulphuric acid. Sulphuric Acid Potassium Hydrate—KOH. 1000 Cc. containing 48.9 p., 56 p. 1 Cc. V. S. containing 0.0489 Gm., 0.056 Gm. 25 Cc. V. S. containing 25 X 0.56 — 1.40 Gm. potassium hydrate ; now if 28 Gm. of the solution were taken, it would then contain 5 per cent, of the anhy- drous salt [(1.4 -5- 28) X 100], or 5 per cent, of 28 = 1.40 Gm. Exercise.—How much potassium hydrate can be made from 90 Gm. of potassium bicarbonate? Since, according to the equation, 199.7 parts (2 X 99.88) of KHCO3 yield 137.9 parts of K2CO3, hence, 90 Gm. of KHC03 will yield 62.1 + Gm. of K2CO3:— khco3 k2co3 khco3 k2co3 199.7 : 137.9 : : 90 : x ; x = 62.1 + Again, since 137.9 parts of K2CO3 when boiled with excess of slaked lime (Ca(OH)2) will yield 122 parts of KOH (2 X 56), hence, 62.1 -4- Gm. of K2CO3 will under like circumstances yield 50.4 + Gm. of KOH K2CO3 KOH K2CO3 KOH 137.9 : 112 :: 621 : x ; x — 50.4 + If the solution be made up to 1000 Gm., it will contain in round numbers 5 per cent, of potassa. Liquor Potassii Arsenitis (Fowler’s Solution).—This solu- tion contains 1 per cent.* of arsenous acid (As2O3) in solution as potassium arsenite (K2As2O4). On boiling potassium bicarbonate and arsenous acid together, the following reactions probably take place:— (a) 2KHCO3 4- As2O3 + Aq — 2KAsO2 + 2CO2 + H2O + Aq. Potassium metarsenite. or (5) 4KHCO3 + As2O3 + 3H2O = 2K2HAsO3 + 4H2O + 4CO2. Potassium Arsenous Acid Potassium Bicarbonate. Acid. Orthoarsenite. The German and British pharmacopoeias employ normal po- tassium carbonate instead of the bicarbonate; a slight excess of alkaline carbonate remains in the solution. This solution should * Practically 1 per cent., there being 10 Gm. of As2O3 in 1000 Cc. of solution, which weighs 1009 Gm. AQUEOUS SOLUTIONS. 239 not be kept longer than a year at the most, since it becomes weaker in therapeutic effect, owing to the gradual oxidation of the arsenotis to arsenic acid; the arsenic salts being less potent than the arsenous. The solution should therefore be kept in well filled bottles. Only the pure arsenous acid in lumps should be used, and not the commercial, which is very often adulterated or impure. The object of adding compound tincture of lavender is to im- part sufficient taste and color to the solution to prevent its being mistaken for water. The solution is incompatible with salts of iron, magnesium and calcium. In cases of arsenical poisoning, emetics, calcined mag- nesia or the official arsenic antidote, viz., ferric hydrate with mag- nesia, should be administered as soon as possible. The two latter form insoluble, inert double compounds with soluble arsenic salts. Assay.—The pharmacopoeial method consists in adding deci- normal iodine V. S., to the solution of arsenous salt containing an excess of sodium bicarbonate and mixed with a little starch, until the blue color produced ceases to disappear. The addition of iodine to arsenous acid in alkaline solution causes its oxida- tion to arsenic acid, the iodine thereby being reduced to hydri- odic acid, with disappearance of color. As soon as all of the arsenous is oxidized to arsenic acid, then the next drop of iodine (which is free) will strike a blue color with the starch added to the solution. The reaction is as follows :— AsA + 41 + 4NaHCO3* = As2O5 + 4NaI + 4CO2 + 2H2O Arsenous Iodine. Sodium Arsenic Sodium Carbonic Water. Oxide. 4 X 126.5 Bicarbonate. Oxide. Iodide. Acid. 197.68 The addition of the extra 2 Gm. of sodium bicarbonate serves the purpose of combining with the liberated hydriodic acid, which, if present in free condition, would interfere with the reac- tion. From the equation we see that 4 atoms of iodine (4 X 126.5) are necessary to oxidize one molecule (197.68) of arsenous to arsenic oxide. Hence, one atom of iodine is equivalent to | of a molecule of arsenous oxide. Iodine. Arsenous Oxide. 126.5 parts 49.42 parts. N 1000 Cc. 10 V. S. 12.65 Gm 4.942 Gm. 1 Cc. V. S. 0.01265 Gm 0.004912 Gm. 50 Cc of V. S. Iodine = 50 X 0.004942 = 0.247 + Gm., AsA Hence, if 24.7 Cc. of the solution had been taken, and 0.247 Gm. of arsenous oxide were found contained in it, then the solu- tion must be of 1 per cent, Exercise.—If 10 Gm. of a sample of Fowler’s solution required 18 Cc. of iodine volumetric solution to produce a blue color, * The NaHCO3 merely plays the part of a solvent for the As203, hence the formula KAsO2 or (NaAs02) is not used here, f See Footnote, page 238. 240 HANDBOOK OF PHARMACY. under the conditions given in the U. S. P., what per cent, of ar- senous oxide would it contain? Since 1 Cc. of iodine volumetric solution = 0.004942 Gm. of As2O3, hence, 18 Cc. of iodine volumetric solution = 18 X 0.004942 = 0.0889 + Gm. of As2O3. If 10 Gm. of the solution had been taken, then (0.0889 4- 10) X 100 = 0.8. The sample, therefore, contains T87 per cent, of As2O3. Liquor Potassii Citratis.—The reaction that takes place on mixing solutions of citric acid and potassium bicarbonate is as follows:— 3KHCO3 + H3C6H5O7 + H2O = K3C6H5O7 + H2O 4- 3CO2 Potassium Bicarbonate. Citric Acid. Neutral Potassium Citrate. 3 X 99.8 209.5 305.6 The solution contains neutral potassium citrate with free citric and carbonic acids, the latter imparting a pleasant acidulous taste to the solution. The solution should always be dispensed fresh. Exercise.—How much citric acid will be necessary to neutralize 8 Gm. of potassium bicarbonate; also how much potassium citrate will be produced ? If 299.4 parts of KHC03 require 209.5 parts of H3C6H5O7, then 8 Gm. of KHCO3 will require 5.6 — Gm. of H3C6H5O7:— 3KHCO3 H3C6H5O7 KHCO3 H3CfiH5O7 299.4 : 209.5 : : 8 : x x — 5.6 — If 299.4 parts of KHCO3, when neutralized with citric acid, will yield 305.6 parts of potassium citrate, then 8 Gm. of KHC03 will yield 8.1 + Gm. of K3C6H5O7:— 3KHCO3 k3c6h5o7 khco3 k3c6h5o7 299.4 : 305.6 : : 8 : x a: = 8.1 + Liquor Sodj^.—This solution, like that of potassa, can be made by dissolving the caustic alkali in the necessary amount of water, or by boiling the necessary quantity of the carbonated alkali and slaked lime together with water. Thus :— Na2CO3 + 10H2O + Ca(OH)2 = 2NaOH + CaCO3 + 10H2O Sodium Carbonate. Calcium Sodium Calcium Water. 285.4 Hvdrate. Hydrate. Carbonate. 2 X 40 The method of preparation and preservation, and the incom- patibles, are the same as those given under Liquor Potassse. Assay.—The method of assay is also the same as that of Liquor Potassse:— H2SO4 + 2NaOH = Na.2SO4 + 2H2O Sulphuric Acid. Sodium Hvdrate. Sodium Sulphate. Water. 98.8 2 X 40 Sulphuric Acid. Sodium Hvdrate. 97.8 p. 2 X 40 p. 1000 Cc. V. 8.,48.9 Gm. = 40 Gm. 1 Cc. V. S 0.489 Gm. — 0.040 Gm. 25 Cc. V. 8. H2SO4 = 25 X 0.040 — 1.0 Gm. of sodium hydrate. AQUEOUS SOLUTIONS. 241 Hence, if 20 Gm. of the solution were taken, it would contain 5 per cent, of sodium hydrate [(1.0 20) X 100]. Liquor (Solution of Chlorinated Soda.—La- barraque’s Solution).—The value of this solution depends upon the amount of sodium hypochlorite present, which should yield, according to the U. S. Pharmacopoeia, 2.6 per cent, by weight of available chlorine. The reaction which takes place on mixing the solutions of chlorinated lime and sodium carbonate is most probably as follows:— Ca(OCl)2 + CaCl2 + 2Na2CO3 = 2NaOCl + 2NaCl + 2CaCO:) Chlorinated Lime. Sodium Sodium Sodium Calcium Carbonate. Hypochlorite. Chloride. Carbonate. Hot water is used for the purpose of rendering the precipitate of calcium carbonate as dense as possible, so that it may rapidly settle. Labarraque’s Solution is a superior disinfectant, but it is also employed as an antiseptic. When used as a wash it should be diluted with 5 to 10 parts of water. The addition of acids or acid salts to the solution causes it to give off chlorine gas. It is incompatible with the iodides and bromides, causing a liberation of iodine or bromine; likewise incompatible with many metallic salts and many organic substances. A preparation analogous to this in every respect is the Liquor Potassae Chloratae, or Javelle water. Assay.—The assay method is based on the fact that the chlorine liberates an equivalent amount of iodine from potassium iodide (the chlorine itself being set free by the addition of HC1); this liberated iodine is then estimated by means of decinormal sodium hyposulphite, V. S.* If, then, we know how much iodine has been liberated, the amount of chlorine present is readily calculated. On adding the hydrochloric acid to the solution, all of the available chlorine is liberated :— 2NaOCl + 4HC1 = 2NaCl + 2H2O + Cl2. Then for every atom (35.3) of chlorine liberated, one atom (126.6) of iodine is set free from its combination in the potassium iodide; thus:— 2C1 + 2KI = 2KC1 + I2 Chlorine. Potassium Iodide. Potassium Chloride. Iodine. 2 X 35.3 2 X 126.6 Starch being added to the solution, the latter is colored blue by the free iodine. To this solution is added, drop by drop, the decinormal solution of sodium hyposulphite, until the blue color disappears; thus :— 2(Na2S2O3.5H2O) + I2 = 2NaI + Na2S4O6 + 10H2O Sodium Hyposulphite. Iodine. Sodium Sodium Water. 2 X 247.6 2 X 126.6 Iodide. Tetrathionate. * See Decinormal Sodium Hyposulphite Solution. 242 HANDBOOK OF PHARMACY. Since 247.6 parts of hyposulphite are equivalent to 126.6 parts of iodine, and this is liberated by 35.3 parts of chlorine, one molecule of the hyposulphite is equivalent to one atom of chlorine. 2Na2S2O35H2O 21 2C1 2X247.6 “ 2X126.6 ~ 2X35.3 or 247.6 p. = 126.6 p. = 35.3 p. hence 247.6 p35.3 p. 1000 Cc. of the Sodium Hyposulphite, V.S. = 24.76 Gm. . . 3.53 Gm. 1 Cc. of the Sodium Hyposulphite, V.S. — 0.2476 Gm. . 0.00353 Gm. 50 Cc. = 50 X 0.00353 = 0.1765 Gm. of chlorine. If 6.74 Gm. of the solution were taken, and it were found to contain 0.1765 Gm. of chlorine gas, then the per cent, of available chlorine would be [(0.1765 -s- 0.74) X 100] = 2.6 + per cent. Exercise.—If, in making up Labarraque’s Solution according to the U. S. P., the chlorinated lime taken was found to contain 30 per cent, of available chlorine, what should be the chlorine strength of the finished product? If 75 Gm. of the chlorinated lime are taken, and 30 per cent, of this is available chlorine, then the amount of chlorine in the finished 1000 Gm. of product would be 30 per cent, of 75, or 22.5 Gm. or 2.25 per cent. Hence the solution would contain 2.25 per cent, of available chlorine. Liquor Sodii Arsenatis.*—This is a form of administering the official sodium arsenate (Na2HAsO4), containing 1 per cent, of the salt. The dose, antidotes, and uses are the same as that of Fowler’s Solution. Liquor Sodii Silicatis (“ Soluble Glass”).—This is made by fus- ing together 1 part of fine white sand and 2 parts of dried sodium carbonate, and dissolving the product in boiling water, filtering, and evaporating. It is used in bandaging in surgery. The commercial solution contains about 30 to 35 per cent, of sodium silicate. Liquor Zinci Chloridi (Burnett’s Disinfectant).—Since com- mercial zinc contains iron as an impurity, nitric acid is added to the solution, for the purpose of oxidizing the ferrous to ferric chloride (see page 230). Zn + 2HC1 = ZnCl2 + H2 Zinc. Hydrochloric Acid. Zinc Chloride. Hydrogen. 65 2 X 36.3 135.8 The solution is evaporated to dryness and the residue fused to remove all nitric acid ; some zinc carbonate is then added, where- by the iron is precipitated as insoluble ferric oxide, and this is then filtered off by pouring the solution through a pledget of spun glass or fibrous asbestos. Fe2Cl6 4- 3Zn CO3 = Fe.2(COi3)3 + 3ZnCl2 Ferric Chloride. Zinc Carbonate. Ferric Carbonate. Zinc Chloride. Fe2(CO3)3 = Fe2O3 + 3CO2 Ferric Carbonate. Ferric Oxide. Carbonic Acid. * Pearson’s Solution is sometimes confounded with this, but is ten times weaker, containing about per cent, of anhydrous Sodium Arsenate. AQUEOUS SOLUTIONS. 243 The solution is a powerful disinfectant, also a valuable wash when properly diluted with water. Exercise.—How much anhydrous zinc chloride can be made from 250 Gm. of pure metallic zinc ? Since, according to the above equation, 65 parts of zinc will yield 135.8 parts of zinc chloride, 240 Gm. of zinc will yield 538.3 -f- Gm. of zinc chloride. Zn ZnCl2 Zn ZnCl2 65 : 145.8 : : 240 : x x = 538.3 LIQUORES, U. S. P. Title. Main Constituent.* Synonym. Liquor Acidi Arsenosi, .... Arsenous Acid, 1 %. Ammonii Acetatis, . . Arseni et Hydrargyri Ammonium Acetate, ab. 7 %. Spirit of Mindererus. lodidi, Arsenic Iodide, 1 % ; Mercuric Iodide, 1 %. Donovan’s Solution. Calcis, Ferri Acetatis, .... Ferri Chloridi, .... Ferri Citratis, .... Ferri et Ammonii Ace- Calcium Hydrate, 0.17 %. Anhydrous Ferric Acetate, 31 %. Anhydrous Ferric Chloride, 37.8%. Circa, 43 % Ferric Citrate. Lime Water. tatis, Ferri Nitratis, .... Ammonium Acetate. Anhydrous Ferric Nitrate, 6.2%. Basham’s Mixture. Ferri Subsulphatis, . . Ferri Tersulphatis, . . Hydrargyri Nitratis, . Basic Ferric Sulphate. Ferric Sulphate, 28.7 %. Mercuric Nitrate, 60 %. Monsel’s Solution. lodi Compositus, . . . Magnesii Citratis, . . . Iodine, 5 % ; KI, 10 %. Magnesium Citrates. Lugol’s Solution. Plumbi Subacetatis, Plumbi Subacetatis Lead Subacetate, 25 %. Goulard’s Extract. Dilutus, Potassse, Lead Subacetate. Potassium Hydrate, 5 %. Lead Water. Potassii Arsenitis, . . . Arsenous Acid, 1 %. Fowler’s Solution. Potassii Citratis, . . . Sodte, Anhydrous Potassium Citrate, 9 %. Sodium Hvdrate, 5 %. Neutral Mixture. Sodse Chloratae, .... Available Chlorine, 2.6 %. Labarraque’s Solution. Sodii Arsenatis, .... Sodii Silicatis, .... Sodium Arsenate, 1 %. Sodium Silicate. Hai le’s Solution. Zinci Chloridi, .... Zinc Chloride, 50 %. Burnett’s Disinfecting Solution. * The expression per cent., as employed in some instances, as Liquor Potassii Arsenitis, Acidi Arsenosi, etc., is strictly speaking inaccurate, because in these instances a definite weight of the active agent is contained in a definite volume of product : the volume (expressed in Cc.), does not always correspond to weight (Gm.). For example, the specific gravity of Fowler’s Solution is 1.009, that is, 1000 Cc. weighs 1009 Gm.; it would then coutain per cent, of Arsenous Acid, instead of 1 per cent. See page 137. 244 HANDBOOK OF PHARMACY. INFUSA. Infusions (inf undo, I pour in) are aqueous solutions of the soluble principles of drugs, obtained by maceration in hot or cold water. They differ from decoctions in that a lower degree of heat is employed. Infusions are usually prepared from drugs which contain volatile principles, such as chamomile, valerian, cascarilla, etc., since the process of decoction, requiring a higher degree or a longer application of heat, would not only destroy these principles, but also extract much inert starchy and extractive matter. The drug should be in a coarsely comminuted condition for hot infusions; for cold infusions, where percolation is resorted to, the drug should be in coarse powder. Infusions are usually made by pouring pure water upon the drug contained in a suitable well-covered vessel, then allowing it to stand (macerate) until cold, or for a specified period (for instance, one-half hour), as directed in the U. S. P. Other Phar- macopoeias direct that after the addition of boiling water the vessel (well closed) be placed on a steam-bath and allowed to “ digest” for 5 or 10 minutes. The process of cold percolation is employed only in the U. S. Pharmacopoeia (Infusum Cinchonse, Infusum Pruni Virginianae). The general strength of infusions, unless otherwise specified (as should be done in the case of potent drugs), is 1 part of the drug, in coarsely comminuted condition, to 20 parts of the finished product. The twenty parts of boiling water are poured upon the drug, and the mixture allowed to macerate for half an hour. It is then strained, with little or no pressure, enough hot water being poured through the strainer to make the product up to the desired quantity. In preparing infusions of aromatic drugs or of such as contain volatile principles, the operator should exercise some judgment and care, for in these cases prolonged contact with hot water may injure or destroy these principles, and too high a temperature may extract starch and inert matter. Infusions are best prepared by suspending the drug contained in a porous container* in the upper part of the infusion vessel, thereby securing its exhaustion by means of circulatory displace- ment. The Water, on becoming saturated, sinks to the bottom, displacing a fresh portion, which rises so as to come into contact with the drug. This method renders it unnecessary to stir the mixture. Such a form of infusion pot is found in that devised by Squire (Fig. 325), which consists of a plain porcelain pot, in which is suspended a perforated diaphragm for holding the drug, the whole being covered by a well-fitting lid. The hot or cold water is poured into the pot until the drug is just covered; the pot is then covered and set aside for the specified time, when the * The drug must be coarse enough not to fall through the perforations. AQUEOUS SOLUTIONS. 245 infusion is poured off. If the volume is not sufficient, an addi- tional quantity of water is poured over the drug until the desired quantity is obtained. When such a mug is not at hand, an ordinary porcelain teapot may be used, in which the drug, con- tained in a bag of cheese-cloth, is suspended (by means of a string, through the hole in the lid) in the hot water. Both of these methods render straining unnecessary. Fig. 326 illus- trates another form of tinned copper infusion mug in which the inner vessel, a-d, is suspended in an outer bath, b-c, which contains boiling water, the entire vessel being placed upon a gas stove. The process of percolation is employed in making infusions of those drugs the active principles of which are readily taken up by cold water. Percolation can be successfully applied to infu- Fig. 325. Fig. 326. Infusion Mug with Bath. Squire’s Infusion Mug. sions, since the proportion of water to drug is relatively very large; hence exhaustion is insured. Infusions which contain volatile oils will keep much longer and better than those not containing them, or those in which albumin- ous and mucilaginous matters predominate. Preservative agents, such as alcohol, boric or salicylic salts, etc., should not be used unless specially ordered ; it is often advisable to heat the infusion to the boiling point, and to transfer it, while hot, to small bottles, which should be entirely filled, corked, and sealed. Infusions should not be made from fluid extracts. An aqueous infusion of a drug will often have an entirely differ- ent therapeutic effect from an alcoholic or hydro-alcoholic prepar- ation of the same, since the different menstrua will dissolve out 246 HANDBOOK OF PHARMACY. different principles or different proportions of the principles. Thus, an aqueous infusion of digitalis is a powerful diuretic, while a preparation made by adding the corresponding amount of fluid extract or tincture of digitalis to water will be but feebly diuretic, but act powerfully upon the heart. Moreover, the addition of concentrated alcoholic or fluid ex- tracts to water is nearly always accompanied by precipitation, which renders the preparation so unsightly as to necessitate filtra- tion, and this, if done, will often remove, practically, most of the activity, the result being a worthless preparation. Besides, the introduction of alcohol into the preparations which is caused thereby, is, in many cases, seriously objected to by the physician. It is a direct violation of the pharmacopoeia! instructions and of the intentions of the physician. Infusions are incompatible with salts of the heavy metals, such as iron, mercury, silver, etc. INFUSA, U. S. P. Title. Per Cent, of Active Constituent.* Properties—Dose. By Maceration. Infusum Digitalis, . . Infusum Senns Com- Digitalis, 1.5 %. Diuretic, etc., 4 to 15Cc. positum, Senna, 6 % ; MgSO4 and Manna, each 12%. Purgative, 30 to 80 Cc. By Percolation. Infusum Cinchonae, . . Infusum Pruni Virgini- Cinchona, 6 %. Tonic, 30 to 60 Cc. ans. Wild Cherry Bark, 4 %. Tonic, Sedative, 30 to 90 Cc. * See Footnote on page 225. AQUEOUS SOLUTIONS. 247 DECOCTA. Decoctions (decogw, I boil thoroughly) are aqueous solutions of the soluble matter of drugs, obtained by boiling with water. Decoctions are prepared from those drugs the active principles of which are not materially injured or dissipated by heat and are not readily extracted by cold or warm water. The process should be performed with care, so as to avoid subjecting the drug to too high a degree or too long an application of heat, for it must not be forgotten that with increase of the amount of extractive present the boiling point rises. Earthenware vessels are generally preferred for making decoc- tions. However, tinned copper answers just as well. The general method for the preparation of decoctions when the strength is not specified (which should be done in the case of potent drugs) is as follows: The substance (1 part), in a coarsely comminuted condition, is placed in a suitable vessel provided with a well-fitting cover, together with 20 parts of cold pure water. The vessel is then covered and the contents boiled for fifteen minutes. When the temperature has fallen to about 40° C.,the mixture is expressed and strained, and sufficient cold water passed through the strainer to make the finished product measure 20 parts by volume. On standing, decoctions usually deposit a sediment which should not be removed. What has been said about the preserva- tion and incompatibles of infusions, may also be applied to decoc- tions. Decoctions should, for like reasons, not be prepared from fluid extracts. Title. Per Cent, of Main Constituents* Properties. Decoctum Cetrarise, . . . “ Sarsaparill ae Iceland Moss, 5 %. Demulcent. Compositum, Spl’a., 10 % ; Sasf., 2 % ; Guaiac, 2 °/o ; Glycyr., 2% ; Mezereum, 1 %. Alterative. DECOCTA, U. S. P. * See Footnote on page 225. 248 HANDBOOK OF PHARMACY. MUCILAGINES. Mucilages are aqueous, viscid and adhesive solutions. Under this term, the U. S. Pharmacopoeia understands a solution of a plant gum, or substance of a mucilaginous nature. In other phar- macopoeias this term is made to embrace also solutions of starch and dextrin. Mucilages are very prone to ferment, becoming sour and offensive; they should therefore be made in small quantities, and preserved in well-closed jars in a cool place. These solutions may be prepared by suspending the substance, enclosed in a bag of cheese-cloth, in a vessel of hot or cold water. In some instances it is desirable to employ water impregnated with the soluble parts of tolu (tolu water) as solvent, the presence of the balsam tending to preserve the preparation from fermen- tation. Other preservative agents may sometimes be used, par- ticularly when the mucilage is not intended for internal use. Thus, mucilage of acacia may be preserved by the addition of about 10 grains of chloral to the ounce. Title. Per Cent, of Main Constituents.* Cold Process. Mucilago Acaciae “ Sassafras Medullae . . . Acacia, 34 %. Sassafras Pith, 2 %. Hot Process. Mucilago Tragacanthae f “ Ulmi Tragacanth, 6 % ; Glycerin, 18 % Elin, 6 %. MUCILAGINES, U. S. P. * See Footnote on page 225. fThis may be quickly prepared by placing the powdered tragacanth in a dry graduate, adding sufficient alcohol to form a thin, smooth paste, then pouring in the necessary amount of boiling water, agitating constantly with a spatula until a thin, smooth mucilage results. CHAPTER XXVII. ACETOUS SOLUTIONS. Medicated Vinegars are solutions of medicinal principles in diluted acetic acid (or vinegar). This class of preparations was formerly made by using vinegar as a solvent, but, owing to the presence in the latter of extractive matters, and its variable strength, they were prone to undergo decomposition upon stand- ing. Hence to secure the permanency of the preparation, diluted acetic acid of definite strength has been substituted for vinegar. This has peculiar solvent powers, in that it takes up many organic principles (alkaloids, glucosides, etc.) which are not soluble in water alone. These vinegars, even when prepared with diluted acetic acid, are prone to deposit a sediment and to undergo fer- mentation, for which reason some pharmacopoeias direct the addi- tion of a small amount of alcohol to the finished preparation. The U. S. Pharmacopoeia has adopted the uniform drug strength of 10 per cent., employing the official diluted acetic acid, contain- ing 6 per cent, by weight of absolute acid, as menstruum. There are two vinegars official, viz., Acetum Opii (so-called Black Drop) and Acetum Scillae; these are made by the process of maceration. ACETA—(Vinegars). Title. Active Constituent.* Properties—Dose. Acetum Opii (Black Drop), Opium, 10 %. Sedative, 0.3-1 Cc. Acetum Scillae, Squill, 10 %. Expectorant 1-3 Cc. ♦ See Footnote on page 225. 249 CHAPTER XXVIII. ALCOHOLIC OR HYDROALCOHOLIC SOLUTIONS. SPIRITUS—(Spirits'). Spirits are alcoholic solutions of volatile substances. Accord- ing to the nature of the substance dissolved and the method of procedure, we may divide the 25 official spirits into three classes, viz., those prepared by 1. Solution in Alcohol. 2. Chemical Reaction and Solution. 3. Distillation. The Spirits should be kept in well stoppered vials in a cool place. These are made by dissolving or macerating the substance or substances directly in alcohol. In preparing the so-called essences, only the best quality of volatile oils should be employed; in three instances maceration is called for (Sp. Limonis, Menthae piperitae, and Menthae viridis). 1. SPIRITS PREPARED BY SOLUTION IN ALCOHOL. Title. Active Constituents. {Tie—Dose. Spiritus JEtheris, zEtheris Compositus, | Ammoniae,* f Ether, 32.5 % vol. Ether, 32.5 % vol. Ethereal Oil, 2.5 % vol. Gaseous Ammonia, 10 % wt. Ammonia Carb. Stimulant, 3-10 Cc. Anodyne, 2-6 Cc. Anodyne, 2-6 Cc. Stimulant, 0.5-2 Cc. Ammoniae Aromati- 1 Ammonia Water. cus, Oils, Lemon, Lavender, Nut- Stimulant, 2-4 Cc. I meg. Amygdalae Amarae, . . Oil, 1 % vol. Flavor. Anisi, Oil, 10 % vol. Flavor. Aurantii, Oil, 5 % vol. Flavor. r Oil, Orange, 20 % vol. Flavor. Aurantii Compositus, - Oil, Lemon, 5 yc vol. Oil, Coriander, 2 % vol. Flavor. Flavor. ' Oil, Anise, | % vol. Flavor. Camphorse, Camphor, 16 % wt. Stimulant ; Sedative 0.3 4 Cc. Chloroformi, Cinnamomi, Gaultherise, Glonoini, Chloroform, 6 % vol. Oil, 10 % vol. Oil, 5 % vol. C3H5(NO3)3 1 % wt. Sedative, 0.6-4 Cc. Stimulant, 1 Cc. Flavor. Cardiac Stimulant, 0.06-0.1 Cc. Juniperi, Oil, 5 % vol. Oil, Juniper, 0.4 % vol. Diuretic, 2-4 Cc. Juniperi Compositus, | Oil, Caraway, 0.05 % vol. 1 Oil, Fennel, 0.05 % vol. Diuretic, 7-15 Cc. * Some pharmacopoeias recognize this under the title of Liquor Ammonii Caustici Spirituosus. 250 ALCOHOLIC OR HYDROALCOHOLIC SOLUTIONS. 251 Title. Active Constituents. Use—Dose. Lavandulae, Oil, 5 % vol. Flavor. Liinonis, Oil, 5 % vol.; Peel, 5 % wt. Flavor. Menthae Piperitae, . . Oil, 10 % vol.; Herb, 1 % wt. Carminative, 1-2 Cc. Menthae Viridis, . . . Oil, 10 °/o vol.; Herb, 1 % wt. Oil, Bay, 0.8 % vol. Carminative, 1-2 Cc. Myrciae, Oil, Orange, 0.05 % vol. Oil, Allspice, 0.05 % vol. Perfume. Myristicae, Oil, 5 % vol. Flavor. Phosphori, Phosphorus, 0.12 % wt. Elixir Phosphori. 2. SPIRITS PREPARED BY CHEMICAL ACTION AND SOLUTION. There is but one spirit official which belongs to this class, viz., Spiritus 2Etheris Nitrosi. By the reaction between nitrous acid (derived from sodium nitrite) and alcohol, ethyl nitrite is pro- duced; and this is preserved by solution in alcohol. The solution should contain 4 per cent, of ethyl nitrite. 3. SPIRITS PREPARED BY DISTILLATION. Aside from the two given under this class, some of those of Class 1 may be prepared by distillation, yielding a product of a more delicate flavor and odor than that produced by mere solu- tion. Title. Preparation. Per Cent, of Alcohol. Spiritus Frumenti, . . . Distillation of mash of fer- mented grain, and at least 2 years old. 44 % to 50 % wt., or 50 % to 58 % vol. Spiritus Vini Gallici, . . Distillation of fermented juice of grapes, and at least 4 years old. 39 % to 47 % wt., or 46 % to 55 % vol. EXPLANATORY. Spiritus JEtheris Nitrosi (Sweet Spirit of Nitre).—This is an alcoholic solution of ethyl nitrite (C2H5ONO or C2H5NO2) an or- ganic compound belonging to the class of esters. This was made, according to the U. S. Pharmacopoeia of 1880, by the action of nitric acid on alcohol:— (a) C2H5OH + HNO3 = CH3COH + HN02 4- H2O Alcohol. Nitric Acid. Acetic Aldehyde. Nitrous Acid. Water. (b) c2h5oh + hno2 = c2h5no2 + h2o Alcohol. Nitrous Acid. Ethyl Nitrite. Water. (c) CH3COH 4- HN03 = CH3COOH + hno2 Acetic Aldehyde. Nitric Acid. Acetic Acid. Nitrous Acid. This process is objectionable for two reasons: first, because the operation is difficult to regulate, and dangerous to the inexperi- enced operator; and second, because the product is largely contami- nated with aldehyde (also acetic ether), which soon oxidize to acetic acid, causing a gradual decomposition of the ester. The present pharmacopoeia process possesses the advantage, that it is easily operated and controlled, and that it yields a pure 252 HANDBOOK OF PHARMACY. ethyl nitrite, free from aldehyde and acetic ether. The nitrous acid is produced by the reaction between sodium nitrite and sulphuric acid (NaNO2 + n2SO4 = NaHSO4 + HNO2) in the pres- ence of alcohol; * hence, the liberated acid reacts in statu nascendi upon the alcohol, with immediate production of ethyl nitrite, which distills over, contaminated with alcohol and free nitrous acid. These latter two are removed by pouring the entire distillate into a separating flask containing a solution of the sodium car- bonate in ice-cold water, then washing the ethyl nitrite (which floats on the surface as a yellowish-colored liquid) by rotating (not shaking); the alkaline solution absorbs the alcohol and nitrous acid. The aqueous solution is then drawn off, and any trace of water remaining in the ethyl nitrite is removed by shaking it with a little dry potassium carbonate. This operation should not be performed in the neighborhood of a stove or gas flame, because of the extreme volatility and inflammable nature of the ester. It is well to place the separating flask on ice at intervals while operating. The presence of water and the action of sunlight and air on pure spirit of nitre cause its rapid decomposition (shown by its acid reaction) by the splitting up of ethyl nitrite into nitrous acid and alcohol; hence the preparation should be preserved in well-stoppered vials in a cool and dark place. Spirit of nitrous ether should never be kept in large vessels (carboys), since, owing to its volatile nature, it rapidly loses strength. Acetic acid fre- quently occurs in samples of the commercial spirit; this is due to its having originally contained aldehyde, which, under ordinary conditions, rapidly oxidizes to acetic acid (CH3COH — 0 = CH3- COOH), imparting an acid reaction to the preparation, and caus- ing effervescence when a crystal of potassium bicarbonate is dropped into it. Only the deodorized alcohol of the U. S. P. should be used in this preparation; in the presence of a weaker alcohol, the ethyl nitrite rapidly undergoes decomposition; hence the fraudulent dilution of spirit of nitrous ether with water is a very reprehen- sible practice. Spirit of nitrous ether yields a green color with antipyrine; if it contains any free nitrous acid, it liberates iodine and bromine from their combinations. The presence of traces of nitrous acid may be detected by the blue coloration of guaiac paper. Alkalies, when allowed to remain in contact with the spirit, cause its gradual decomposition. The proportion of nitrous ether in spirit of nitre cannot be ascertained by means of its specific gravity, for the addition of ethyl nitrite (sp. gr. 0.900) to deodorized alcohol (sp. gr. 0.816), increases the specific gravity of the latter the same as does water. * It should be noted that the amount of Sodium Nitrite directed in the formula given by the U. S. Pharmacopoeia is too large. It would be correct if Potassium Nitrite bad been directed. The proper amount is 635 Gm. The specific gravity of Spirit of Nitrous Ether is nearly 0.820, not 0 836 — 0.842 as given in the earlier issues of the U. S. P. ALCOHOLIC OR HYDROALCOHOLIC SOLUTIONS. 253 Assay*—The process of the Pharmacopoeia is that proposed by A. H. Allen, in 1885. It consists in measuring the volume of nitrogen dioxide given off by a known volume of the spirit, when decomposed by the addition of potassium iodide and sul- phuric acid according to the following equation:— c2h5no2 + ki + H2SO4 = C2H5OH + khso4 + i + no Ethyl Nitrite. Potassium Sulphuric Acid. Alcohol. Potassium Acid Iodine. Nitrogen 78.87 Iodide. Sulphate. Dioxide. 29.97 From this it is seen that 78.87 Gm. of ethyl nitrite will yield 29.97 Gm. of nitric oxide, which measures under normal pressure at 0° C. (32° F.) 22327 Cc. One gramme of ethyl nitrite will yield at 0° C. 298.249 Cc. of nitric oxide gas, or 1 Cc. of the gas will represent 0.0033529 Gm. of ethyl nitrite. NO c2h5no2 no c2h5no2 298.249 Cc. : 1.0 : : 1 Cc. : x. x — 0.0033529. It will be observed that the above figures express the volume of the gas at 0° C. As we cannot carry on the opera- tion at this temperature, we must make an allowance for the difference in volume of gas at higher temperatures. Accord- ing to the law, gases increase in volume, or 0.003663 Cc. for each degree Centigrade. For example, let us assume that we have obtained 40 Cc. of gas, the temperature being 20° C., and the baro- metric pressure 740 Mm. It is first nec- essary to reduce this volume to cubic centimeters expressed at 0° C. This is done by dividing the number of cubic centimeters obtained by 1, plus as many times 0.003663 as there are degrees of temperature; thus we divide 40 by 1.07326 [1 + (20 X 0.003663)], whereby we obtain 37.26 Cc., at 0° C., and at the normal barometric pressure of 760 Mm. (30 inches). If accuracy is desired, we must take the degree of barometric pres- sure into consideration, for according to Boyle’s law, “ the temperature remaining the same, the volume of a given quantity of gas is inversely as the pressure it bears.” Hence we may make the necessary correction by multiplying the volume of gas by the number of millimeters (or inches) of pressure and dividing by 760 (or 30). Thus, in this Fig. 327. Alien’s Nitrometer (Curtmann’s Modification). * A very exhaustive article on the assay of spirit of nitrous ether was published by Dr. C. O. Curt- man in the Western Druggist of 1892, p. 244. 254 HANDBOOK OF PHARMACY. example, if the pressure be 740 Mm., the corrected volume would be (37.26 X 740 760) = 36.27 + Cc. If it is desirable to convert this into weight of ethyl nitrite, then we multiply 36.27 Cc. by 0.0033529 (1 Cc. NO = 0.0033529 + Gm. C2H5NO2) = 0.12160 4- Gm. ethyl nitrite. Therefore 40 Cc. of nitric oxide gas at 20° C., and 740 Mm. measure 36.27 Cc. when reduced to 0° C. and 760 Mm. The assay operation is performed with an instrument called a Nitrometer, of which there are several modi- fications, that of Curtman’s design being preferred by the Pharma- copoeia.* Exercise.—A sample of 5 Cc. of spirit of nitrous ether, when assayed by the U. S. P. process, yielded 50 Cc. of nitric oxide gas, the temperature of the room (and that of the liquid in the nitrometer) being 25° C., and the barometric pressure 750 Mm. How much nitric oxide (NO), by volume will it yield, and also what per cent, by weight will it contain of ethyl nitrite? 50 Cc. -4- 1.091575 [1 + (25 X 0.003663)] = 45.85 Cc. (corrected for temperature'). (45.85 Cc. X 750 -4- 760) = 45.24 Cc. Nitric Oxide (corrected for temperature aud pressure. Hence 5 Cc. of the spirit of nitre yield 9.04 + times its volume (45.24 Cc.) of nitric oxide gas. 45.24 Cc. x 0.0033529 = 0.151685 + Gm. Ethyl Nitrite. Spir. Nitre. Ethyl Nitrite. 5 Cc. =4.1 Gm. : 0.151685 :: 100 : x a; = 3.7 % Therefore the sample contains 3.7 per cent, by weight of ethyl nitrite. Exercise.—Were it possible to obtain the theoretical yield with no loss, how much ethyl nitrite could be made from 550 cubic centimeters of deodorized alcohol U. S. P. ? We first ascertain how much 100 per cent, alcohol is contained in 550 Cc. of deodorized alcohol; 550 X 0.816 (sp. gr.) = 448.8 Gm. by weight; 92.5 per cent, of this — 415.14 Gm. of pure alcohol. The reaction takes place according to the equation— c2h5oh + hno2 = c2h5no2 + h2o Alcohol. Nitrous Acid. Ethyl Nitrite. Water. 46 p. 74.8 p. As 46 parts of absolute (100 per cent.) alcohol are capable of yielding 74.8 parts of ethyl nitrite, hence 415.14 Gm. of alcohol wrould yield 675.05 Gm. of ethyl nitrite. Alcohol. Ethyl Nitrite. Alcohol. Ethyl Nitrite. 46 : 74.8 : : 415.14 : x x — 675.05 Therefore, if the conditions above stated could be carried out, we would obtain a yield of 675.05 Gm. of ethyl nitrite. * The instructions for operating this are given in the U. S. P., part iv, page 509. ALCOHOLIC OR HYDROALCOHOLIC SOLUTIONS. 255 Spiritus Glonoini (Liquor Trinitrini B. P.—Spirit of Nitro- glycerin).—This contains 1 per cent, by weight of glonoin (gly- ceryl or propenyl trinitrate), or, as it is more properly known, nitroglycerin. The latter is obtained by the action of a cold mixture of nitric and sulphuric acids on glycerin; the reaction being C3H5(OH3) + 3HNO3 = C3H5(NO3)3 + 3H2O Glycerin. Nitric Acid. Nitroglycerin. Water. Owing to the explosive nature of nitroglycerin, special attention is directed to the precautions given by the Pharmacopoeia in regard to the storage and handling of the Spirit. As a remedy it should be dispensed with caution, being a powerful cardiac stimulant in doses of one to two minims. 256 HANDBOOK OF PHARMACY. VINA MEDICATA—{Medicated Wines). Medicated Wines are a class of preparations similar to tinc- tures, only differing as to menstruum, which is, according to the U. S. Pharmacopoeia, either a dry, white wine (Vinum Album) or a mixture of white wine with alcohol. Red Wine (Vinum Rubrum) does not enter into any of the official medicated wines. Since wines themselves readily undergo fermentation when exposed to the air, the medicated wines, which contain additional extractive matter, are still more prone to de- composition, undergoing acetic and mucous fermentation, becom- ing thereby ropy and sour. In all instances, in order to enhance the stability of the pre- paration, the Pharmacopoeia has directed the addition of alcohol, either direct, or in the flavoring constituent. Though not as stable as the tinctures, the medicated wines present an advantage in being of a lesser alcoholic strength, hence possessing a lower stimulating effect, which, in the case of the tinctures, often inter- feres with the action of certain medicinal agents, such as sedatives, expectorants, etc. The greatest care should be exercised in selecting only the purest wine obtainable, and it should be subjected to the proper tests as specified in the Pharmacopoeia. Medicated Wines, owing to their liability to change, should be made up in small quantities only, and kept in well-stoppered bottles, in a cool place. It is a very important point, in the preparation of medicated wines, to observe that the wine employed be of proper alcoholic strength. With this object in view, the U. S. Pharmacopoeia has given a ready method for the estimation of alcohol in wines, which is also applicable to some tinctures and fluid extracts. In addi- tion to this, there is another accurate method which is often employed by chemists; this consists in mixing a certain volume (say 50 Cc.) of a wine or fluid containing alcohol with an equal bulk of water (neutralizing any free acid that may be present, by the addition of a little chalk), then distilling carefully until a volume of distillate is obtained, equal to that of the sample of wine or fluid taken (50 Cc. as above). This distillate represents the alcoholic strength of the sample, which is readily ascertained by the determination of its specific gravity and then finding the corresponding percentage in the alcoholometric tables. ALCOHOLIC OR HYDROALCOHOLIC SOLUTIONS. 257 VINA MEDICATA, U. S. P. Title. Active Constituents.* Properties. Dose. VlNUM Antimonii, Tartar-Emetic, 0.4 %. Expectorant, 30-60 nt- Colcbici Radicis, . . Colchicum Root, 40 %. Diuretic, 10-60 nt- Col chici Seminis, . . . Colchicum Seed, 15 %. 30-120 m. Ergotae, Ergot, 15 °/o. Emmenagogue, Parturient 3-15 Cc. Ferri Amarum, .... Cit. Iron and Quinine, 5 %. Tonic, 8-15 Cc. Ferri Citratis,.... Cit. Iron and Ammonium, 4%. u 8-15 Cc. Ipecacuanhas, Fl’d. Ext. Ipecac, 10 %. Expectorant, 10-30 PL. Opii, Powd. Opium, 10 %. Sedative, 15-20 nt- Album, Alcohol, 10-14 %, by weight. Base. Rubrum, “ 10-14 %, “ * See Footnote, page 225. 258 HANDBOOK OF PHARMACY. Tinkturen, Germ.; Teintures, Alcooles, French ; Alcoholados, Span. Tinctures are alcoholic or partially alcoholic solutions of the useful constituents of drugs, which are usually not wholly solu- ble in the menstruum. (Tincture of Iodine, Tinct. of Ferric Chloride, and perhaps a few others are included in this class from long custom). Menstruum.—The strength of the menstruum employed in different tinctures varies according to the nature of the drug. Before a suitable menstruum can be selected, the nature of the active constituents of the drug must be studied, and such a sol- vent selected as will take up those principles with as little inert matter as possible, and yet yield a permanent and elegant prep- aration. For this reason, various menstrua are directed by the Pharmacopoeia, and unless for a satisfactory reason, a weaker or stronger menstruum than that directed, should not be employed. The most common menstruum employed is alcohol diluted to different degrees of strength. The alcohol of the U. S. Pharma- copoeia is directed to be of the specific gravity 0.820; that of the British 0.838; of the German, 0.830 to 0.834 ; and of the French, 0.819. In a few instances, the U. S. Pharmacopoeia directs the addition of glycerin to the menstruum; this adds to the perma- nency of tinctures containing tannin-like principles. Such men- strua as aromatic spirit of ammonia and ethereal spirit (ether 7 p., alcohol 3 p.), are also employed, these being known as ammoniated tinctures and ethereal tinctures.* Strength.—The U. S. Pharmacopoeia directs a certain quantity of the air-dried drug, expressed in grammes, to be employed to make 1000 cubic centimeters of the finished tincture. The British Pharmacopoeia directs, on an average, one part (by weight) of the drug to be represented by 8 parts by measure of the finished tincture. In the French, German and Austrian Pharmacopoeias, one part of the drug (by weight) is represented by 5 or 10 parts (by weight) of the tincture. The strength of tinctures prepared from potent drugs varies considerably among different foreign Pharmacopoeias. It is therefore well to bear this important point in mind in dispensing U. S. Pharmacopoeia tinctures in foreign prescriptions. TINCTU R2E—(Tinctures). * Teintures ithiries of the French Pharmacopoeia. ALCOHOLIC OR HYDROALCOHOLIC SOLUTIONS. 259 Tinctura.—100 Parts. Parts of Drug (dry). By Weight. By Measure. U. S. P.» Ph. Ger. Ph. Fr. B.P. Aconiti (leaves) 20 “ (root), 35 10 20 12.5 Aloes, 10 20 2.5 Belladonna Foliorinn, 15 20 5 Cannabis Indicae (herb), 25 20 “ “ (extract), 5 Cantharftlis, 5 10 10 1.25 Cinchonte, 20 20 20 20 Colchici Seminis, 15 10 20 12.5 Digitalis (Ph. Ger. fresh pulp), 15 83.3 20 12.5 Gelsemii, 15 12.5 Hyoscyami, 15 20 12.5 lo'di, 7 9.1 7.7 2.5 Lobelias, 20 20 20 12.5 Nucis Vomicae (Tr. Strychni), Ext. 2 Gms. 10 20 Ext. 1% grs. Opii, . . 10 10 13 7.5 Physostigmatis, 15 20 Rhei, 10 10 Aq. 20 10 Stramonii Seminis, 15 12.5 “ Foliorum, 20 Veratri (albi), 10 20 Veratri Viridis, '. 40 20 Preparation.—For the preparation of tinctures only the best obtainable quality of a drug should be employed. The use of cheap and second-rate material is a culpable and reprehensible practice. The market affords an abundance of first-class drugs at a reasonable price for the quality. The various methods employed in the preparation of tinctures are:—first, Solution; second, Maceration; third, Digestion; fourth, Percolation. 1st. Solution.— This is applicable in such instances as tinctures of iodine and tolu, where the material is wholly or practically soluble in alcohol. 2d. Maceration.^—This process is preferred by the majority of foreign pharmacopoeias. For this purpose large, strong bottles with a wide mouth are selected, the drug (in coarse powder or particles) and menstruum are introduced, and they are then well corked and set aside for a period of from 7 to 14 days. The tem- perature of the room should be about 20° C.; the bottles should be conveniently placed, so that they may be shaken once or twice daily. At the end of the period of maceration the fluid portion is drained off, the residue then transferred to the strainer, deprived of as much of the fluid as possible by hand pressure, then enclosed securely in the straining-cloth, and subjected to pressure in a tincture press. The tincture is allowed to settle and is then * This is only approximate for the U. S. P., for the drug is expressed in parts by weight, and the finished product in parts by measure. t Concerning the comparative advantages and disadvantages of Maceration and Percolation, see page 189. 260 HANDBOOK OF PHARMACY. filtered. No attempt is made to bring the strained liquid to a definite volume by washing the dregs with menstruum. 3d. Digestion.—This is maceration between the temperatures of 30° and 40° C. It is employed in such cases where the drug is difficult of extraction, or where rapid exhaustion is desired. In this operation the drug and menstruum should be placed in a large glass flask, which is placed on a water- or sand-bath. The flask is closed with a perforated stopper, into which may be fitted an inverted condenser (Fig. 151), or a long (4-5 ft.) plain glass tube (air cooler), for the purpose of condensing the volatilized solvent. The apparatus is allowed to become cold before the contents are drained off. 4th. Percolation.—While the principle of percolation or dis- placement has been known and applied in chemical and indus- trial operations for a very long time, it was first applied, officially, to the preparation of tinctures, fluid extracts, etc., in this country, in the Pharmacopoeia of 1840. It is now also recognized to some extent by the pharmacopoeias of England, France, Germany, Switzerland, etc. Percolation as applied to the preparation of tinctures, although demanding care and close attention, is not fraught with the same difficulties as in the preparation of fluid extracts, since the volume of menstruum is largely in excess of that necessary to insure the exhaustion of the drug. This should not, however, lead to carelessness, for no matter how large the excess of men- struum may be, should the operator have packed the drug care- lessly, and not have devoted proper attention to the operation, exhaustion cannot be expected. The U. S. Pharmacopoeia directs a short period of maceration, previous to beginning percolation. This precaution should always be observed, and the time should rather be lengthened than shortened. The British Pharmacopoeia demands a preliminary maceration of forty-eight hours, which is certainly a point in its favor. The U. S. Pharmacopoeia directs that the drug be percolated until a certain volume (1000 Cc.) is obtained. Hence, the men- struum which is retained by the drug is lost. To avoid this, it has been suggested to adopt the method of the British Pharma- copoeia. According to this, after the whole of the menstruum (equal in volume to the quantity of tincture to be obtained) has been added, and percolation ceases, the marc is to be transferred to a tincture press, the expressed and filtered liquid mixed with the percolate, and the whole then made up to the proper volume by adding more menstruum. Some operators attempt to recover the menstruum retained by the drug by forcing it out with water. This is not advisable, since the vegetable tissues, on coming in contact with water, swell and often choke the percolator. Besides, water takes up other principles than alcohol, and since the diffusion of the one into the other cannot be prevented, this diluted menstruum, generally ALCOHOLIC OR HYDROALCOHOLIC SOLUTIONS. 261 contaminated with inert extractive, flows into the more or less alcoholic percolate, causing thereby cloudiness or precipita- tion. The practice of preparing tinctures by diluting Fluid Ex- tracts* should be condemned, particularly so in the case of potent drugs. Preservation.—Tinctures should be kept in well-stoppered bottles, away from the direct rays of the sun. As a guide to the estimation of the quality and strength of tinctures, the German Pharmacopoeia specifies the limits of specific gravity; the per- centage of dry residue left on evaporation on the water-bath ; the percentage of ash; or the percentage of acid expressed in milli- grammes of KOH, necessary to neutralize 10 Gm. of tincture diluted with 100 Gm. of water. These figures, however, do not give any decisive clue as to the quality of the tincture. When the activity of a drug resides in certain definite proximate prin- ciples, the only accurate method of judging the quality of its preparations is by assay. The U. S. Pharmacopoeia has thus standardized two of its tinctures, viz., those of Opium and Nux Vomica. TINCTURE HERBARUM RECENTIUM. This class of preparations was introduced many years ago by Hahnemann, and is extensively used at present in homoeopathic and eclectic practice. They were first prepared by the addition of the freshly-expressed juice to twice its weight of alcohol. The United States, as well as French Pharmacopoeias, adopted the process of Soubeiran, which consisted in macerating the fresh,cut or bruised drug with alcohol in definite proportions. As a rule, these are very active preparations, for it is justly claimed that the process of drying, in order to prepare drugs for the process of grinding and powdering, injures or alters many sensitive active principles. On the other hand, uniformity in the strength of these preparations cannot be expected, for the freshly-collected drug contains a variable amount of moisture, according to the time of gathering and the length of subsequent exposure. The U. S. gives the following directions: “ These tinc- tures, when not otherwise directed, are to be prepared by the fol- lowing formula: Take of the fresh herb, bruised or crushed, 500 Gm.; alcohol, 1000 Cc.; macerate the herb with the alcohol for fourteen days; then express the liquid and filter.” Among the tinctures made by this process and in frequent use are those of Rhus Toxicodendron, Conium, Digitalis, Hyoscyamus, Pulsatilla, Gelsemium, Aconite, Belladonna, etc. * “ Tinctures from Fluid Extracts,” J. W. England, Druggists' Circular, 1893, p. 245. fThe French Pharmacopoeia directs equal parts of the fresh drug and alcohol of 90 and to mace- rate 10 days. 262 HANDBOOK OF PHARMACY. SUCCI—JUICES. These are a class of preparations official in the British Pharma- copoeia, made by bruising and expressing fresh, succulent drugs. The juice is then mixed with a definite volume of alcohol (1 vol. alcohol to 3 vols. juice), the mixture set aside for seven days, and filtered. These preparations vary in strength for the same reasons which were just given under Tinctures of Fresh Herbs, which latter were introduced into the U. S. Pharmacopoeia in lieu of the “ Succi.” The British Pharmacopoeia recognizes Succus Belladonnae, Conii, Hyoscyami, Scoparii,and Taraxaci. EXPLANATORY (Tinctures). There are 71 tinctures official in the U. S. Pharmacopoeia. Tinctura Ferri Chloride—This preparation should be al- lowed to stand at least 3 months before being dispensed, as directed by the U. S. Pharmacopoeia. By this time it will have developed an agreeable ethereal odor due to the formation of a small amount of ethyl chloride (C2H5C1). Tincture of iron is incompatible with alkalies, alkaline earths or carbonates (production of Fe2(OH)6 or Fe2O3); likewise with preparations containing tannic acid (inky mixtures); also with mercurous salts (forming mercuric com- pounds) ; with mucilage of acacia it often produces a jelly. Assay.—See Liquor Ferri Chloridi. Tinctura Iodi.—Freshly prepared tincture of iodine forms a precipitate upon the addition of water; after long standing, how- ever, it is often found to yield a clear solution with water. This is due to the formation of hydriodicacid produced by the reaction between the iodine and alcohol. The British Pharmacopoeia adds potassium iodide to its tinc- ture for the purpose of rendering it miscible with water. This is not objectionable when it is intended for internal use ; but, as it is exceedingly rare to administer iodine in this form, the advan- tage of the addition of KI is scarcely apparent. The tincture should be recently prepared. It is incompatible with salts of the metals (forms insoluble metallic iodides); also alkalies, alkaline carbonates, ammonium chloride (iodide of nitro- gen, explosive), starch (iodide of starch), sodium hyposulphite (decolorized), and most alkaloids. The so-called Decolorized Tincture of Iodine is made by digest- ing 10 parts each of iodine, sodium hyposulphite and water, until solution is effected, then adding 16 parts of spirit of ammonia, shaking, adding 75 parts of alcohol, and filtering after three days. The title of the preparation is very misleading, for it does not contain a trace of free iodine, it having all combined with the ALCOHOLIC OR HYDROALCOHOLIC SOLUTIONS. 263 alkalies, forming sodium and ammonium iodide, sodium tetra- thionate, with some ethyl iodide (C2H5I) and triethylamine hydrio- dide (N(C2H5)3HI). Assay.—The U. S. Pharmacopoeia directs that 6.3 Cc. of the tincture be added to a solution of 2 Gm. of potassium iodide in 25 Cc. of water: the alkali iodide is added for the purpose of pre- venting the precipitation of the iodine in the aqueous liquid. Gelatinized starch is then added, which forms a blue colored solution with the free iodide. To the mixture is now slowly added decinormal solution of sodium hyposulphite,* until the blue color disappears. One molecule of iodine (2 X 126.6 parts) unites with the two molecules of sodium hyposulphite (2 X 247.6 parts) to form the soluble, colorless, sodium iodide,thus:— 2(Na2S2O3.5H2O) + 21 = 2NaI + Na.2S4O6 4- IOH.,0 Sodium Hyposulphite. Iodine. Sodium Iodide. Sodium Water. 2 X'247.6 2 X 126.6 Tetrathionate. One molecule Hyposulphite, 247.6 p. One atom Iodine, 126.6 p. 24.76 Gm. Hyposulphite (1000 Cc.) — 12.66 Gm. Iodine. 0.02476 “ (1 Cc.) — 0.01266 “ 35 Cc. Hyposulphite = 35 X 0 01266 — 0.443-f-Gm. Iodine. Since 6.3 Cc. of tincture were taken, then it must contain of iodine [(0.443 -s- 6.3) X 100] = 7 Gm. in 100 Cc. Tinctura Opii.—The directions of the Pharmacopoeia should be strictly adhered to, in the employment of a powdered opium, the morphine strength of which has been previously ascertained by assay. Crude opium (except on a manufacturing scale, and with rigid assay of the product) should never be used, because, from its variable percentage of moisture, it would yield a prepara- tion of a very unreliable strength. The object of the Pharmaco- poeia is to secure uniformity of strength ; any deviation from this, in so important a preparation, is indeed a serious matter. Assay.—The present official method of assay, for this tincture, is very simple, and no apothecary should excuse himself for applying it. The process is as follows :— “ If 100 Cc. of Tincture of Opium be assayed by the process im- mediately following, it should yield from 1.3 to 1.5 Gm. of crys- tallized morphine. Assay of Tincture of Opium. Tincture of Opium, one hundred cubic centimeters 100 Cc. Ammonia Water, three and five-tenths cubic centimeters, . . . 3.5 Cc. Alcohol, Ether, Water, each, a sufficient quantity. Evaporate the tincture to about 20 Cc., add about 40 Cc. of water, mix thoroughly, and set the liquid aside for an hour, oc- casionally stirring, and disintegrating the resinous flakes adhering * See Decinormal Solution of Sodium Hyposulphite. 264 HANDBOOK OF PHARMACY. to the capsule. Then filter, and wash the filter and residue with water, until all soluble matters are extracted, collecting the wash- ings separately.” The tincture should be slowly evaporated in a dish or beaker glass of about 150 Cc. capacity, on a water-bath, and not boiled. A higher temperature will result in a partial destruction of the mor- phine. Before an attempt is made to precipitate the morphine, such impurities as resin and caoutchouc, with as much coloring and extractive matter as possible, should be removed; otherwise these would be carried down with the morphine precipitate, and give false results. Hence the tincture is evaporated to a small bulk (20 Cc.), when the loss of alcohol causes the partial separation of the resin and caoutchouc. This is made more complete by the addition of 40 Cc. of cold water, in which these are comparatively insoluble. After standing the specified time, it should be carefully filtered through a small (3 in.) plain filter, the guiding-rod being used to direct the flow of fluid without loss. The residue in the capsule or beaker is rinsed on to the filter and the washing con- tinued the filtrate comes through devoid of all traces of bitter taste ; or better, until a few drops of the filtrate collected on a watch-glass, and acidulated with a drop of dilute hydro- chloric acid, ceases to give a precipitate with Mayer’s Reagent* ; or with Lugol’s Solution. “ Evaporate in a fared capsule, first, the washings to a small volume, then add the first filtrate, and evaporate the whole to a weight of 14 Gm. Rotate the concentrated solution about in the capsule until the rings of extract are redissolved, pour the liquid into a fared Erlenmeyer flask, having a capacity of about 100 Cc., and rinse the capsule with a few drops of water at a time, until the entire solution weighs 20 Gm. Then add 10 Gm. (or 12.2 Cc.) of alcohol, shake well, add 25 Cc. of ether, and shake again. Now add the ammonia water from a graduated pipette or burette, stopper the flask with a sound cork, shake it thoroughly during ten minutes, and then set it aside, in a moderately cool place, for at least six hours, or over night.” The weaker solution is first evaporated to a small volume, and the first filtrate, which contains nearly all of the morphine, is then added. In this way the injurious effect of prolonged heat is avoided. After having transferred the entire solution into a fared assay flask, by washing with a little water until the whole weighs 20 Gm., we are ready for the precipitation of the mor- phine. This alkaloid is in solution, combined chiefly with meconic acid, and inasmuch as morphine is practically insoluble in water (1 in 4350), it may be readily precipitated from its solu- tion by the addition of an alkali, preferably ammonia (since soda or potassa readily dissolves this alkaloid). The ammonia ♦Prepared by dissolving 13.546 Gm. of mercuric chloride and 49.8 Gm. of potassium iodide in suf- ficient distilled water to make 1000 Cc. ALCOHOLIC OR HYDROALCOHOLIC SOLUTIONS. 265 water must be of ten per cent, strength, and not more than 3.5 Cc. should be added, for an excess of this, over and above that necessary to combine with the meconic acid present, will cause some of the morphine to be retained in solution. Alcohol and ether are added before the ammonia water; the volume of the former is not sufficient to exert any solvent effect on the mor- phine, while its presence serves to retain the coloring matter in solution, preventing its being carried down with the mor- phine. The ether serves to promote the rapid and thorough separation of the morphine as well as to take up coloring matter and narcotine. “ Remove the stopper carefully, and, should any crystals ad- here to it, brush them into the flask. Place in a small funnel two rapidly-acting filters, of a diameter of 7 Cm., plainly folded, one within the other (the triple fold of the inner filter being laid against the single side of the outer filter), wet them well with ether, and decant the ethereal solution as completely as possible upon the inner filter. Add 10 Cc. of ether to the contents of the flask, rotate it, and again decant the ethereal layer upon the inner filter. Repeat this operation with another portion of 10 Cc. of ether. Then pour into the filter the liquid in the flask, in portions, in such a way as to transfer the greater portion of the crystals to the filter, and, when this has passed through, transfer the remaining crystals to the filter by washing the flask with several portions of water, using not more than about 10 Cc. in all. Allow the double filter to drain, then apply water to the crystals, drop by drop, until they are practically free from mother-water, and afterwards wash them, drop by drop, from a pipette, with alcohol previously saturated with powdered morphine. When this has passed through, displace the remaining alcohol by ether, using about 10 Cc., or more if necessary. Allow the filter to dry in a moderately warm place, at a temperature not exceeding 60° C. (140° F.) until its weight remains constant, then carefully transfer the crystals to a fared watch-glass and weigh them. “The weight found represents the amount of crystallized mor- phine obtained from 100 Cc. of the Tincture.” The filter is first wetted with ether, otherwise, should some of the aqueous filtrate be poured, through carelessness, on the filter, this would prevent the ether from filtering through. After the ether washings have all been decanted upon the filter, the latter is allowed to stand a few minutes until the ether has evaporated, then the aqueous fluid containing the crystals of morphine in suspension is poured, in portions, upon the filter. Crystals always remain adhering to the sides of the flask. These can be easily removed by rinsing out first with a portion of the filtrate, or, if necessary, they may be detached by means of a rubber-tipped glass-rod. The flask is now rinsed out with 10 Cc. of water, used in portions. The U. S. P. directs, that, as soon as the filter has drained, water should be dropped (not poured) over the crystals 266 HANDBOOK OF PHARMACY. until they are free from mother liquor; for this purpose not more than about 8 to 10 Cc. of water should be used.* If the crystals are of a light gray or buff color, they will be sufficiently pure, but should they be of a brown, or very dark gray color, then they should be further washed with alcohol saturated with morphine, followed with ether as directed. It is important that the ether follow the morphinated alcohol as soon as the latter has dis- appeared from the surface of the precipitate on the filter; other- wise, the morphine introduced by the morphinated alcohol might remain in the precipitate, upon evaporation of the alcohol, and the ether would not be able to displace it. The drying is done at a moderate heat, since it is only necessary to remove the ether, when crystallized morphine will remain behind. Tincture of Opium is incompatible with solutions containing free ammonia (aromatic spirit of ammonia), solutions containing tannic acid, and other substances affecting alkaloids. One grain of powdered opium is represented, in U. S. measures, by 10.5 minims (U. S.), 14 minims (B. P.) 11.3 minims (Ph. Ger.), and 9 minims (Fr. Ph.) of the tincture. The powdered or dry opium employed by these several Phar- macopoeias should contain of morphine, 13 to 15 per cent, of crys- tallized (U. S.), about 10 per cent, of anhydrous (B. P.), at least 10 to 12 per cent, of anhydrous (Fr. Ph.), and 10 per cent, of anhy- drous (Ph. Ger.). One hundred parts of crystallized morphine correspond to 94.06 parts of anhydrous; and. 100 parts of anhydrous correspond to 106.31 parts of crystallized morphine. * Water saturated with morphine (morphinated water) may be employed in larger quantities, as it does not exert any solvent action on the morphine. ALCOHOLIC OR HYDROALCOHOLIC SOLUTIONS. 267 Official Title. Bek Cent.* Active Constituents. Constituents. Menstruum. Dose. Ti nctura— Opii Camphorata, Each 0.4 P. Opium, Benzoic Aeid, Camphor, each 4 Gm., Oil Anise 4 Cc. Dil. Alcohol, Glycerin. 0.5-15 Cc. Nucis Vomicae, 2 Ext. Nux Vomica 20 Gm, Ale. 3 p., Water 1 p. 0.3-1 Cc. Cantharidis 5 P. Cantharides 50 Gm. Alcohol. 0.3-1 Cc. Capsici, 5 P. Capsicum 50 Gm. Ale. 95 p., Water 5 p. 0.5-3 Cc. Mosch i, 5 Musk 50 Gm. Dil. Alcohol. 1-2 Cc. Strophanthi, 5 P. Strophanthus 50 Gm. Ale. 65 p., Water 35 p. 0.2-0.6 Cc. lodi 7 Iodine 70 Gm. Alcohol. External. Aloes, 10 Aloes 100 Gm., Liquorice Root 200 Gm. Dil. Alcohol. 0.3-15 Cc. Aloes et Myrrh®, 10 Aloes, 100 Gm., Myrrh 100 Gm., Liquorice Root 100 Gm. Ale. 75 p., Water 25 p. 2-7 Cc. Arnie® Radicis, 10 Arnica Root 100 Gm. Ale. 65 p., Water 35 p. External. Bryoni®, 10 Bryonia 100 Gm. Alcohol. External. Calumb®, 10 Calumba 100 Gm. Ale. 60 p., Waler 40 p. 3-14 Cc. Cardamom!, 10 Cardamon 100 Gm. Dil. Alcohol. 3-8 Cc. Catechu Composita, 10 Catechu 100 Gm., Cassia 50 Gm. Dil. Alcohol. 2-10 Cc. Chirat®, 10 Chirata 100 Gm. Ale. 65 p., Water 35 p. 2-8 Cc. Cinchon® Composita, 10 Red Cinchona 100 Gm., Serpentaria 20 Gm., Bitter Orange Peel 80 Gm. Cevlon Cinnamon 100 Gm. Ale. 85 p.,Water 7.5 p.,Glycerin. 3-8 Cc. Cinnamom i 10 Ale. 75 p.,Water 20 p. Glycerin. 3-15 Cc. Croci 10 Saffron 100 Gm. Dil. Alcohol. Color. Gentian® Composita, 10 Gentian 100 Gm., Bitter Orange Peel 40 Gm., Cardamom 10 Gm. Ale. 60 p., Water 40 p. 3-8 Cc. Kino, . 10 Kino 100 Gm. Ale. 65 p.,Water 20 p., Glycerin. 2 8 Cc. Matico, 10 Matico 100 Gm. Dil. Alcohol. 3-8 Cc. Opii, 10 P. Opium 100 Gm. (Calc. Phosp.) Dil. Alcohol. 0.3-0 9 Cc. Opii Deodorati, 10 P. Opium 100 Gm. (Ether—Calc. Phos.) Ale. 20 p., Water 80 p. 0.3 0.9 Cc. Quassi®, 10 Quassia 100 Gm. Ale. 35 p., Water 65. 2-4 Cc. Rhei, 10 Rhubarb 100 Gin., Cardamom 20 Gm. Ale 60 p.,Water 30 p., Glycerin. 3-15 Cc. Rhei Dulcis, 10 Rhubarb 100 Gm., Liquorice 40 Gm., Anise 40 Gm., Cardamom Ale. 50 p.,Water 40 p., Glycerin. 3-8 Cc. Serpen tari®, 10 10 Gm. Serpentaria 100 Gm. Ale. 65 p., Water 35 p. 2-8 Cc. Suinbul, 10 Sumbtll 100 Gm. Ale. 65 p., Water 35 p. 1-4 Cc. Tolutana, 10 Balsam Tolu 100 Gm. Alcohol. Flavor. Vanill®, 10 Vanilla 100 Gm., Sugar 200 Gm. Ale. 65 p , Water 35 p. Flavor. Ferri Chloridi, 13.6 Sol. Fe2Cl6 250 Cc. Alcohol. 0.3-1 Cc. Belladonn® Foliorum, .... 15 Belladonna Lvs. 150 Gm. Dil. Alcohol. 0.3-0.9 Cc. Cannabis Indic®, 15 Cannabis Ind. 150 Gm. Alcohol. 0.3-1 Cc. Colchici Seminis, 15 Colchicum Seed 150 Gm. Ale. 60 p., Water 40 p. 0.6-3 Cc. Digitalis, 15 Digitalis 150 Gm. Dil. Alcohol. 0.3-1.5 Cc. Gelsemii, 15 Gelsemium 150 Gm. Ale. 65 p., Water 35 p. 0 1-0 9 Cc. Hyoscyami, 15 Hyoscyamus 150 Gm. Dil. Alcohol. 0.6-3 Cc. SYLLABUS OF TINCTURES. * See Footnote on page 225. 268 HANDBOOK OF PHARMACY. Official Title. Per Cent.* Active Constituents. Constituents. Menstruum. Dose. Tinctura— Physostigmatis, 15 Physostigma 150 Gm. Alcohol. 0.3-0.6 Cc. Sanguinari®, 15 Sanguinaria 150 Gm., Acetic Acid 20 Cc. Ale. 60 p., Water 40 p. 1-2 Cc. Scill®, 15 Squill 150 Gm. Ale. 75 p., Water 25 p. 0 3-1 Cc. Stramonii Seminis, 15 Stramonium Seed 150 Gm. Dil. Alcohol. 0.3-0.6 Cc. Arnie® Florum, 20 Arnica Flos. 200 Gm. Dil. Alcohol. External. Asafcetid®, 20 Asafcetida 200 Gm. Alcohol. 0.5-2 Cc. Aurantii Amari, 20 Bitter Orange Peel 200 Gm. Ale. 60 p., Water 40 p. Flavor. “ Dulcis, 20 Fresh Sweet Orange Peel 200 Gm. Alcohol. Flavor. Benzoini, 20 Benzoin 200 Gm. Alcohol. Lotion. Calendul®, 20 Calendula 200 Gm. Alcohol. External. Cimicifug®, 20 Cimicifuga 200 Gm. Alcohol. 3-7 Cc. Cinchona;, 20 Cinchona 200 Gm. Ale. 67.5 p., Water 25 p., Gly- 3-7 Cc. Cubeb®, 20 Cubeb 200 Gm. cerin. Alcohol. 2-7 Cc. Gall®, 20 Nutgall 200 Gm. Alcohol, Glycerin. Lotion. Guaiaci, 20 Guaiac 200 Gm. Alcohol. 1-4 Cc. “ Ammoniata, 20 Guaiac 200 Gm. Sp. Ammonia Arom. q. s. 1-4 Cc. Humuli, 20 Hops 200 Gm. Dil. Alcohol. 3-12 Cc. Hydrastis, Ipecacuanhas et Opii, .... 20 Hydrastis 200 Gm. Dil. Alcohol. 1-3 Cc. 20 Fl. Ext. Ipecac 100 Cc., Deod. Tr. Opium 1000 Cc. Dil. Alcohol. 0.3-1 Cc. Krameri®, 20 Rhatany 200 Gm. Dil. Alcohol. 2-8 Cc. Lobeli®, 20 Lobelia 200 Gm. Dil. Alcohol. 0.5-1 Cc. Myrrh®, 30 Myrrh 200 Gm. Alcohol. 1-1.5 Cc. Pyrethri, Quillaj®, 20 Pyrethrum 200 Gm. Alcohol. External. 20 Quillaja 200 Gm. Ale. 35 p., Water q. s. External. Khei Aromatica, 20 Rhubarb 200 Gm., Cinnamon, Cloves each 40 Gm., Nutmeg Dil. Alcohol, Glycerin. 1.5-10 Cc. Valerian®, 20 20 Gm. Valerian 200 Gm. Ale. 75 p., Water 25 p. 3-8 Cc. “ Ammoniata, . . . 20 Valerian 200 Gm. Sp. Ammon. Ar. q. s. 3-8 Cc. Zingiberis, 20 Ginger 200 Gm. Alcohol. 1-3 Cc. Benzoini Composita 20 Benzoin 120 Gm., Purif. Aloes 20 Gm., Storax 80 Gm., Balsam Alcohol. Lotion. Aconiti, Veratri Viridis Cardamomi Composita, .... 35 Tolu 40 Gm. Aconite Root 350 Gm. Ale. 70 p., Water 30 p. 0.06-0.18 Cc. 40 Veratrum Viride 400 Gm. Alcohol. 0.06-0.3 Cc. 40 Cardamom, Cinnamon each 20 Gm., Caraway 10 Gm., Cochineal Dil. Alcohol, Glycerin. Aromatic. Lactucarii, Lavandnl® Composita, .... 50 5 Gm. Lactucarium 500 Gm. (Benzine). Dil. Alcohol, Glvcerin. 0.5-3 Cc. Oil Lavender Fl. 8 Cc., Oil Rosemary 2 Cc., Cinnamon 20 Gm., Cloves 5 Gm., Nutmeg 10 Gm., Red Saunders 10 Gm. Ale. 70 p.,Water 25 p., Dil. Ale. 2-7 Cc. SYLLABUS OF TINCTURES.—Continued. * See Footnote on page 225. ALCOHOLIC OR HYDROALCOHOLIC SOLUTIONS. 269 EXTRACTA FLUID A—{Fluid Extracts). Fluid Extracts are concentrated fluid preparations of nearly uniform strength, representing the activity of the drug, volume for weight. When properly prepared they afford a permanent, active, concentrated liquid, representing the drug in definite pro- portions. As required by the U. S. Pharmacopoeia, 1 cubic centimeter of the preparation represents the medicinal activity of 1 gramme of the drug. Previous to 1880, the strength was represented by 1 troy-ounce of the drug to 1 fluidounce of the fluid extract. On comparison it will be seen that our present fluid extracts are about 5 per cent, weaker than those of the Pharmacopoeia of 1870, thus:— 100 troy ounces of drug (3110.4 Gm.) yield 100 fluidounces (2956.4 Cc.) of fluid extract.—U. S. P., 1870. 100 grammes of drug yield 100 Cc. of fluid extract.—U. S. P., 1880 and 1890. It will be seen that according to the U. S. Pharmacopoeia of 1870, 3110.4 Gm. (100 troy ounces) of drug yielded 2956.4 Cc. (100 fluidounces) of fluid extract, instead of 3110.4 Cc., as the present Pharmacopoeia requires; hence there is a difference of 154 Cc. in the proportion of volume to drug, which render our present fluid extracts about 5 per cent, weaker as compared with those based on troy weight and fluidounces, and which is certainly a point in their favor. The British Pharmacopoeia directs that its liquid extracts (with the exception of those of cinchona, glycyrrhiza, opium and pareira), be made of the strength of 1 avoirdupois ounce to 1 fluidounce imperial. They are practically identical with our own. The German Pharmacopoeia has introduced four fluid extracts, the method of preparation and strength of which is the same as those directed by the U. S. Pharmacopoeia. The U. S. Pharmacopoeia directs that all fluid extracts be pre- pared by the process of percolation, with authority to employ the method of repercolation, if this be found desirable. Menstruum.—The U. S. Pharmacopoeia directs the employ- ment of certain menstrua, which are selected with the view of extracting all the activity of the drug, and at the same time of affording a stable preparation. The different menstrua employed consist of alcohol, various mixtures of alcohol and water, and either of these in conjunction with glycerin. In two instances (triticum and castanea) boding water is employed to exhaust the drug, with subsequent addition of alcohol, or alcohol and glycerin, to insure the stability of the preparation. Acetic acid of a strength varying from about 60 per cent, to 20 per cent, or less, has been used by Dr. Squibb as a menstruum for drugs containing ethereal oils, aromatic resins, alkaloids, etc. 270 HANDBOOK OF PHARMACY. It is claimed to yield a very effective and palatable preparation; in experiments with nux vomica and belladonna this menstruum has proven its superiority to alcohol. Fluid Extracts are prepared by “ simple ” or “ fractional perco- lation.” By “simple” percolation we understand that the entire drug is percolated at one operation; under this head we have the official process, that of vacuum percolation, and percolation combined with maceration and pressure. In “ fractional percolation ” the drug is divided into two or more portions, the reserved (first) percolate from each portion is set aside, while the subsequent (weaker) percolates are employed for macerating and percolating each subsequent portion. This process is known as that of repercolation. PERCOLATION (U. S. Pharmacopoeia Process). The U. S. Pharmacopoeia of 1890 directs that all fluid extracts be prepared by the process of percolation. 1000 Gm. of the drug of the proper degree of fineness are moistened, packed, macerated and percolated (see Percolation, page 191), until exhausted. From 700 to 900 Cc. of the first portion of the percolate are pre- served, and the weaker portion is evaporated at a low tempera- ture (50° C.), to the consistence of a soft extract, which is then dissolved in the reserved portion, to which enough menstruum is finally added to make the finished preparation measure 1000 Cc. The objections to the U. S. Pharmacopoeial process of 1870 were that the weak percolate, when evaporated to an ascertained volume, sustained a loss of most or all of its alcohol, leaving a more or less aqueous residue, which, when added to the strongly alcoholic reserved portion, caused a precipitation of more or less resinous or other active matter. The operator should be careful not to employ too high a degree of temperature in evaporating the weak percolates, otherwise injury or destruction of organic principles is liable to occur. The official process is often objected to, because of the employment of heat in part of the operation ; however it must be remembered that from 75 to 90 per cent, of the activity of the drug is represented by the reserved portion, and that but a very small percentage is subjected to the action of heat, as a rule, which, if properly regulated, will not materially injure the prep- aration (exceptions are Allium, Prunus Virginiana, etc.). Repercolation (“ fractional ” * percolation), as described by Dr. Squibb, its originator (1866), “ consists in the successive applica- tion of the same percolating menstruum to fresh portions of the substance to be percolated.” Its object is the preparation of a fluid extract without the use of heat. The operation may be briefly described thus: 32 parts of the drug in powder are divid- ed into four equal portions of eight parts each, one of which is *See Prof. Diehl’s paper, “ Proceed. Am. Phar. Assoc.,” 1878, p. 681. ALCOHOLIC OR HYDROALCOHOLIC SOLUTIONS. 271 moistened, packed, macerated, then percolated until exhausted, this weaker percolate being received in several distinct portions. The first six parts of the percolate are reserved, and the remaining portions are used successively for moistening and percolating the second eight parts of the powder. Of the second percolate 8 parts are reserved, and the weaker percolate which is again received in several portions, used for the following third portion, as directed above. The third and fourth fractions of 8 parts each are then treated in the same manner, 8 parts of percolate being reserved from each fraction. Finally, the four reserved portions of 6 + 8 + 84-8 fluidounces are mixed to obtain 30 parts of fluid extract.* The weak percolate remaining over from the last portion of the drug is set aside for a subsequent operation on a fresh lot of the same drug. The National Formulary gives the following directions:— Fractional Percolation.—Take of the drug, in powder of the prescribed fineness, sixteen (16) troy ounces, and divide this into three portions, of eight (8), five (5) and three (3) troy ounces, respectively. Moisten the first portion (8 troy ounces) with the menstruum and percolate in the usual manner. Set aside the first three (3) fluidounces of the percolate, and continue until twenty-four (24) fluidounces more of percolate have passed, which should be re- ceived in several portions, so that the more concentrated will be separate from the last, weak percolate. Then moisten the second portion of the drug (5 troy ounces) with the most concentrated of the percolates received during the * As a practical example of this operation a typical description of the preparation of a fluid extract, as given by Dr. Squibb, is cited :— EXTRACTUM CINCHONAS FLUIDUM—(Fluid Extract of Cinchona). R Yellow Cinchona, in powder No. 50, 32 parts. Stronger Alcohol, s. g. 0.819, 2 parts, ) For sufficient Glycerin, s. g. 1.250, 1 part, > quantity of Water, 2 parts J menstruum. Weigh the stronger alcohol, glycerin, and water in succession, in any convenient quantity at a time, into a fared bottle, and mix them thoroughly for a menstruum. Moisten 8 parts of the cinchona with 8 parts of the menstruum, by thoroughly mixing them, and allow the mixture to stand 8 hours in a closely covered vessel. Then pass the moist powder through a No. 8 sieve, and pack it firmly in a percolator. Pour menstruum on top until the mass is filled with liquid and a stratum remains "on top unabsorbed ; cover the percolator closely and macerate for 48 hours. Then arrange the percolator for an automatic supply of menstruum, and start the percolation at such a rate as to give 1 part of percolate in about 4 hours. Reserve the first 6 parts of percolate and continue the percolation until the cinchona is exhausted, separating the percolate received after the reserved portion into fractions of about 8 parts each. Moisten a second port ion of 8 parts of the cinchona with 8 parts of the weak percolate—the portion that was obtained next after the reserved percolate—and allow the moist powder to stand for 8 hours in a vessel closely covered. Then pack it moderately in a percolator, and supply the percolator auto- matically with "the remaining fractions of the weak percolate in the order in which they were received, and finally, with fresh menstruum until the cinchona is exhausted. Percolate in the same manner and at the same rate as with the first portion of cinchona, and reserving 8 parts of the first percolate, separate the weaker percolate into fractions of about 8 parts each. Percolate the third and fourth portions of 8 parts each of the cinchona in the same way as the second portion. Finally mix the four reserved percolates together to make 30 parts of finished fluid extract; and having corked, labeled, and numbered the bottles containing the fractions of weak percolate, set them away until the process for cinchona is to be resumed. When this fluid extract is to be again made, repeat the process as with the second portion, and reserve 8 parts of the first percolate as finished fluid extract from each 8 parts of cinchona from that time forward so long as the fractions of weak percolate are carried forward with which to commence each operation. Upon this small scale the percolate from the first portion should weigh from 3 to 4 times the weight of the powder; and for the repercolations from 5 to 7 times the weight of the powder. 272 HANDBOOK OF PHARMACY. preceding operation after the first 3 fluidounces had passed, and percolate again in the usual manner, using the several reserved percolates, successively, as menstrua. Set aside the first five (5) fluidounces, and continue the percolation until ten (10) fluidounces more have passed, which should also be received in several portions. Finally moisten the third portion of the drug (3 troy ounces) with the most concentrated of the last reserved percolates, and proceed as directed for the second portion. Collect the first eight (8) flaid- ounces separately, and mix them with the two portions previously set aside so as to make sixteen (16) fluidounces of Fluid Extract. This process is adapted for the preparation of solid as well as fluid extracts, but not for other pharmaceutical preparations made by percolation. This process yields a perfect fluid extract without the use of heat, thereby adapting it to the most sensitive drug. It recom- mends itself to the apothecary, in that it avoids the loss and expense caused by subsequent concentration; it nearly always insures a perfect preparation, because, though it be indifferently applied, the inaccuracies of one operation are likely to be made up and compensated in others, so that, when the results of the different percolations are mixed together, the general result will be practically uniform. The only disadvantage the process offers, is that it necessitates the keeping of a series of weak percolates which must be stored away, to be used for the same drug in a subsequent operation. These methods are employed principally by manufacturers on the large scale. The first method consists of a combination of percolation with expression. One hundred parts of the drug are moistened, packed, and allowed to macerate several days in a percolator; percolation is then commenced and continued, until 120 parts of menstruum have been added, then -when the perco- lation ceases, the upper stratum, constituting about one-fifth of the drug, is removed and subjected to powerful pressure; the fluid obtained is poured over the balance of the moist drug in the percolator, and when this again ceases to percolate, a second like portion is removed and treated as before; this procedure is continued until the entire amount of drug has been expressed. The reserved percolates are mixed with the fluid obtained from the last expression, making a total of 95 parts of fluid extract. The second method is simply that of maceration and expression, in which the drug is allowed to macerate from 10 to 12 days with about its own weight of menstruum. The maceration is conducted in a tight cylindrical copper vessel, which is inverted at intervals to facilitate the action of the solvent. At the end of the specified time, the drug is removed and subjected to powerful pressure; the marc is returned to the macerator and sufficient PERCOLATION AND MACERATION WITH EXPRESSION. ALCOHOLIC OR HYDROALCOHOLIC SOLUTIONS. 273 menstruum is added to make up the desired yield. The products of the two expressions, when mixed, constitute the fluid extract. Maceration and Percolation in Vacuo.—As already ex- plained (page 206), the principle underlying this process is this: that, by exhausting the air from the drug, the menstruum is rapidly brought into intimate contact with the cells of the drug, whereby the maceration and exhaustion is expedited. This form of apparatus has been adopted by some of our manufacturers for the preparation of Fluid Extracts. The advantages claimed are that it can be very economically operated, requiring only 16 fluid- ounces of menstruum for the exhaustion of each pound of drug, besides avoiding much loss of alcohol; and also economizing time. No class of pharmaceutical preparations has met with so much favor as the fluid extracts. They certainly deserve their popu- larity, for (if properly prepared) they fully represent all of the active properties of the respective drugs, in a compact form. Aside from this, they present another advantage over the tinc- tures, namely, this, that owing to their concentrated form, they contain a proportionally much smaller amount of alcohol, the presence of which is a serious objection in such preparations as tincture of conium or of digitalis, for the medicinal action of these drugs is considerably counteracted by the antidotal effects of the excess of the alcohol present. Preservation.—Fluid Extracts should be kept from the direct rays of the sunlight, and in a room where there is but little varia- tion of temperature. These precautions should be observed so as to avoid changes that may arise from possible precipitation, which, however, cannot be altogether avoided. The various causes which give rise to precipitates in fluid extracts are, according to the researches of Lloyd :*— 1st. Oxidation.—Many vegetable principles are prone to unite with oxygen, forming thereby new and insoluble compounds, which, on being precipitated, carry more or less of the active constituents with them. Again, an interaction between the plant principles may take place, either gradually or suddenly, with the formation of new or insoluble bodies. Fluid extracts of astringent drugs, such as geranium, stillingia, cinchona, etc., which contain large amounts of tannates, especially drugs containing red tannates, form, in time, precipitates which are insoluble in all menstrua. 2d. Change of Solvent Power by Evaporation.—Medicinal sub- stances are very frequently deposited through a loss of the solvent power of the menstruum, in consequence of the evaporation of alcohol during percolation, or particularly so upon mixing the reserved alcoholic with the evaporated aqueous percolate. * “ Precipitates in Fluid Extracts,” Proceed. Am. Phar. Assoc., 1882, p. 509; 1883, p. 336; 1884, p. 410 ; 1885, p. 411. 274 HANDBOOK OF PHARMACY. 3d. Change of Temperature.—Through a lowering of the tem- perature, precipitation results from the inability of the liquid to hold in solution matter which was perfectly soluble in it at a higher temperature. For this reason many manufacturers prefer to prepare their fluid extracts during the winter. “ The fact that the drugs employed are merely air-dry and contain varying amounts of moisture, gives rise to the most important cause of precipitation, namely the change of the alcoholic strength of the menstruum. Some plant powders are very hygroscopic and absorb from 5 to 15 pounds of water per 100, absorbing moisture even in the driest weather. Hence when such drugs are percolated the first part of the percolate contains the water, which is thereby converted into a dilute alcohol, and hence differs from later percolates in alcoholic strength.” This is illustrated by Lloyd in Fluid Extract of Cannabis, which, upon percolation with alcohol, yields a first percolate of reddish-brown color, while the later ones are of deep green color. “ The first portions of such percolates contain gum, extract- ives, and bodies which are more soluble in water than alcohol, while the last portions contain the resins, oils, and such bodies which are more soluble in an alcoholic menstruum; hence, when the several percolates are mixed, a gradual separation of the several dissolved matters takes place.” Still another cause is given by Lloyd, as follows: “ The solvent power of the menstruum varies at different stages of the operation of percolation, aside from that due to the presence of more or less water. . . . Plants contain more or less of gums, gummy extractives, fixed and volatile oils, resins, oleo- resins, resinoids, glucosides, tannates, glucose, sugar, chlorophyll, alkaloids, inorganic salts, etc. As the menstruum enters the powder it extracts the matter soluble in that fluid, and this at once forms a new menstruum, which has power to dissolve sub- stances which are only partly soluble or insoluble in the original menstruum. Thus, during percolation, a constantly changing menstruum is passing through the powder, although the original menstruum be the same. The percolate is accordingly variable in composition and solvent powers; it may be considered as a collection of percolates and menstrua of different solvent power and varying composition, and hence one fraction of it may react with another, giving rise to precipitation.” The quality, that is, strength of a fluid extract or of any liquid pharmaceutical preparation should never be judged by its color. The amount of solid residue left upon evaporation, or the specific gravity, gives also no reliable criterion ; the only sure method of ascertaining the medicinal value of such a preparation is to test its activity physiologically, or where it is possible, to make an assay of its active constituents. CHAPTER XXIX. SYRUPI—(Syrups—Strops—Sirupi). Syrups are dense saccharine solutions, generally medicated or flavored. A dense solution of sugar in water is called simple syrup. When this is impregnated with one or more medicinal sub- stances, it is called a medicated syrup. Simple syrup is employed as a vehicle for the administration of medicinal substances. In order to render it more pleasant and better able to disguise the taste, syrup flavored with aro- matic substances is also employed. The presence of sugar exerts a strong preservative influence upon aqueous extracts of plants, which, without this, would ferment quickly. The preservative action of concentrated solu- tions of sugar is such, that they do not afford nourishment for micro-organisms, since the sugar withdraws water from these, which is essential to their cell-growth. For this reason, the amount of sugar in the syrup must be adjusted with a view to its preservation. Should the syrup be too concentrated, upon standing, a portion of the sugar is liable to crystallize out, caus- ing thereby a diminution in saccharine strength, giving rise to the same difficulty of fermentation that would take place were the syrup made too weak. For the preparation of simple syrup, the U. S. Pharmacopoeia employs about 18.6 parts sugar to 10 parts of water,* the British Pharmacopoeia 20 parts to 10, the German Pharmacopoeia 15 parts to 10, the French Pharmacopoeia 18 parts to 10.f If the solution contains alcohol or much extractive, then a correspondingly smaller amount of sugar must be taken. Only the best refined white sugar should be employed, and this should conform to the U. S. Pharmacopoeia requirements of Preparation.—The method of preparation depends largely upon the nature of the substances employed. * Bulk of syrup, resulting from the solution of sugar in water: Sugar. Waler. Bulk. Sp. Gr. 32 ozs. Av. 24 fld. ozs. 45 fld. ozs. 1.273 32 “ 20 41 1.298 32 “ 16 “ 37 1.330 28 “ 14 “ 30 “ 1.317 28 “ 16 “ “ 1.311 24 16 32 “ 1.290 20 “ 16 29 “ 1.264 16 “ 16 26% “ 1.231 f Differences of climate partly warrant this difference of concentration. I The so-called rock-candy syrup should not be employed in preparing the official syrups. 275 276 HANDBOOK OF PHARMACY. 1st. The sugar is dissolved in the medicated liquid by a moderate degree of heat (for instance, a water-bath). 2d. The sugar is dissolved in the fluid by a moderate degree of heat, and the solution then raised to the boiling point. 3d. The sugar is dissolved by agitation or by percolation with the wld, medicated solution. 4th. The sugar is added in the form of ready-prepared syrup to the concentrated medicated liquid. The hot process (1st and 2d) is employed in preparing syrups from such solutions of drugs as are not injured by heat. The first method is adapted for preparing such syrups as those of orange or lemon, as the degree of heat is not sufficient to cause any injury to the preparation. The main objection to this process, however, is that it does not yield as clear and bright a syrup as process No. 2. In the preparation of syrups from drugs which are not injured by heat, the second process is preferable. In this the syrup is raised to the boiling point, whereby albuminous matters are coagulated, which are afterwards removed by strain- ing. Syrups which require concentration should be boiled briskly, until they have become sufficiently dense; this may be ascertained by dipping a rod or spatula into the liquid, and noting the viscosity on cooling. The syrup, on cooling, should not form a pellicle or crust upon the surface, which would show that it has been concentrated too far. The object of rapid con- centration is to avoid the browning of the syrup, which is caused by the prolonged application of heat. Saccharometers are often employed for this purpose; these enable the operator to control the concentration to a close degree of accuracy. The cold process is best adapted for the preparation of such syrups as those of garlic, almond, orange flowers, etc., as these depend on the presence of sensitive volatile principles for their activity. The sugar is dissolved either by simple agitation or by percolation as directed in the U. S. Pharmacopoeia. Syrups pre- pared according to this method from aqueous extracts of drugs, are very liable to ferment, owing to the presence of albuminous and certain extractive matters. These can be removed only by boiling, which causes their coagulation and precipitation. With this end in view, the Pharmacopoeia employs an alcoholic menstruum to exhaust the drug, thus avoiding the extraction of inert matter, while the active principles are retained in solution. In the concentration of these alcoholic solutions, care should be taken that the evaporation be carried on at as low a temperature as possible. The method of preparing syrups by the addition of fluid ex- tracts to simple syrup, is not under all circumstances advisable. Syrups made in this way usually deposit a sediment in time. The presence of a small amount of alcohol thus added is liable to bring about acetic fermentation of the syrup. SYRUPI. 277 Clarification.—Before the sugar is added, the medicated fluid should be perfectly clear and transparent. Many syrups after being prepared contain particles of finely divided matter in suspension, which interfere with their transparency, hence it is necessary that they be clarified. This may be accomplished by adding paper pulp (prepared from white filter paper) to the syrup, and agitating, or better, by adding it and heating it with the syrup during the process of solution, then filtering through paper of loose texture. The white of eggs (albumen) is also employed for this purpose; it should be beaten with a little water to form a froth, then mixed with the syrup, and the mixture boiled for a short time. The albumen coagulates, forming a scum which rises to the surface, which must be removed by skimming. The syrup is then filtered through paper or flannel. Preservation.—The fermentation (souring) of syrups is brought about by a variety of causes. One cause is the pouring of a syrup into an unclean or carelessly rinsed bottle. The presence of but a very small amount of old, partly soured syrup, or rinse-water, is sufficient to ruin the most carefully made preparation in a very short time. Syrups which contain too little sugar are very prone to ferment,'since, according to reasons already given, weak saccharine liquids afford excellent media for the growth of various microscopic organisms. Those syrups which contain too much sugar, deposit a portion of it on the sides and bottom of the vessel on standing; this causes a diminution in saccharine strength and liability to the same difficulty as above. Prolonged boiling of syrups, particularly when they contain acids, causes a partial inversion of the cane sugar into invert, or grape sugar. This latter is deposited in the bottle as a white, granular mass, thereby weakening the syrup, which rapidly fer- ments, owing to the favoring influence of the grape sugar present. Again, pouring hot syrups into bottles and not entirely filling them, favors fermentation, since the ascending aqueous vapors condense above and flow back to the surface, thereby diluting the upper layer of syrup; fermentation once having started, it rapidly extends throughout the entire mass. Bottles should hence be well filled and repeatedly shaken until cold. The commencement of vinous, or of acetic fermentation is readily noticed by the fluidity and frothiness of the syrup as well as by the odor ; the fluidity is caused by the loss of sugar, which has decomposed into carbonic acid (causing the frothing), and alcohol or acetic acid which are distinguished by their odor. The preparation may be saved if fermentation has not pro- ceeded too far, by boiling, which destroys the germs. It should not be forgotten, however, that this can only be applied to such as are not injured by heat. Syrups should be preserved in well filled, cork-stoppered vials in a cool place. 278 HANDBOOK OF PHARMACY. EXPLANATORY. Syrupus Acidi Hydriodici.—The hydriodic acid is developed by the reaction between the potassium iodide and tartaric acid, thus:— KI + H2C4H4O6 = KHC4H4O6 4- HI Potassium Tartaric Acid. Acid Potassium Hydriodic Iodide. 149.6 Tartrate. Acid. 165.5 127.5 The dilute alcohol is employed as solvent for the purpose of assisting the separation of the potassium bitartrate which is insoluble in this menstruum. The potassium hypophosphite * acts here as preservative agent, preventing decomposition of the hydriodic acid, which is caused by the separation of iodine, brought about by the influence of light and air (2HI -f- 0 — H2O -f- I2). The reaction between the hypophosphite and liberated iodine is as follows:— KH2PO2 + 41 4- 2H2O = KI + H3PO4 + 3HI Potassium Iodine. Water. Potassium Phosphoric Hydriodic Hypophosphite. Iodide. Acid. Acid. It is important that the potassium iodide be free from iodate, otherwise subsequent discoloration of the syrup will take place, through liberation of iodine by the action of the acid solution on the iodate in presence of iodide. This syrup is incompatible with potassium chlorate, mineral acids and salts of the metals; see also Syrupus Ferri lodidi. Assay.—In the U. S. Pharmacopoeia process of assay 31.88 Gm. of the syrup are first neutralized exactly with ammonia water, whereby ammonium iodide (HI J- NH3.H2O = NHJ -f- H2O) is formed. This is done in order to avoid the liberation of free nitric acid, which would prevent the precipitation of the silver iodide upon the addition of decinormal silver nitrate V. S., thus: AgNO3 + HI = Agl -f- HNO3. After neutralization with am- monia the reaction is as follows:— AgNO3 4- NHJ = Agl + NH4NO3 Silver Nitrate. Ammonium Silver Ammonium 165.5 Iodide. Iodide. Nitrate. HI = 127.5 Yellow potassium chromate f is used as indicator, to show the end of the reaction; the silver solution is added until the red color produced ceases to disappear on stirring, leaving the solu- tion of a permanent red tint (silver chromate). The silver will not unite or remain united with the yellow chromate of potassium (indicator) as long as any free hydriodic acid (or NHJ) is present, but as soon as the last trace of this has been precipitated, then * It is probable that traces of hypophosphorous acid are also produced H2C4H4O6 + KH2PO2 = KHC4H4O6 + H3PO2 Tartaric Acid. Potassium Acid Potassium Hypophosphorous Hypophosphite. Tartrate. Acid. t See Decinormal Silver Nitrate Volumetric Solution. SYRUPL 279 the next addition of silver solution produces the red silver chro- mate, at which point we stop. Since one molecule (169.5 parts) of silver nitrate is equivalent to one molecule (127.5 parts) of hydriodic acid, we have— AgNO3 Hl Silver Nitrate. Hydriodic Acid. 16.95 Gm. (1000 Cc. f0 V. S.) = 12.75 Gm. 0.01695 Gm. ( 1 Cc. ? y. S.) = 0.01275 Gm. 25 Cc. = 25 X 0.01275 = 0.3188 Gm. of Hydriodic Acid = 1 per cent, of 31.88 Gm. Or [(0.3188 -s- 31.88) X 100] = 1 per cent. Therefore, if 31.88 Gm. of the sample required 25 Cc. of deci- normal silver solution under the above conditions, the syrup is of the strength (HI) of 1 per cent. Exercise.—How much hydriodic acid can be produced from 13 Gm. of potassium iodide? If, according to the equation (page 278), 165.5 parts of potas- sium iodide are capable of yielding 127.5 parts of hydriodic acid, then 13 Gm. of potassium iodide will, under the same circum- stances, yield 10 + Gm. of hydriodic acid, for KI Hi KI Hl 165.5 : 127.5 :: 13 : x x = 10 -f- Gm. Exercise.—How much . tartaric acid is necessary to decompose 13 Gm. of potassium iodide into hydriodic acid ? According to the same equation, 149.6 parts of tartaric acid are necessary for the decomposition of 165.5 parts of potassium iodide, hence 13 Gm. of potassium iodide would require 11.7 + Gm. of tartaric acid:— ki h2c4h4o6 ki h2c4h4o6 165.5 : 149.6 : : 13 Gm. : x x = 11.7 + Gm. The U. S. P. requires 12 Gm. of tartaric acid for this purpose, so there is a slight excess of about 0.3 Gm. above the theoretical amount. Syrupus Allii (Syrup of Garlic).—The value of garlic depends upon its volatile oil, which consists mainly of allyl disulphide fc3h5—si rc3H5—s ] I I I (60 per cent.) and allyl propyl disulphide I I (7 L C3H5—s J . I c3h7 s j per cent.); these are very volatile, hence the syrup should be pre- pared by the cold process. The best menstruum for this purpose is diluted acetic acid. Syrupus Amygdala?.—This syrup is demulcent and sedative. The latter property is due to the presence of a small amount of hydrocyanic acid, which is formed, together with benzaldehyde (oil of bitter almonds), by the action of water upon the glucoside amygdalin contained in the almonds, under the influence of another 280 HANDBOOK OF PHARMACY. constituent, emulsin, which acts as a ferment, but does not take part in the reaction itself: C20H27NOu 4- 2H2O 4- Emulsin = 2C6H12O6 4- HCN 4- C6H5COH 4- Emulsin Amyg- Water. Glucose. Hydrocyanic Benzaldehyde. dalin. Acid. This syrup is prepared by the cold process, to avoid any danger of volatilizing the prussic acid. The same ferment or albuminoid, emulsin, also aids in emulsionizing the fixed oil present in the almonds, when the latter are triturated with water, the result being a milk-like fluid. Syrupus Calcis (Liquor Calcis Saccharatus, B. P.)—Cane sugar unites with different oxides and hydroxides of the metals to form a class of soluble compounds known as Saccharates. This is the case with calcium hydrate, the sugar forming with it at least four different compounds, according to the proportion of the two and the temperature employed (C12H220n. zCaO). When admin- istered, it should be well diluted with water. The syrup should be kept in well-closed vials, since it readily absorbs carbon dioxide from the air. Syrupus Ferri Iodidi.—On bringing iodine and clean, bright iron wire (card teeth) in contact, in presence of water, the follow- ing reaction takes place:— (a) Fe 4- 21 = Fel2 Iron. Iodine. Ferrous Iodide. 55.9 2 X 126.6 308.9 The reaction is known to be complete by the solution assum- ing a greenish color. Care should be taken that no particles of iodine remain adhering around the sides or neck of the flask, otherwise in pouring off the solution it will become contaminated with free iodine. The resulting syrup should have a bright pea- green color, free from any trace of yellowish cast. The solution on exposure to the air, also the syrup on standing, is prone to become discolored (yellow to brown), due to the separation of free iodine, thus:— (&) Fel2 4- 2H2O 4- O = Fe(OH)3 4- I 4- HI Ferrous Water. Oxygen. Ferrous Iodine. Hydriodic Iodide. Hydrate. Acid. The U. S. Pharmacopoeia directs to test for the presence of free iodine by the addition of starch paste, which produces a blue color. When in such a condition, the syrup should not be dis- pensed. The syrup or solution of ferrous iodide may be kept indefinitely, retaining its pea-green color, if a few pieces of clean iron wire (card teeth) be placed in the bottle, which is to be kept well closed. Should it have become discolored, it is best exposed to the direct sunlight; this causes a re-combination of the free iodine with the iron present. SYRUPI. 281 Syrup of ferrous iodide is incompatible with potassium chlo- rate, since free iodine is liberated, thus:— (c) 2FeI2 -|- KC1O3 — Fe2O3 + KC1 + 41 Also with salts of the metals, such as those of mercury, lead, silver, etc.; likewise with the inorganic acids. Assay.—The amount of ferrous iodide present is ascertained by means of decinormal solution of silver nitrate, which reacts according to the following equation :— (d) 2AgNO3 4- Fel2 = 2AgI + Fe(NOs)2 Silver Nitrate. Ferrous Iodide. Silver Iodide. Ferrous Nitrate. 2 X 169.5 308.9 Now, in this case, a measured excess of the silver solution is added, and the amount of uncombined silver is ascertained by means of decinormal potassium sulphocyanate V. S.,* ferric ammonium sulphate T. S. being used as indicator.! 1.55 Gm., or, if greater accuracy is required, 1.5447 Gm. of the Syrup are weighed off, and if it be of proper strength, 10 per cent, of this (0.155) should be ferrous iodide. To just precipitate this, 10 Cc. of the silver solution are required, for (e) 2AgNO3 Fel2 Silver Nitrate. Ferrous Iodide. 2 X 169.5 p., 308.9 p. 169.5 p.,154.4+ p. 16.95 Gm. (1000 Cc. V. S.), 15.444- Gm. 0.01695 Gm. (1 Cc. V. S.), 0.0544+ Gm. 10 Cc. = 10 X 0.01544 = 0.1544 + Gm. Fel2. But, since an excess of silver solution over and above what is necessary for the precipitation of the ferrous iodide has been added, this excess is estimated by adding decinormal potassium sulphocyanate V. S., until a red-brown tint remains after shaking. This shows that the sulphocyanate solution has precipitated all of the/ree silver nitrate, and that the slight excess of the sulpho- cyanate has reacted with the ferric ammonium sulphate, produc- ing a red-brown color (sulphocyanate of iron). (/) KSCN + AgNO3 = KNO3 + AgSCN Potassium Silver Nitrate. Potassium Silver Sulpho- Sulphocyanate. Nitrate. cyanate. Potassium Sulphocyanate, 97 p. = Silver Nitrate, 169.5 p. 9.7 Gm. (1000 Cc. V. S.) = 16.95 Gm. (1000 Cc. V. S.) 0.0079 Gm. (1 Cc. V. S.) = 0.01695 Gm. (1 Cc. V. S.) Thus one cubic centimeter of the sulphocyanate solution is equivalent to one cubic centimeter of the silver solution. The U. S. Pharmacopoeia states that only one cubic centimeter of the sulphocyanate solution should be required, if we had originally added 11 Cc. of the silver solution. Hence, 10 Cc. of this has been consumed by the ferrous iodide, indicating, accord- * See Decinormal Volumetric Potassium Sulphocyanate Solution. f Potassium chromate cannot be used here as indicator, since it reacts with the ferrous salt. 282 HANDBOOK OF PHARMACY. ing to the equation e, that the syrup is of proper strength (10 per cent.). Exercise.—Two grammes of a sample of Syrup of Ferrous Iodide were titrated. First, 12 Co. of decinormal silver nitrate V. S. were added, and afterward 3 Cc. of decinormal potassium sulphocyanate V. S. were required, until the solution assumed a red-brown color, ferric ammonium sulphate T. S. being used as indicator. What was the strength of the syrup? Since 1 Cc. of the sulphocyanate V. S. is equivalent to 1 Cc. of the silver V. S., hence 9 Cc. (12 Cc. — 3 Cc. = 9 Cc.) of the silver solution were consumed by the ferrous iodide. Now, since 1 Cc. of decinormal silver nitrate V. S. is equivalent to 0.0154 Gm. of ferrous iodide, hence 9 X 0.01544 = 0.1389 Gm.; consequently the 2 Gm. of the syrup contain 0.1389 Gm., or 6.94 + per cent, of ferrous iodide.* Exercise.—How much ferrous iodide can be obtained from 83 Gm. of iodine? Since, according to equation a, 253.2 parts of iodine yield 308.9 parts of ferrous iodide, 83 Gm. of iodine will yield 101.2 + Gm. of ferrous iodide, for Iodine. Ferrous Iodide. Iodine. Ferrous Iodide. 253.2 : 308.9 : : 83 : x x = 101.2 + Gm. ferrous iodide. Thus 83 Gm. of iodine will yield 101.2 + Gm. of ferrous iodide. * In a reaction of this kind the theoretical yield is never obtained, for moisture and impurities in the iodine will lower the results. SYRUPI. 283 TABLE OF U. S. P. SYRUPS CLASSIFIED ACCORDING TO MODE OF PREPARATION. Title. Active Constituents. Properties. Dose. Hot Process. Syrupus Acidi Hydriodici, . . HI, 1%. Alterative, 20 nv Calcis, Calcium Saccharate. Antacid, 20 m. Picis Liquidae, . . . Tar. Expectorant, 4-8 Cc. Eubi Idaei, Raspberry Juice. Vehicle. .’ 4 Sarsaparillae Com- positus, Fid. Ext. Sarsaparilla ; Fid. Alterative, 15 Cc. Ext. Senna. Syrupus. Vehicle. Tolutanus, Balsam of Tolu. Vehicle. Cold Process. Syrupus Allii, Garlic. Stimulant, Expec., 4 Cc. Althaeae, Marshmallow. Demulcent. Amygdalae, Almond—HCN. Demulcent, Sedative. Aurantii, Sweet Orange Peel. Vehicle. Aurautii Florum, . . Orange Flower Water. Vehicle. Calcii Lactophos- phatis, Calcium Lactophosphate. Tonic, 10-15 Cc. Hypophosphitum, . . Ca, K, Na, Hypophosphites. Tonic, 4-8 Cc. Ipecacuanhae, .... Fid. Ext. Ipecac. Expectorant, 2-30 nt. Lactucarii, Lactucarium. Hypnotic, 7-10 Cc. Pruni Virginianae, . . Wild Cherry. Vehicle. Scillae, Vinegar of Squill. Expectorant, 10-30 nt. Diaphoretic. Scillae Co., Fid. Ext. Squill ; Fid. Ext. Senega ; Tartar Emetic. Senegae, Fid. Ext. Senega. Expectorant, 3-8 Cc. Sennae, Senna. Cathartic, 4-15 Cc. Zingiberis, Fid. Ext. Ginger. Vehicle. Simple Admixture with Syrup. Syrupus Acaciae, Mucilage of Acacia. Vehicle. Acidi Citrici, .... Citric Acid. Vehicle. Ferri lodidi, .... Ferrous Iodide, 10%. Alterative, 10-20 Cc. Ferri, Quininae et f Ferric Phosphate, 2%. 1 Strycbninae Phos-j Quinine Sulphate, 3%. >■ Tonic, 4 Cc. phatum, . . . . ( Strychnine, 0.02%. J Hypophosphitum cum Ferro, .... Ferrous Lactate, 1% Syrup of Tonic, 4-8 Cc. Hypophosphites. Krameriae, Fid. Ext. Krameria. Astringent, 2-4 Cc. Rhei, Fid. Ext. Rhubarb. Laxative, 4 Cc. Rhei Aromaticus, . . Arom. Tr. Rhubarb. Purgative, 4 Cc. Rosae, Fid. Ext. Rose. Vehicle. Rubi, Fid. Ext. Rubus. Astringent, 4-8 Cc. 284 HANDBOOK OF PHARMACY. MELLITA— (Honeys). The official Honeys are a class of thick or semi-liquid, sweet, medicated preparations, differing from syrups in that honey is employed as the base instead of simple syrup. This class of preparations was formerly quite popular, but their number has been gradually lessened by the various pharma- copoeias, until at present Mel Despumatum and Mel Rosse consti- tute the only ones remaining. These two are employed simply as bases, or vehicles, for the administration of other remedies. Great caution should be observed in the selection of honey for pharmaceutical purposes; for, because of its peculiar viscidity, it is easily adulterated with glucose. Mel Despumatum. — The U. S. Pharmacopoeia directs the strained honey to be clarified by heating it on a water-bath with paper pulp, as long as any scum (consisting of wax and other lighter impurities) rises to the surface. This is removed by skimming. Then, after straining, 5 per cent, of glycerin is added for the purpose of protecting the honey from any change. A more brilliant preparation is obtained if it be filtered through paper* in a steam-jacketed funnel (“Hot Filtration,” page 179). Various other clarifying agents are in use and have been sug- gested, among which are gelatin, white of egg, Irish moss, animal charcoal, aluminum hydroxide, etc.; but all these require that the honey be diluted with water, necessitating therefore subse- quent evaporation, which results in impairing the aroma and often the color of the honey. These consist of simple or medicated honey mixed with acetic acid. Oxymel of the British Pharmacopoeia consists of a mixture of clarified honey (40 oz.), acetic acid, and water (each 5 fl. oz.). Other pharmacopoeias direct that the honey be mixed with dilute acetic acid and evaporated. The simplest process is that of the Ph. Ger. I, which consists in mixing 40 parts of clarified honey with 1 part of acetic acid (sp. gr. 1.040). The most popular preparation of this class is the Oxymel Scillse, which is made by mixing Vinegar of Squill with clarified honey. OXYMELLITA. B. P. Fr. Ph. Germ. Ph. Vinegar of Squill, 1 pt. 1 pt. 1 pt. Clarified. Honey, 1.6 pt. 4 pt. 2 pt. * For filtering syrups, honey, oils, etc., Schleicher & Schtill’s filter paper, Nos. 586 and 584, are especially adapted. SYRUPI. 285 ELIXIRIA—{Elixirs). Elixirs are sweetened, aromatic, hydro-alcoholic, medicated preparations. The word “elixir” is derived from the Arabic ilcsir (itself derived from the Greek), a name applied by alchemists to a wonderful powder capable of transforming base metals into gold and silver. This term was later applied to compound tinctures which were supposed to possess rare medicinal virtues. In modern times, this title was applied in European countries to concentrated alcoholic extracts of drugs usually of disagreeable taste. Later, in American pharmacy, it has been applied to an entirely different class of preparations, characterized by their pleasant aromatic taste and containing from 20 to 25 per cent, of alcohol. The objection to these preparations is that, owing to the small percentage of medicinal agent present, the dose is necessarily large, the alcohol present often seriously interfering with the medicinal action of the drug. The U. S. Pharmacopoeia recognizes Elixir Aromaticum, which is employed simply as an aromatic flavoring agent, and Elixir Phosphori, each cubic centimeter of which represents 0.00025 Gm. of phosphorus, corresponding to about of a grain in each teaspoonful. CHAPTER XXX. SOLUTIONS (G-ycerin as Solvent). GLYCERITA—(Glycerites). Glycerites are solutions of medicinal agents in glycerin. Glycerin, because of its valuable solvent properties and freedom from rancidity, forms an excellent vehicle for the external appli- cation of many organic and inorganic substances. Glycerin not only effectually protects sensitive compounds from oxidation and change, but also affords permanent elegant solutions which form emollient and soothing applications. Such concentrated solutions as those of carbolic, tannic, and gallic acids, etc., are very convenient, because they readily yield clear solutions on dilution with water. The U. S. Pharmacopoeia recognizes 6 glycerites. GLYCERITA, U. S. P. Title. Constituents. Properties. Glyceritum Amyli, . . . Starch, Water, each 10 Gm. Glycerin, 80 Gm. Emollient, Base, and Excipient. “ Acidi, Carboli- ci, . . . . Carbolic Acid, 20 Gm. Glycerin, 80 Gm. Diluted as a Wash. “ Acidi, Tanni- ci, . . . . Tannic Acid, 20 Gm. Glycerin, 80 Gm. Local Application, Astringent. “ Boroglycerini, Boric Acid, 310 Gm. Glycerin to make 1000 Gm. Antiseptic. “ Hydrastis,. . Hydrastis, Water (Alcohol). Glycerin. Diluted, Wash. “ Vitelli, . . . Egg Yolk, 45 Gm. Glycerin, 55 Gm. Local Application. 286 CHAPTER XXXI. SOLUTIONS (Oleic Acid as Solvent). Oleates are solutions of bases (metallic or alkaloidal) in oleic acid. These preparations as recognized by the Pharmacopoeia are not definite chemical compounds; they are simply solutions obtained by triturating the medicating substance with a large excess of oleic acid. In the preparation of the oleates, wherever possible, the application of heat should be avoided, since, owing to the reducing properties of the oleic acid, the metallic oxides may be reduced to their metals, which precipitate from solution. As an example of this, the official oleate of mercury, even when prepared in the cold, will on standing deposit more or less metallic mercury. This decomposition will take place more rapidly if heat has been employed in its preparation. In preparing the oleates of any of the metals, only the freshly precipitated, well-dried metallic oxide should be used, on account of the comparatively greater solubility of the freshly prepared oxide. When preparing the oleates of the alkaloids, it must be remembered that only the free alkaloids, and not their salts, are soluble in oleic acid. When the free alkaloid is not at hand, it can be readily prepared from any of its salts by dissolving the necessary quantity in water, by aid of a little dilute acid if necessary, then adding slowly, with constant stirring, diluted ammonia water, or another suitable alkali, until it is in slight excess. The precipitated alkaloid is then collected on a plain filter, washed with cold water to remove most of the ammonium or alkali salt present, and dried at 100° C., when it is ready for solution in the oleic acid. In preparing these oleates, only porcelain or glass utensils should be used, and either glass rods or horn spatulas should be used for stirring Dry Oleates.—These dry oleates, or more properly oleopalmi- tates, are not official; they are definite chemical compounds obtained by interaction between solutions of sodium oleate and metallic salts. Sodium Oleate may be made by warming 100 parts of oleic acid in a dish to 60° C., then adding a solution of 16 parts of caustic soda in a mixture of 30 parts of alcohol and 90 parts of water, until the acid is neutralized, which is shown by the fact that a faint red tint is imparted to the solution by phenolphta- lein. This soap (sodium oleate) is then dissolved in about 2000 parts OLE AT A—(Oleates'). 287 288 HANDBOOK OF PHARMACY. of water, and into it is poured, under constant stirring, a solution of the salt (in molecular proportion) in about 800 parts of water. The resulting precipitate should settle rapidly, leaving a clear, supernatant liquid. Should this not be the case, but the solution remain of a milky appearance, then an insufficient amount of the salt has been added. The reaction takes place according to the following equation:— 2C17H33COOH + 2NaOH = 2C17H33COONa + 2H2O Oleic Acid. Sodium Hydrate. Sodium Oleate. Water. 2 X 281.3 2 X 40 2 X 303.3 2C17H33COONa + Zn(C2H3O2)2 = { }Zn + 2NaCffI3O2 Sodium Oleate. Zinc Acetate. _V *?, , Sodium 2 X 303.3 182.8. Zinc Oleate. Acetate. The following formula may be given for practical use:— Oleic Acid (sp. gr. 0.890 to 0 900), 100 grains. Sodium Hydrate 16 grains or q. s. Alcohol, 1 fluidrachm. Zinc Acetate, 550 grains. Or, Lead Acetate, 675 grains. Or, Copper Sulphate, 442 grains, etc. If cold solutions are employed, the oleate will form a light, flocculent precipitate; if the solutions are hot, the oleate will form a soft, sticky mass. If a dry pulverulent oleate is desired, the precipitate obtained under the beforenamed conditions is collected on a strainer and well washed until all traces of the inorganic salt formed in the reaction have been removed; it is then dried by spreading it out on porous tiles or bibulous paper and placing it in a dry place. The oleate obtained by precipitation from a hot solution should be washed by stirring it with hot water, then deprived of water by placing it in a dish on a water-bath and heating. When cold it may be moulded into sticks or pul- verized. These oleopalmitates* may be more conveniently made by dissolving 1 part of Castile soap (sodium oleopalmitate) by means of heat in 8 parts of water, allowing to stand 24 hours so as to permit the deposition of the greater portion of sodium pal- mitate; the clear, supernatant liquid, consisting of sodium oleate, is then decanted off. To this solution is now added, under the same conditions as already mentioned, a slight excess of an aqueous solution of a metallic salt. It should be observed that the saline solution should not contain any free acid, otherwise free palmitic acid will be precipitated. For all practical purposes, an oleate prepared as above directed is sufficiently free from palmi- tates.! These Oleates are employed in dermal medication, their medi- cinal properties depending upon the base present, and their action being influenced by the readiness with which oleic acid is absorbed by the skin. * Druggists' Circular, 1885, page 2. f Dr. L. Wolff, Amer. Jour. Phar., 1881, p. 545. SOLUTIONS. 289 The Pharmacopoeia recognizes two oleates made from a metallic base, viz., Oleatum Hydrargyri and Zinci, and one made from an alkaloid, viz., Oleatum Veratrinae. Exercise.—It is desired to prepare 1 fluidounce of a 25 per cent, solution of Oleate of Quinine, it being assumed that the operator has no free quinine (that is, the alkaloid itself) in stock, but that he has the sulphate. The first step will be to ascertain how much of the free alka- loid will be needed ; thus, 25 per cent, of 410.1 grains, the weight of one fiuidounce of oleic acid (455.7 X 0.900), is 102.5 + grains, the weight of the alkaloid necessary; this is then to be dissolved in 353.2 grains of oleic acid. Owing to the fact that the alkaloid does not occupy the same bulk, weight for weight, as the oleic acid, we would obtain a little less than one fluidounce, hence it is better to prepare a little more (taking, for instance, 500 grains of oleic acid) than necessary, and to throw the slight excess away, or to reserve it for future use. The 102.5 grains of the alkaloid Quinine, which are required for the above-given problem, must be prepared from the Sulphate. Now, if, according to the follow- ing equation, 646.6 parts of Quinine correspond to 870.2 parts of the Sulphate, to obtain 102.5 grains of the alkaloid will require 137.9 fl- grains of the Sulphate. (C20H24N2O2)2H2SO4.7H2O + 2NH4OH = 2C20H24N2O2 + (NH4)2SO4 + 9H2O Quinine Sulphate. Ammonia Water. Quinine. Ammonium Water. 870.2. 2NH3 = 34. 2 X 323.3 Sulphate. For Quinine. Quinine Sulphate. Quinine. Quinine Sulphate. 646.6 : 870.2 : : 102.5 : x x = 137.9 + Hence, we would require 137.9 + grains of quinine sulphate and 353.2 grains of oleic acid to prepare a fluidounce (approxi- mately) of a 25 per cent, solution. CHAPTER XXXII ETHEREAL SOLUTIONS. OLEORESIN JE-(Oleoresins). Oleoresins are ethereal extracts of an oleoresinous nature, obtained from vegetable drugs by percolation with ether. The drugs selected for this class of preparations are those whose activity resides chiefly in their fixed oil and resin. These constituents are readily extracted from the drug by means of such solvents as ether, chloroform, acetone,* benzin, etc. Among these the Pharmacopoeia selects ether as the most suitable. Fluid extracts are also prepared from some of these drugs, but they do not represent the same medicinal properties, since alcohol extracts a different class of principles. The Pharmacopoeia directs that the drug be firmly packed in a suitable percolator for volatile liquids, and that this be provided with a glass stopcock (Fig. 307). In the absence of such an apparatus, any small percolator may be used, and loss through volatilization of men- struum be guarded against by closing the top of the percolator securely by means of a large jar- cork, through which air is admitted by means of a small tube. The perforated cork inserted in the outlet of the percolator should carry a long glass tube which extends into a securely covered receiving bottle, allowance being, of course, made for the escape of air. Rubber should not be used. Another form of percolator adapted to this pur- pose is shown in Fig. 328. The powdered drug is packed in the percolator, a, and the solvent poured over it. After sufficient maceration, the stopcock, c, is opened sufficiently to allow the proper rate of percolation. The connecting tube is to prevent any loss of volatile solvent, also for the purpose of equal- izing the air pressure. It will be seen that the process of perco- lation demands the handling and use of comparatively large quantities of ether, which, with the subsequent distillation neces- sary, renders the process more or less dangerous as well as wasteful. These difficulties are readily overcome, when only small quantities of the drug are to be operated upon, by the use of the Soxhlet’s Extraction Apparatus (Fig. 329), which permits the complete extraction of the powdered drug with a very small amount of ether. In the flask, a, is placed the necessary volume Fig. 328. Percolator for Volatile Solvents. * G. M. Beringer, Amer. Jour. Phar., p. 145, 1892. 290 ETHEREAL SOLUTIONS. 291 of ether (about 50 Cc.). The powdered drug (about 50 Gm.), e, having been firmly packed into a cartridge of filter paper, is introduced into the Soxhlet tube, d; the latter is in turn con- nected with the upright condenser, c. The flask, a, is now heated gently on a water-bath, the vapor of the ether rises through b, condenses above and drops on to the powder in the cartridge. After percolating through to the bottom of the tube, d, the solvent charged with the soluble matter of the drug rises in the siphon, f, which, as soon as it becomes sufficiently filled, discharges its con- tents into the flask, a. This process repeats itself, and is continued until the drug is exhausted, requiring usually from one to two hours. The flask, a, may be connected with a condenser, and the solvent recovered by distillation, or the con- tents of a may be poured into an evaporating dish and the slight excess of ether allowed to evapo- rate spontaneously. Commercial oleoresins vary considerably in quality; it therefore behooves the apothecary to prepare his own. The Pharmacopoeia recognizes six oleoresins; specifying in the instance of oleoresin of male fern, that the granular-like deposit (filicic acid) to which the activity is mainly due, should be thor- oughly mixed with the liquid portion before use. In oleoresin of cubeb a waxy and crystalline de- posit (cubebin) also occurs on standing, but as this has no medicinal value, it should be discarded. The oleoresins should be administered in diluted form, either in emulsion or pill. Male-fern is best administered in gelatin capsules. The U. S. Pharmacopoeia recognizes 6 Oleoresins. Fig. 329. Soxhlet’s Extraction Apparatus. OLEORESINA5, U. S. P. Title. Color—Average Yield. Properties. Dose. Oleoresina Aspidii, . . . Dark-Green, about 16-18%. Tamicide, 30-60 no. 14 Capsici, . . . Dark Red-Brown, about Stimulant, | to 1 no- 17-20%. Rubefacient. 4 4 Cubeba:, . . . Greenish-Brown, about Diuretic. 18-22%. Expectorant, 5-30 no. 44 Lupulini, . . Reddish Brown ; about 55 %. Tonic, sedati ve, 2-10 no. 44 Piperis, . . . Greenish-Black, about 6-8%. Stimulant, | to 1 no- 4k Zingiberis, . . Dark-Brown, about 5%. Stimulant, j to 1 no. 292 HANDBOOK OF PHARMACY. COLLODIA—{Medicated Collodions). The medicated Collodions consist of collodion impregnated with medicinal substances. They are only employed externally. Collodion, the base of this class of preparations, is prepared by dissolving pyroxylin (soluble gun cotton) in a mixture of 3 parts of ether and 1 part of alcohol. The Pyroxylin is obtained by the action of nitric acid (with assistance of sulphuric acid) upon cotton (cellulose). When nitric acid is caused to react on cellulose (C6Hi0O5), various substitution products are formed, according to the strength of the acids employed, being designated as mono-, di-, and tfn-nitrocellulose,* etc. Only one of these, the di-nitrocellulose, is completely soluble in the ether-alcohol mix- ture; this should not be confounded with the explosive hexa- (or tri-) nitrocellulose. When collodion is applied to a dry surface, the ether and alcohol rapidly evaporate and leave a transparent, adhesive, and con- tractile film behind. For this reason it forms a valuable application for keeping together the edges of small wounds, or for covering ulcers or abraded surfaces. When it is simply desired to protect the surface, a flexible (non-contracting) film is desirable; for this purpose the official Collodium Flexile should be used. Collodion is made the vehicle for the application of various remedies, such as iodine, cantharides, corrosive sublimate, etc. Because of the volatile nature of the ether, the collodions should be kept in well-stoppered vials in a cool place, and because of the extremely inflammable nature of both the pyroxylin and the ether-alcohol, it should not be dispensed or applied in proximity to a light, or fire. Title. Constituents. Use. Collodium, Pyroxylin, 30 Gm.; Ether, 750 Cc.; Alcohol, 250 Cc. Protective Application. Collodium Cantharidatum, Cantharides, 60 Gm.; Chloro- form; Flexible Collodion, 85 Gm. Blistering Application. Collodium Flexile, . . . Collodion, 920 Gm.; Canada Turpentine, 50 Gm.; Castor Oil, 30 Gm. Protective Application. Collodium Stypticum, . . Tannic Acid, 20 Gm.; Alcohol, 5 Cc.; Ether, 25 Cc. Styptic Application. COLLODIA, U. S. P. * These are compounds in which the nitric acid residue (NO3) replaces hydroxyl (Oil) groups in the cellulose formula. The double formula of cellulose (C12H20Oi0) is taken. Then by the action of nitric acid under different circumstances we obtain, CjoHigOg (NOS),Mono-nitrocellulose. C12H13O8 (N03)2, Di-nitrocellulose, official soluble gun cotton. Ci2II1707 (NO3'3, .... Tri-nitrocellulose. C12H1404 (NO3 6,Hexa-nitrocellulose, explosive gun cotton. CHAPTER XXXIII. MIXTURES. FLUID MIXTURES. These consist of transparent, or opaque fluids, resulting from the mixing of various liquids, or liquids and solids. LINIMENTA. Liniments, according to the Pharmacopoeia, are solutions or mixtures of various medicinal substances with alcohol or oleag- inous fluids, intended for external application. When dispensed, they should always be properly labeled as Liniments, or for “External Use.” The U. S. Pharmacopoeia recognizes 9 Liniments. LINIMENTA, U. S. P. Title. Constituents. Base. Linimentum Ammoniae, Ammonia Water, 350 Cc.; Cotton Seed Oil. (Volatile Alcohol, 50 Cc.; Cotton Seed Belladonnae, Oil, 600 Cc. Camphor, 50 Gm.; Fl’d. Ext. Fl’d. Ext. Belladonna. Calcis (Catron Oil), . . Belladonna, to make 1000 Cc. Solution Id me ; Linseed Oil, Linseed Oil. Camphor®, equal parts. Camphor, 200 Gm.; Cotton Cotton Seed Oil. Chloroformi, Seed Oil, 800 Gm. Chloroform, 300 Cc.; Soap Soap Liniment. Saponis, Liniment, 700 Cc. Soap (powd.), 70 Gm.; Cam phor, 45 Gm.; Oil Rosemary, 10 Cc.; Alcohol, 750 Cc.; Water, to make 1000 Cc. Soft Soap, 650 Gm.; Oil Lav- Diluted Alcohol. Saponis Mollis, .... Diluted Alcohol. Sinapis Coinpositum, . ender Flowers, 20 Cc.; Alco- hol, 300 Cc.; Water, to make 1000 Cc. Vol. Oil Mustard, 30 Cc.; Fl. Ext. Mezereum, 200 Cc.; Camphor, 60 Gm.; Castor Oil, 150 Cc.; Alcohol, to make 1000 Cc. Resin Cerate, 650 Gm.; Oil Alcohol. Terebinthinae, .... Oil of Turpentine. Turpentine, 350 Gm. 293 294 HANDBOOK OF PHARMACY. MISTURA?—{Mixtures). Mixtures, as here understood, are a class of aqueous prepara- tions which contain solid, insoluble substances, in such a con- dition of subdivision, that, upon agitation, the particles remain for some time in a state of suspension. In three instances the Pharmacopoeia directs the intervention of gum arabic or sugar for the purpose of assisting suspension. As exception to the above definition, due to the indiscriminate use of the term, we have two solutions included under this class, viz., Mistura Glycyrrhizae Composita and Mistura Rhei et Sodae. This class of preparations should not be kept on hand any great length of time, since they are prone to ferment. The U. S. Pharmacopoeia recognizes 4 Mixtures. MISTURzE, U. S. P. Title. Constituents. Properties. Dose. Mistura Cretae, (Chalk Mixture). Comp. Chalk Powder, 200 Gm.; Cinnamon Water, 400 Cc.; Water, sufficient to make 1000 Cc. Antacid, 15 Cc. ‘ ‘ Ferri Composita, (Griffith's Mixture). ‘ ‘ Glycyrrhizae Com- Ferrous Sulphate, 6 Gm. ; Myrrh, 18 Gm.; Sugar, 18 Gm.; Potassium Carbonate, 8 Gm.; Spirits Lavender, 60 Cc.; Rose Water, sufficient to make 1000 Cc. Tonic, 30-60 Cc. posita, .... (Brown Mixture). Ext. Liquorice, pure, 30 Gm.; Syrup, 50 Cc. ; Mucilage Acacia, 100 Cc.; Camphor- ated Tr. Opium, 120 Cc.; Wine of Antimony, 60 Cc.; Spirits of Nitrous Ether, 30 Cc.; Water, sufficient to make 1000 Cc. Expectorant, 5-30 Cc. “ Rhei et Sodae, . . Sodium Carbonate, 35 Gm.; Fid. Ext. Rhubarb, 15 Cc.; Fid. Ext. Ipecac, 3 Cc.; Gly- cerin, 350 Cc.; Spirit of Peppermint, 35 Cc.; Water, sufficient to make 1000 Cc. Carminative, 2-4 Cc. Laxative, 15-60 Cc. MIXTURES. 295 EMULSA, OR EMULSIONES—(Emulsions). Emulsions are artificial mixtures of a milky appearance, which consist of oils, fats or resinous substances suspended in water by the intervention of some viscid, or mucilaginous substance. The object sought is to break up the substance which is to be emulsified, into as minute particles as possible, enveloping each of these in a coat of the emulsifying agent, which tends to pre- vent them from reuniting. Natural Milk, which consists of minute globules of fat (butter) suspended in water by means of the casein present, may be regarded as a sample of a perfect emulsion. The more closely an artificial emulsion can be made to resemble milk, the more permanent will be the product. An emulsion is perfect when the oil globules are invisible to the naked eye. The completeness of emulsification may be judged by placing a sample on a slide under the lens of a microscope, and comparing the size and uniformity of the oil globules of the emulsion with those contained in a sample of milk. Emulsions may be divided into three classes—the Natural Emulsions, the Gum-Resin and Seed Emulsions, and the Oil or Artificial Emulsions. 1st. Natural Emulsions are such as exist ready formed in nature, such as milk, yolk of egg, certain plant juices, etc. 2d. Gum-fem and Seed Emulsions.—Such gum resins as am- moniac, asafoetida, and myrrh, when triturated with water, form emulsions in which the resinous and oily constituents are sus- pended by means of the gummy matter present. In preparing these emulsions (Emulsa, U. S. P.), the powdered gum-resins should never be employed, since the process of drying and powdering not only destroys the volatile constituents, but also the emulsifying properties of the gum. Selected tears of the gum resins should be reduced to a coarse powder and then triturated with a small quantity of water, until a smooth paste is obtained, then the balance of water added, and the mixture finally strained. Under this class, the Pharmacopoeia recognizes two, viz.: Emul- sum Ammoniaci and Emulsum Asafoetidae. On triturating such seeds or fruits as the poppy, hemp or almonds with water, an emulsion is obtained in which the oily matter present is suspended (emulsified) by means of the albumi- nous and gummy matter. Under this class the Pharmacopoeia recognizes Emulsum Amygdalae, in which acacia and sugar are added to enhance the permanency of the preparation. 3d. Oil or Artificial Emulsions.—There are a great many differ- ent agents and methods by which we can produce artificial emulsions; most general among these, are the two methods known as the Continental and English. 296 HANDBOOK OF PHARMACY. 1st. The Continental Method. This method depends on the formation of a nucleus obtained by- agitating or triturating together certain quantities, by weight, of oil, gum and water. This so-called nucleus being once prepared, it may be diluted with water, in all proportions, without any danger of subsequent separation. This method never fails to produce a model emulsion, if the proper proportions (by weight) of oil, gum, and water be observed. The German Pharmacopoeia directs the following proportions: oil, 2 parts; pulverized acacia,* 1 part; water,f 1| parts, for such oils as are difficult to emulsionize, like the class of volatile oils. For the class of fatty oils (cod-liver oil, castor oil, etc.), the propor- tion of acacia to oil may be reduced to 1 part of gum to 4 parts of oil. The operation may be carried out in three different ways, the first being the most generally employed. (а) The 2 parts (or 4) of oil are stirred with the 1 part of powd. acacia in a dry mortar, then the If parts of water, are added at once, the whole being rapidly stirred with the pestle until a thick, creamy emulsion results, which is then diluted as desired. After some experience, this operation may be carried out in a bottle, which must, however, be thoroughly dry before the acacia is introduced. The chief mistake committed by beginners is that they permit the acacia and oil to remain too long in contact, whereby the gum becomes a hard mass, which afterward dissolves only with great difficulty. The two should be stirred or shaken together sufficiently long enough to thoroughly coat each particle of gum with a layer of oil, after which the water should be immediately added. (б) The 1 part of pulv. acacia is triturated with If parts of water until a uniform paste results, then the 2 parts (or 4) of oil are added at once and triturated rapidly until a thick, creamy emulsion nucleus results. (c). In a mortar place 1 part of powdered acacia; in a flask shake a mixture of 2 parts (or 4) of oil and If of water, and pour this over the gum, stirring rapidly until emulsified. This nucleus should, when properly prepared, present a uniform, creamy appearance; a pearly, translucent appearance assumed by the mixture indicates that an insufficient amount of water or gum is present, and that globules of uncombined oil are floating about. If this is not quickly remedied, the emulsion will “ crack,” that is, the oil will separate from the aqueous fluid. 2d. The English Method.—This method is applied generally to uncertain combinations, and must be followed carefully to insure * Coarsely powdered (granulated) acacia should always be preferred for making emulsions, because, of its ready solubility, and when triturated with oil or water, it is not liable to form “ lumps” like the tine powder; the latter is also open to the objection that it is often found adulterated in the market. f That is, as much in weight as one-half of the sum of the weight of oil and gum together. MIXTURES. 297 success. A thick, smooth mucilage of gum and water is first prepared in a mortar, and to this are added the oil and water, alternately, in small portions at a time, under rapid stirring, so as to break up the oil into globules, which are immediately enveloped by the viscid solution. Care should be taken in the early stage of the process to add the oil and water very cautiously, until a thick, creamy emulsion is obtained ; afterward they may be added more rapidly. A fresh portion of oil should never be added until the former has been thoroughly emulsionized. It often happens, from too great haste in adding the first por- tions of oil and water, or by reason of the mucilage not being thick enough, that the emulsion “ cracks; ” when this is the case, a fresh portion of thick mucilage of acacia should be taken and the mixture re-emulsionized in this by thorough trituration after each addition. As an example of this method of emulsionizing, the following formula is selected :— R. Copaibae, f 3 vj Pulv. Acaciae, £iij Aquae, q. s. ad. Place the Acacia (granulated) in a mortar and triturate with two drachms of water, until a perfectly smooth, thick paste results; then add under constant, rapid stirring, alternately, first a little of the copaiba, then a little water, continuing thus until all of the balsam has been thoroughly emulsified, after which the balance of the water may be added. In the preparing of an emulsion, such as usually prescribed by physicians, the various ingredients should be mixed in the follow- ing order: first, the emulsion nucleus of the oil is prepared; then the flavoring is added, if it be an oil; and this is followed by the syrup and the greater portion of the diluent. Should there be any salts, solid extracts, etc., to be combined, they are dissolved in a little of the reserved diluent and added last with agitation. Should there be small amounts of alcoholic liquids or acid solutions to be added, they should be diluted with a portion of the diluent, and added last, in small portions, the mixture being well agitated after each addition. Among the many proposed, the following are the most important:— Tragacanth forms an excellent emulsifying agent, a much less quantity of it being required than of acacia, while it yields, at the same time, a more prominent emulsion. For emulsifying the fatty oils, a smooth paste* composed of 1 part of tragacanth and OTHER EMULSIFYING AGENTS. * Best made by placing 1 part of pulverized tragacanth in a graduate, thoroughly moistening ■with the same amount of alcohol, then adding the boiling water under constant agitation. 298 HANDBOOK OF PHARMACY. 20 parts of water is macle, and to this is added at once, with rapid stirring, 20 parts of the oil to be emulsified, and 10 parts of water. For volatile oils (oil of turpentine, cubebs, etc.), the fol- lowing procedure may be followed: Oil, 8 parts; powdered traga- canth, 1 part, and water 15 parts. To the oil, contained in a dry bottle or mortar, add the tragacanth and shake or stir well, then add the water (15 parts), and agitate vigorously. This may be followed by the syrup and remaining diluents, added gradually in portions, the mixture being agitated after each addition. Yolk of Egg.—This being a perfect natural emulsion, forms an excellent nucleus, yielding a permanent combination. The albu- men of the egg should be entirely removed (as its presence is apt to give rise to failure), the yolk is placed in a mortar and ren- dered perfectly smooth by trituration, then, with a rapid circular motion of the pestle, the oil is added by degrees; should it become too thick, a little water may be added, which is then to be fol- lowed by the syrup and the other constituents. The emulsifying power of one fair-sized egg is equivalent to about 10 grammes of gum arabic or 1.25 grammes of tragacanth. The National Formulary has the following formula:— Cod-liver Oil, 8 fl. ozs. (other fatty oils may be substituted in place of this). Glycerite of Yolk of Egg, ... 2 J fl. ozs. Syrup of Tolu, 2 fl. ozs. Flavoring, (a sufficient quantity). Water, enough to make 16 fl. ozs. “ Triturate the glyconin in a mortar with the oil added in small portions at a time, and thoroughly incorporate each portion before adding the next. Then, continuing the trituration, gradu- ally add the syrup of tolu and flavoring. Finally, add enough water to make 16 fluidounces.” Dilute acids or acid salts or glycerin may be added to these emulsions without danger of causing them to “ crack.” Irish Moss.—For emulsifying oils, this is superior to acacia, because a subsequent separation of the emulsion does not take place. It also retains resinous bodies longer and more effectually in suspension. On the other hand it does not effect as fine a subdivision of the oil as is the case with acacia. In using Irish Moss it is necessary first to prepare a clear smooth mucilage. For this purpose 1 part of Irish Moss is washed in cold water to remove the adhering impurities and saline matter, then placed in a capsule or beaker and 40 parts of water added, then heated on a boiling water-bath for at least 15 minutes, under frequent stirring. The resulting mucilage* is then strained through wetted muslin, and enough water passed through the strainer to make * Should the mucilage be of a dark-brown color, it may be readily bleached by adding a few cubic centimeters of sulphurous acid, agitating, then placing in a capsule and heating on a water-bath until the odor of the acid has entirely disappeared. MIXTURES. 299 the product weigh 40 parts. Five parts of this mucilage are suffi- cient to emulsionize 8 parts of oil (fixed). To the mucilage con- tained in a bottle, add the oil in portions, agitating thoroughly after each addition; follow this up by the syrup, flavoring, and water as may be necessary. These emulsions are very prone to fermentation; hence, when it is necessary to preserve them for any greater length of time, it is well to introduce about 1 part of alcohol (substituting this for the same volume of water) into each 16 parts of emulsion. The mucilage of Irish Moss may be better preserved by pour- ing it while hot into bottles, which are filled to the neck, then adding a' thin layer of olive or cotton-seed oil, and securely sealing and preserving in a cool place. Quillaja Bark.—This contains a principle (called saponin), which possesses powerful emulsifying properties, but, owing to the large amount necessary and its expectorant properties, it should not be employed unless by consent of the physician. For pre- paring emulsions, it is employed in the form of a tincture, which may be made, according to the U. S. Pharmacopoeia, by boiling 200 Gm. of the bark, in fine chips, with 800 Cc. of water, washing the residue, boiling the whole liquid down to 600 Cc., then strain- ing, adding 350 Cc. of alcohol, filtering, and adding enough water to the filtrate to make it measure 1000 Cc. One part of the tinc- ture is sufficient to emulsionize 8 parts of fixed oil (cod-liver oil, castor oil, etc.). Volatile oils (oil of turpentine, cubebs, etc.) require their own measure of the tincture. The valuable feature of Quillaja as an emulsionizing agent lies in the fact that it is utterly indifferent to all substances tending to destroy gum emulsions. Extract of Malt.—This forms a valuable emulsifying agent for cod-liver oil, for which purpose it is admirably adapted thera- peutically. An extract of malt should emulsify its own weight of cod-liver oil. The oil should be gradually added to the extract of malt under constant stirring. Casein (Saccharated).—In the prototype of a perfect natural emulsion, milk, we find that the fat (butter) is held in suspension by the casein of the milk. The idea of the employment of this casein occurred to M. L6ger, of Paris, who proposed a process* for its separation and use. Fie directs that such substances as resins, balsams, oleoresins, etc., should be first dissolved in a small amount of alcohol. Then for a 100 Cc. mixture, about 8.5 Gm. of saccharated casein, dissolved in an equal weight of water, is added, * Lexer’s process is briefly as follows: To 4 liters of milk add 60 Cc. of ammonia water (Ph. Fr., 20 per cent.), shake well, and set aside for twenty-four hours. It will then have separated into two layers, the semi-saponified fat above, and the lacto-serum below. Draw off the lower layer, precipi- tate the casein by acetic acid, collect the magma on a strainer, and express the liquid. Remove the casein from the strainer, mix it with 10 Gm. of sodium bicarbonate by thorough trituration, and finally add enough sugar to obtain a powder containing, when dry, about 10 per cent, of its weight of casein. 300 HANDBOOK OF PHARMACY. the mixture thoroughly shaken, after which the remaining con- stituents are added in their proper order with continual shaking. For emulsifying the oils the manipulations are the same as with acacia. It is claimed for this emulsifying agent that it yields perfect and stable emulsions, which are very palatable and easily tolerated by the most delicate stomach, which cannot be said of gum-arabic emulsions. Pancreatin, a mixture of natural ferments, forms an excellent emulsifying agent when employed in an alkaline medium (as sodium bicarbonate). The emulsions obtained by means of it are rarely permanent, but are often preferred, because of their easy assimilation, for the administration of such fats as cod-liver oil to consumptives. Pancreatin is often added to emulsions to assist the thorough emulsification of the fats or oils. It should be mixed with an equal bulk of sodium bicarbonate and dissolved in a small quantity of water; to this is then added the oil or emulsion gradually, the mixture being well shaken after each addition. Gelatin has been proposed (patented) for emulsifying paraffin oils. The patent directs that in 12 parts of a solution of gelatin (4 ounces to the gallon of water), 1 part of phosphate or carbonate of sodium or potassium is to be dissolved. This mixture is capable of emulsifying from 24 to 36 parts of animal or vegetable oils. For emulsifying mineral oils, the alkali is replaced by soft soap. Salol is melted in a warm mortar and emulsified with powdered acacia, according to the continental method, warm water being employed. On standing, it separates as a fine powder, which is easily reincorporated by agitation. Jouisse’s formula is as follows: Salol and pulverized acacia, each, 4 Gm., tragacanth 0.2 Gm., tincture of tolu 10 Gm., syrup 30 Gm., water, sufficient quantity. The tincture of tolu is added to the water, the mixture strained, and the emulsion made as above directed. Resins or Resinous Substances (Guaiac, Jalap, Turpentine, etc.) should, if possible, be reduced to a powder and rubbed with one- half their weight of pulverized acacia, with gradual addition of water; or they may be dissolved in a little alcohol and emulsified with yolk of egg, mucilage of chondrus (Irish moss), or traga- canth. Camphor should be first pulverized by the aid of a little alcohol or ether, then mixed with ten times its weight of gum arabic or with yolk of egg. EMULSIFICATION OF SPECIAL DRUGS. MIXTURES. 301 Waxes (Spermaceti, Cacao Butter, etc.) are emulsified like the fixed oils, the fat being first melted, then poured into a hot mor- tar (the pestle being also heated). An equal weight of pulverized acacia is added and the whole thoroughly triturated, then hot water (1| times as much as there is of fat) is gradually added under constant stirring. Lycopodium, or Lupulin.—These are rubbed in a mortar with a little water until a crumbly mass is obtained, then triturated with an equal weight of acacia, and the water gradually added with trituration. Balsam Peru.—This may be emulsionized with yolk of egg or acacia. Of the latter, a quantity is taken equal in weight to the amount of balsam used. Pressure should not be used in preparing emulsions—it is the triturating (agitating) motion that is desired. The motion should be rapid and light. Over-manipulation often causes “ cracking.” A rather deep mortar with shallow bottom should be selected for this purpose. Emulsions of fixed oils should be made with the mortar and pestle, while volatile oils are best emulsified by agitation in a flask or bottle. When small amounts of oils (croton, cubebs, etc.) or volatile fluids (chloroform, etc.) are to be emulsified, it is best to mix them first with a little olive or almond oil, which assists in the suspen- sion and imparts a creamy finish to the emulsion. Alkalies (solution of potassa, solution of lime, borax, etc.) favor the emulsification of fixed oils, but they should never be used, since a combination with the fat-acids takes place with the forma- tion of soap, resulting in the impairment of the therapeutic properties of the oil. The addition of acids, acid solutions, acid salts, glycerin, alcohol, or alcoholic liquids, generally destroys gum emulsions, chiefly owing to the gum being thrown out of solution. The addition of glycerin, alcohol, or large amounts of salts act physically in abstracting water, thereby rendering the emulsionizing agent less viscid. The addition of borax or tincture of iron will cause an acacia emulsion to become gelatinous on standing. When any of the above incompatibles are ordered in small quantity in an emulsion, they should be added last, in diluted condition, and in small portions at a time, the whole being shaken after each addition. When the amount ordered is large enough to destroy a gum emulsion, recourse may be had to yolk of egg, Irish moss mucilage, or tincture of quillaja. NOTES. 302 HANDBOOK OF PHARMACY. The Pharmacopoeia recognizes 4 emulsions: EMULSA, U. S. P. Title. Constituents. Class. Properties. Dose. Emulsum Ammoniaci, Ammoniac, 40 Gm. Water, a sufficient quan- tity to make 1000 Cc. Gum-resin Emulsion. Expectorant, 15-30 Cc. Emulsum Asafcetidae, Asafoetida, 40 Gm. Water, a sufficient quan- tity to make 1000 Cc. Gum-resin Emulsion. Antispasmodic, 15-30 Cc. Sweet Almond, 60 Gm. Emulsum Amygdalae, Acacia p., 10 Gm. Sugar, 30 Gm. Water, a sufficient quan- tity to make 1000 Cc. Seed Emulsion. Demulcent, 60-200 Cc. Chloroform, 40 Cc. Expressed Oil of Al- Emulsum Chloroform i, mond, 60 Cc. Tragacanth, Powdered, 15 Gm. Water, a sufficient quan- tity to make 1000 Cc. Oil Emulsion. Anodyne, 15-20 Cc. CHAPTER XXXIV. SOLIDS. I. FOR INTERNAL USE. PUL VERES—(Powders). Substances which are in a finely subdivided condition are known as powders. Of these we recognize different degrees of fineness; but the official powders are of the finest degree of subdivision. According to the use for which they are intended they may be divided into two classes:— 1st. Those for External Use. 2d. Those for Internal Use. Such powders as are intended for external use, as for dusting* over in- jured or inflamed surfaces, or for insufflation in the treatment of throat affections, or for blowing into the ear or nostrils, should not be mixed by trituration, as this renders them too compact, depriv- ing them of their necessary lightness. When more than one constituent enters into such a powder, they should, if possible, be separately reduced to a very fine powder, then sifted and mixed with a spatula. Such powders should be dispensed in dry vials. Powders intended for internal use may be mixed or triturated in a mortar, as lightness is not the essential feature demanded. Compound powders, whether they contain potent drugs or not, should be thoroughly and uniformly mixed, for the value of the constituents, and frequently the life of the patient, depends on this precaution. When such substances as extracts, oils, liquids or hygroscopic salts, such as potassium acetate or citrate, are to be combined into a powder, these should be first triturated with some dry, absorbent powder, then combined with the balance of the ingredients. Powders which contain hygroscopic substances should not be kept in stock, and when dispensed should be enclosed in waxed paper (paraffin paper). Powders containing volatile substances, such as camphor, am- monium carbonate, etc., should likewise be dispensed in waxed paper. In some instances a chemical reaction! is liable to take place, for instance, in mixtures containing potassium chlorate or hypo- phosphite, and organic substances, such as tannic acid, sulphur, etc. In such cases the powders, separately dried, should be cautiously mixed on smooth paper by the aid of a horn or wooden spatula without friction. In other instances, certain chemicals, * Examples:— Ijt. Lycopodii, 90.0 Jfc. Bismuthi Subearbonatis, 0.008 Acidi Salicylici, 1.0 Pulv. Catechu, 0.005 Rhizomatis Iridis, 9.0 Morphinee Sulphatis, 0.004 II. lodoformi, 10.0 Cumarini, 0.05 f See Incompatibles. 303 304 HANDBOOK OF PHARMACY. when triturated together, liquefy* These should be pulverized separately and then mixed without pressure and dispensed in waxed papers; many of these combinations cannot be dispensed at all without liquefaction; hence the several ingredients should be dis- pensed separately, Dividing.—It is the habit of many pharmacists to divide all powders by hand, collecting the powder and flattening it out to a rectangular shape, then dividing into the necessary number of equal portions by means of a spatula. This habit of guesswork should not be permitted, particu- larly if the powder contains a potent drug. In all cases, where the powder contains an active drug, each portion should be weighed. In those instances in which the powder is of a harmless nature, accuracy of division may be assisted by mechanical devices. Fig. 330 illustrates a cup-shaped device, made of hard wood, which is intended for measuring out certain quantities of powders. It is particularly adapted for measuring Seidlitz mixture. A very convenient device is shown in Fig. 331. This consists of a trough nine inches long, one inch wide, and three-eighths inch deep, closed at one end, and graduated inside. This, together with the leveler and spatula, is made of brass and nickel-plated, the spatula having an ebonized wood handle. The powder is placed in the graduated trough, and the rubber plug placed opposite the graduation denoting the number of powders into which the prescription is to be divided. The powder is then leveled in the trough by means of the leveler, after which the plug is removed, and by use of the spatula in connection with the graduation marks, the powder is accurately divided into the necessary number of parts, each of which is then removed through the open end of the trough. The paper selected for wrapping powders should be of good quality, with a well-calendered or glazed surface. After the required number of powder-papers have been laid out in rows, they should be creased by folding down a narrow margin along one of the longer sides; then after the powder has been distributed upon the several papers, the edge is folded over so as to correspond exactly to the line of the crease; the folded edge is then picked up and turned back toward the operator to such an extent, that a package of a definite and uniform Fig. 330. Seidlitz Powder Measure. Fig. 331. Diamond Powder Divider. * For example Chloral and Camphor, Acetate of Lead and Zinc Sulphate, Antipyrin with Chloral, Naphthol, Piperazin, Sodium Salicylate, etc. SOLIDS—.FOR INTERNAL USE. 305 width results. Then the ends of the powder are folded over by means of a spatula, the length being regulated to suit the size of the box in which they are to be placed. In order to secure uniformity in length, the powder-folder may be employed (Figs. 332-4). This is usually constructed so that various lengths may be accurately adjusted. Nauseous powders are often administered in wafers. These consist of thin brittle sheets (square or circular pieces), made by pouring a mixture of flour and water on hot plates. When used, one of these is first dipped into cold water to render it limp. It is then quickly laid upon a tablespoon ; the powder is emptied into the center, then the edges are folded over so as to enclose it securely on all sides, water is then poured into the spoon and the whole is swallowed without the least difficulty. An improvement on this is the “ cachet.” These are concave discs of wafer, made by dampening and pressing wafer-paper (small discs) between warm moulds. The powder is placed inside, then an empty disc, with its edges moistened, is placed over it and sealed by sufficient pressure. These are dipped into cold water, and swallowed with a draught of cold water. Figs. 332, 333, 334. Powder Folders. Various forms of elaborate apparatus have been devised for sealing these. Among the simpler ones is the apparatus shown in Fig. 335. The nickel-plated mould (a) is so constructed as to hold any size of cachet. One of the halves is placed in the mould, then over the top is placed the “ filler ” (5) to ensure the even filling of the cachet without spilling any of the powder over the edges. Then by means of the holder (c) the empty half is picked up, moistened on a piece of wet felt, and, by pressing, joined to the lower half; an automatic spring enables the opera- tor to loosen the sealed cachet. Fig. 336 illustrates another form in which the cachets are pressed into the circular spaces of plates a and b, then plate c is folded over on to plate b, and, by means of a short funnel, the powders are rapidly deposited in the center of the lower cachets, and if necessary, pressed down and made compact by means of a plunger. When filled, plate c is removed from plate b, then a damping roller is passed over plate a, the edges of the covers being moistened; this is now closed over b with slight pressure, 306 HANDBOOK OF PHARMACY. which seals the cachets, leaving them adhering to the plate a, when opened. A very convenient substitute for the wafers is the Japanese Fig. 335. Apparatus for Filling and Sealing Cachets (Chapereau). Usego paper. This is thin and strong, the powder is laid in the center of a small disc, the ends are gathered and twisted so as to Fig. 336. Cachet Filling and Sealing Apparatus (Konseal). form a small cylindrical package, which is then dipped in water and swallowed. The paper is digested with the medicine. SOLIDS—.FOR INTERNAL USE. 307 GELATIN CAPSULES. The gelatin capsule affords a convenient method of administer- ing nauseous powders and liquids. Capsules are designated as hard and soft. They are made by dipping smooth olive-shaped moulds into a hot solution of gelatin,* allowing the coating to set and then removing. The moulds consist of olive-shaped solid heads (c) of polished bone, ivory, or metal, fixed upon rods (6) of wood, or metal, which are placed upright in perforations in a slab of wood (Fig. 337), in the back of which a handle is fixed. The moulds (olives) with the neck of the supporting rod are slightly oiled by means of a piece of cloth, secured in the base, then the frame is grasped by the handle, and the tips immersed a few seconds in the gelatin solution, which is kept at a uniform temperature (about 40° C.). On removing the moulds, the excess of solution is allowed to run off, then the moulds are rotated so as to distribute the film evenly on all sides; as soon as the mass has set sufficiently, they are put aside until cold and firm enough for removal. A knife is passed round the shank of the mould, close to the bulb, so as to separate that portion adhering to the handle. Then, by grasping the capsule lightly between two fingers it is gently removed, and placed in supports (d) for drying. The soft capsules are filled by means of a syringe with a long- pointed tip, or by means of a pipette. Care must be taken that no fluid of an oily nature be allowed to drop on the upper edge of the capsule. Then by means of a camel’s-hair brush, or glass rod, the open end of the capsule is sealed over with a portion of the melted composition. These soft gelatin capsules are useful for the administration of such liquids as Terebene, Oil of Tur- pentine, Creosote, Apiol, etc.; they are made of various shapes, as ovoid, globular—flattened, round. The small, round (hard) capsules are known as gelatin “ pearls.” Elastic, or soft, empty capsules! can be obtained in the market, being ovoid in shape, elastic, and filled with air. They are placed Fig. 337. Capsule Moulds. Hard Capsules. Soft Capsules. * Gelatin, .... 6 pts., . ... 25 pts. Acacia, .... 1 pt., .... Glycerin, . . ... 10 pts. P. Sugar, .... 1 pt., . . . . 8 pts. Water, . . . . 5 pts., . ... 45 pts. Steep the gelatin in water, when soft add the gum and sugar, and heat in a covered vessel on a water-bath until dissolved. t Made by the Merz Soft Capsule Co., Detroit, Michigan. 308 HANDBOOK OF PHARMACY. on a stick perforated with holes, the elongated tops removed with a scissors, then filled with a pipette, or syringe, and sealed. The empty, hard gelatin capsules, Fig. 340, are of cylindrical shape, their capacity being indicated by various numbers. They should be filled with the powder in dry condition and not in mass form. They may be filled by grasping the longer half between the fingers, and by pressing downward with a slight rotary motion over the powder; for this purpose the powder Fig. 339. Elastic Gelatin Capsules. Fig. 340. Gelatin Capsules (Empty). should be heaped; after the capsules are filled, the tops are slid over as far as possible. Care should be taken to keep the fingers dry and clean, and after filling, to carefully wipe any adhering powder from the surface of the capsule. It is, however, preferable to employ the capsule filler, which is far more cleanly and accurate. There are several forms of these in the market, among which the following may be recommended for their sim- plicity :— The Davenport Capsule Filler, Fig. 341, consists of a funnel of light metal (plated) with a very wide rim, flattened on one side, the tube of which is short and of a size adapted to fit the size of capsule for which it is intended. A plunger is provided for the purpose of forcing the powder com- pactly into the capsule. Globular and Ovoid Gelatin Capsules. Fig. 341. Davenport Capsule Filler. SOLIDS—FOR INTERNAL USE. 309 The Raymond Capsule Filler, Fig. 342, consists of two blocks of hard wood, in the lower one of which sockets are bored sufficiently Fig. 342. Raymond Capsule Filler. Fig. 343. Acme Capsule Filler. deep to accommodate the capsules to one-half of their length. The upper block is pierced with corresponding funnel-shaped holes; 310 HANDBOOK OF PHARMACY. this, when placed over the lower block, encloses the capsules securely. The powders are emptied into the funnel-shaped aper- tures and forced down by means of a wooden plunger. The upper block is then removed and the tops of the capsules slid over the filled, lower portions. The Acme Capsule Filler, Fig. 343, consists of a block of wood, with perforations for holding a dozen capsules. This block slides back and forward in a metallic case, on one end of whose upper side is placed a funnel, through which, by means of a plunger, the powder is readily introduced into the capsules. The U. S. Pharmacopoeia recognizes 9 compound powders. PULVERES, U. S. P. Title. Constituents. Properties. Dose. PULVIS Antimonialis, .... Antimony Oxide, 33 Gm. Ppt. Calcium Phosph., 67 Gm. Diaphoretic, Emetic, 0.2-0.5Gm. Aromaticus, P. Cinnamon, 35 Gm.; P. Ginger, 35 Gm.; P. Carda- mom, 15 Gm.; P. Nutmeg, 15 Gm. Aromatic. Crete Compositus, . Prep. Chalk, 30 Gm.; Acacia, 20 Gm.; Sugar, 50 Gm. Chalk Mixture. Effervescens Compositus (Seidlitz Powder), . Sodium Bicarb., 31 Gm.; Ro- chelle Salt, 93 Gm.; Tartaric Acid, 27 Gm. Laxative. Glycyrrhiz® Compositus, P. Senna, 180 Gm.; P. Liquor- ice, 236 Gm.; Washed Sul- phur, 80 Gm.; Oil Fennel, 4 Gm.; Sugar, 500 Gm. Laxative, 2-8 Gm. Ipecacuanhas et Opii (Dover’s Powder), P. Ipecac, 10 Gm.; P. Opium, 10 Gm.; Sugar of Milk, 80 Gm. Diaphoretic, 0.3-1 Gm. Jalapae Compositus, . . P. Jalap, 35 Gm.; Potass. Bitart.,65 Gm. Cathartic, 1-4 Gm. Morphinae Compositus (Tully’s Powder), . , Morphia Sulphate, 1 Gm.; P. Camphor, 19 Gm.; P. Li- quorice, 20 Gm.; Ppt. Calc. Carb., 20 Gm. Diaphoretic, 0.3-0.9 Gm. Rhei Compositus, . . . P. Rhubarb, 25 Gm.; Magne- sia, 65 Gm.; P. Ginger, 10 Gm. Laxative, Antacid, 0.3-12 Gm. These are a class of powders which contain active substances in a minute state of subdivision, obtained by trituration with sugar of milk. By means of these we can accurately regulate the doses of powerful substances. In the preparation of these powders it is advisable to employ the sugar of milk in small crystals or coarse powder, so that TRITURATIONES—{Triturations). SOLIDS—FOR INTERNAL USE. 311 during the process of trituration, which is necessary to bring it to a fine powder, the medicinal ingredient may at the same time receive thorough and uniform subdivision. The following general formula is given by the U. S. Pharma- copoeia :— “ Unless otherwise directed, Triturations are to be prepared by the following formula:— Take of The Substance, ten grammes, 10 Gm. Sugar of Milk, in moderately fine powder, ninety grammes . 90 Gm. To make one hundred grammes, . . 100 Gm. Weigh the substance and the sugar of milk separately; then place the substance, previously reduced, if necessary, to a moder- ately fine powder, in a mortar; add about an equal measure of sugar of milk, mix well by means of a spatula, and triturate them thoroughly together. Then add fresh portions of the sugar of milk, from time to time, until the whole is added, and continue the trituration until the substance is intimately mixed with the sugar of milk and reduced to a fine powder. TRITURATIO ELATERINI (Trituration of Elaterin). Elaterin, ten grammes, 10 Gm. Sugar of Milk, in moderately fine powder, ninety grammes, . 90 Gm. To make one hundred grammes, . . 100 Gm. Mix them thoroughly by trituration.” EL2EOSACCHARA—OLEOSACCHARA (N.F.)—(Oleosaccharates). Oleosaccharates, or oil-sugars consist of sugar flavored with volatile oil or some other volatile aromatic substance. The German Pharmacopoeia directs that 1 gramme of volatile oil be added to 50 grammes of sugar in moderately fine powder, and the mixture thoroughly triturated. In France, oleosac- charates are made double this strength. The oleosaccharate of vanilla is prepared from 1 part of finely cut vanilla and 9 parts of crystallized sugar (rock candy), triturated until a fine powder results; in place of the vanilla bean, a mixture of vanillin and cumarin is often employed. Under the title of Oleosacchara, the National Formulary directs the following general formula: Volatile Oil, 1 drop. Sugar, 30 grains. Triturate the sugar with the volatile oil to a fine powder. The oleosaccharates are intended as a pleasant aromatic vehicle for administering medicinal substances in powder form. Those pre- pared from volatile oils should be freshly made when wanted for use. Only the best quality* of fresh volatile oil should be employed. * Old resinified oils impart a bitter, unpleasant taste, as well as terebinthinate odor, to the sugar. 312 HANDBOOK OF PHARMACY. MASSES RESULTING FROM ADMIXTURE OF POWDERS WITH FLUIDS. CONFECTIONES—(Confections). Confections (conficio = to make up) are soft masses resulting from the admixture of one or more medicinal substances with sugar. They are usually prepared by incorporating the drug or drugs in paste or powder form with some saccharine liquid. This is a very ancient method of administering medicines, but it has almost gone out of use at present. The Conserve (conserve = to keep) differs from the above in that sugar is added to the fresh drug beaten to a pulp, in sufficient quantity to form a soft mass; the sugar serving as a preservative agent as well as a vehicle. The Electuary* is a mixture of powders with pulps, syrup, or honey. It is of a softer consistence than the confections as under- stood by the Pharmacopoeia. But it should not be too soft, so as to deposit the ingredients on standing. Confections, when they have become hard from drying out, may be restored to a pulpy condition by working them over with a little glycerin. The U. S. Pharmacopoeia recognizes Confectio Rosae, which is employed as a vehicle for massing pills and administering other remedies, and Confectio Sennae, which is employed as a cathartic. Red Rose, powdered, 80 Gm. Sugar, powdered, 640 “ Clarified Honey, 120 “ Stronger Rose Water, 160 Cc. Confectio Ros®. Senna, powdered, 100 Gm. Cassia Fistula, 160 “ Tamarind, 100 “ Prune, 70 “ Fig, 120 “ Sugar, 555 “ Oil of Coriander, 5 “ Confectio Sennae. Water, sufficient to make 1000 Gm. The U. S. Pharmacopoeia recognizes three pill masses. They are permanent preparations and are conveniently kept in stock. MASSjE. Massa Copaibas. (Dose 0.5 to 2 Gm.) Copaiba, 94 Gm. Magnesia, 6 “ Water, a sufficient quantity. On mixing copaiba with magnesia it gradually loses its fluidity, * Having as base, honey or syrup, pulp of prunes or tamarinds. The German Pharmacopoeia directs the following proportions to be observed:— For 1 part of powd. drug, 3 to 5 p. of Honey or Syrup. “1 “ “ “ 4 to 6 p. Prune or Tamarind Pulp. “ 1 “ difficultly soluble salt,... 1 p. of Syrup. “ 1 “ “ “ “ . . . 2 p. of Pulp. SOLIDS— FOR INTERNAL USE. 313 and finally becomes hard and brittle. This is due to the chemical combination of the magnesia with the copaibic acid (hard resin). The length of time required for this combination to take place varies with the condition of the copaiba. For this combination of the copaibic acid and magnesia it is essential that a certain amount of water be present. As there is rarely sufficient in the magnesia, it is generally added. Ferrous Sulphate, 100 Gm. Sodium Carbonate, 100 “ Clarified Honey, 38 “ Sugar, 25 “ Syrup and Water, of each, sufficient to make 1000 Gm. Massa Ferri Carbonatis (Vallet’s Mass). (Dose 0.2 to 0.5 Gm.) Syrup is added to the ferrous sulphate solution and the wash water, to protect the ferrous salt against the absorption of oxygen. Boiling distilled water is employed to avoid the oxidizing action of the air, which is contained in the unboiled water. The reaction which takes place between the ferrous sulphate and sodium carbonate, results in the formation of the greenish-gray colored ferrous carbonate (FeCO3). This readily undergoes oxida- tion ; hence it is necessary to carry on the washing as rapidly as possible, and to protect the ferrous carbonate by employing boiled water and syrup. The product is finally made into a mass with honey and sugar. This contains 42 per cent, of Ferrous Carbon- ate, and is probably the most efficient form for the administration of iron. Mercury, 33 Gm. Glycyrrhiza, powdered, 5 “ Althaea, powdered, 25 “ Glycerin, 3 “ Honey of Rose, 34 “ 100 Gm. Massa Hydrargyri (Blue Mass or Pill). (Dose: 0.2 to 0.5 Gm.) This contains one-third of its weight of mercury. The mass can be prepared on a small scale by the pharmacist, but care must be taken that the extinguishment of the mercury is carried on until the globules are no longer visible through a lens mag- nifying at least ten diameters. Among the various agents that may be employed for the extinguishment of the mercury in this instance, the Confection of Rose is one of the best, as it is not only effective, but also protects the mercury quite well from oxida- tion. However, upon long standing, both mercurous and mer- curic oxide are apt to form, owing to the slow oxidation of the finely subdivided mercury. As these are toxic when present in any quantity, it is necessary that the sample be tested for their presence as directed by the Pharmacopoeia. 314 HANDBOOK OF PHARMACY. TROCHISCI—( Troches). TABELL2E—PASTILLI. Troches (lozenges) are round or oval, solid, flattened masses, consisting of medicinal substances combined with sugar and mucilage. They represent a convenient form of administering such remedies as are intended to act by continual application, through slow disintegration, on the throat. Troches generally vary in weight from one-half to one gramme. According to their method of preparation, they may be divided into two classes. 1st. Those made by compression. In this case the medicinal constituents are mixed with powdered sugar, then moistened with some kind of mucilage, granulated and compressed into tablet form, as described under compressed tablets (page 335). Fig. 344. Troches (various forms'. 2d. Those made by moulding. A mass is prepared, and after rolling it out to the desired thickness, the lozenges are cut out by means of moulds, or the mass is made into pills and reduced to the desired size and shape by compression. In preparing a mass, the one or more medicinal constituents, in a finely powdered condition, are thoroughly mixed with a finely powdered diluent (sugar),* then made into a mass by the careful addition of mucilage of tragacanth. In some instances the Phar- macopoeia directs the use of powdered tragacanth, and that the mass be made up by the addition of water. Great care must be exercised when proceeding by the latter method, to add the water cautiously, while the mass is being thoroughly worked, otherwise it is likely to become too soft for moulding. * Confectioners’ sugar. SOLIDS—.FOR INTERNAL USE. 315 The manufacturer employs machinery for kneading the masses, while the apothecary relies upon the mortar and pestle. For this purpose the pill-pestle, as shown in Fig. 351, is best adapted. After the mass has been prepared, which should be of a consist- ence slightly softer than that of a pill-mass, it is rolled out upon a lozenge-board (Fig. 345), the thickness of the mass being made uniform, and regulated by a frame along the sides of the board upon which the ends of the roller rest. The surface of the mass is dusted with a mixture of powdered sugar and starch, and then divided into lozenges by means of a punch. These punches are made of various sizes and shapes, to suit the taste of the operator. They may consist of a hollow cylinder of tin or steel, or more elaborately constructed, as shown in the form illustrated in Fig. 346. This consists of a hollow cylinder, inside of which, by means of the handle, g i, the plunger, d, is operated ; the screw, a, Fig. 345. Rolling out Mass for Troches. regulates the distance to which the plunger may recede, thereby controlling the thickness of the lozenge. This plunger, d, may consist of a die which stamps a letter or design on the lozenge in the operation of cutting; on pressing the arm, g, at i, the rod at d is forced downward and discharges the lozenge. After being moulded or cut, the lozenges are placed on trays and allowed to dry in a moderately heated drying room. In the absence of a lozenge punch, the mass may be rolled out into a cylinder, cut and formed into pills, which, when pressed with a spatula, may be made to yield a lozenge of any desired thickness, the edges of which may be rounded by rotating between the blades of two spatulas. Should the edges of a 316 HANDBOOK OF PHARMACY. lozenge, thus made, become ragged or crack, this generally indicates that the mass is too dry. It should then be returned to the mortar and worked over with the addition of a little tragacanth mucilage. Aside from sugar and tragacanth, extract of liquorice is often employed as a base. This can be medicated as desired, and owing Fig. 346. Troche Cutter. to its plasticity, can be readily formed into a variety of shapes, as shown in Figs. 347,348. When the mass is rolled out into a thin cylindrical rod (3 to 4 Mm. diameter) and cut into pieces of about 10 to 12 Mm. in length, these little cylinders are designated “ bacilli ” or “ sticklets.” Fig. 348. Fig. 347. Ovoids. Mouth Pastilles. The following mixture may also be employed as a base; 1 part of chocolate (grated), 2 parts of powdered sugar, and 0.05 parts (for 30 Gm. of mass 0.5 Gm.) of powdered tragacanth. Currant paste is also employed as a basis for this purpose. SOLIDS—FOR INTERNAL USE. 317 The U. S. Pharmacopoeia recognizes 15 formulas for troches. Title. Constituents—100 Troches. Active Constituent, to each Trochisci troche. Acidi Tannici, .... Tannic Acid, 6 Gm.; Sugar, powd., 65 Gm.; Tragacanth, powd., 2 Gm. ; Stronger Orange Flower Water, a sufficient quantity. Tannic Acid, 0.06 Gm. Ammonii Chloridi, . . Ammonium Chloride, 10 Gm.; Extractof Liquorice,25Gm.; Tragacanth, powd., 2 Gm.; Sugar, powd., 50 Gm.;Syrup of Tolu, a sufficient quantity. Ammonium Chloride, 0.1 Gm. Catechu, Catechu, 6 Gm.; Sugar, powd., 65 Gm.; Tragacanth, 2 Gm.; Stronger Orange Flower Water, a sufficient quantity. Catechu, 0.06 Gm. Cretae, Prepared Chalk, 25 Gm.; Aca- cia, 7 Gm.; Spirit of Nut- meg. 3 Cc.; Sugar, powd., 40 Gm.; Water, a sufficient quantity. Prepared Chalk, 0.25 Gm. Cubebte, Oleoresin of Cubeb, 4 Gm.; Oil of Sassafras, 1 Cc.; Ex tract of Liquorice, 25 Gm.; Acacia, powd., 12Gm.; Syr- up of Tolu, a sufficient quantity. Oleoresin Cubeb, 0.04 Gm. Ferri, Ferric Hydrate, 30 Gm.; Van- illa, cut, 1 Gm.; Sugar, powd., 100 Gm.; Mucilage of Tragacanth, a sufficient quantity. Ferric Hydrate, 0.3 Gm. Glycyrrhizae et Opii, . . Extract of Liquorice, 15 Gm.; Powd. Opium, 0.5 Gm.: Acacia, powd., 12 Gm.; Sugar, powd., 20 Gm.; Oil of Anise, 0.2 Cc.; Water, a sufficient quantity. P. Opium, 0.005 Gm. Ipecacuanhas, Ipecac., powd., 2 Gm.; Traga- canth, powd., 2 Gm.; Sugar, powd.,65 Gm.; Syrup of Or- ange, a sufficient quantity. Extract of Krameria, 6 Gm.; Sugar, powd., 65 Gm.; Trag- acanth, powd., 2 Gm.; Stronger Orange Flower Water, a sufficient quantity. P. Ipecac, 0.02 Gm Krameriae, Ext. Krameria, 0.06 Gm. Menthae Piperitae, . . . Oil of Peppermint, 1 Cc.; Su- gar, powd., 80 Gm.; Mucil- age of Tragacanth, a suffi- cient quantity. Oil of Peppermint, 0.01 Cc. Morphinae, et Ipecacu- Morphine Sulphate, 0.16 Gm.; Morphine Sulphate, 0.0016 Gm.; P. Ipe- cac, 0.005 Gm. anhae, Ipecac, powd., 0.5 Gm.; Sugar, powd., 65.00 Gm.; Oil of Wintergreen, 0.2 Cc.; Mucilage of Tragacanth, a sufficient quantity. Potassii Chloratis, . . . Potassium Chlorate, 30 Gm.; Sugar, powd., 120 Gm.; Tragacanth, powd., 6 Gm.; Spirit of Lemon, 1 Cc.; Water, a sufficient quantity. Potassium Chlorate, 0.3 Gm. 318 HANDBOOK OF PHARMACY. Title. Constituents—100 Troches. Active Constituent, to each troche. Santonini, Santonin, 3 Gin.; Sugar, powd., 110 Gm.; Traga- canth, powd., 3 Gm., Stronger Orange Flower Water, a sufficient quantity. Santonin, 0.03 Gm. Sodii Bicarbonatis, . . Sodium Bicarbonate, 20 Gm.; Sugar, powd., 60 Gm.; Nutmeg, bruised, 1 Gm.; Mucilage of Tragacanth, a sufficient quantity. Sodium Bicarbonate,0.2 Gm. Zingiberis, Tinct. Ginger, 20 Cc.; Traga- canth, powd., 4 Gm.; Sugar, powd., 130 Gm.; Syrup of Ginger, a sufficient quan- tity. Tincture of Ginger, 0.02 Cc. PILULE—(Pills). Pills are spherical or elongated masses of medicinal substances of such a size as to be convenient for swallowing. The pill forms a very convenient method of administering such substances as are characterized by an unpleasant odor or taste. The weight* of pills varies from 0.1 to 0.3 Gm. for vegetable powders, and up to 0.6 Gm. for inorganic combinations; a pill which is much larger than this is known as a bolus. Very small coated pills are called granules. A piil-mass should be sufficiently plastic to admit moulding, and yet sufficiently firm to enable the pills, when moulded, to retain their shape. To be successful in the preparation of pill-masses, a knowledge of the nature of the substances to be combined is necessary, for, with systematic procedure, the most intractable substances can be managed. Pills should not be made too firm or hard, which would render them insoluble in the stomach, causing thereby nausea and irritation. The pill-mass consists essentially of two parts, viz., the active ingredients, whether solid or liquid, and the excipient, which im- parts the proper degree of consistence and tenacity. Some substances are of such a plastic nature as to render the addition of an excipient unnecessary, as, for instance, the soft extracts; others, like gum-resins or resins, when dry, possess no adhesiveness, yet acquire this property on addition of a little sol- vent, such as alcohol; such powders as extract of liquorice or some of the powdered extracts only require the addition of water to impart adhesiveness; thus, in many instances we develop, and do not impart adhesiveness. When the solid (as camphor, inorganic salts, etc.) does not * The size, as compared to the weight of pills, varies according to the nature of the substance, some being very light and bulky, while others are heavy and compact. SOLIDS—FOR INTERNAL USE. 319 possess adhesiveness, we impart it by the addition of an excipient which has these qualities. Such substances as are in a fluid or semi-fluid condition should be incorporated with inert and absorbent powders, as liquorice root or powdered marshmallow; if the amount of fluid be such as to render the pill too large, it should be first evapor- ated until the residue has the consistence of a soft extract. Pills containing deliquescent substances should be coated im- mediately after their preparation. Inorganic salts which contain water of crystallization should be first dried before being combined into a pill-mass. Powders, when non-adhesive, should be combined with a soft extract or some adhesive excipient; the indiscriminate use of large quantities of powdered acacia or tragacanth is to be con- demned, since they render pills very hard and quite insoluble. When used as excipient they should be combined with a little glycerin. Active or potent substances, such as corrosive sublimate, arsen- ous acid, alkaloids, etc., which are administered in very small doses, should be intimately mixed with some inert powder (sugar of milk, etc.) by trituration, then incorporated into a mass. Care should be taken not to combine substances which react with one another, as, for instance, acid salts and carbonates, silver salts or permanganates with organic matter, etc. The hands and all utensils employed should be kept scrupu- lously clean. The first precaution in making up the pill-mass is to observe that all constituents have been reduced to a very fine powder and thoroughly mixed. Then, if an excipient is necessary, one should be selected which will least increase the size of the pill, and only enough added to yield a uniform and plastic mass. Under all circumstances the mass should be thoroughly worked, so as to secure a perfect and uniform distribution of the medicinal constituents. When the operator is uncertain as to the amount of excipient necessary, it is best to proceed by adding small quantities at a time until the desired degree of plasticity is ob- tained, the mass being rapidly triturated with pressure, the particles of powder that adhere to the sides of the mortar and pestle being detached by means of a spatula. The difficulty with beginners is, that in their haste to obtain a mass, they usually add too much excipient, causing the mass to become soft and pasty. To remedy this, some absorbent powder is generally added, frequently with the result of increasing the size of the pill to that of a bolus. Particular precaution should be observed not to add an excess of water to pill-masses containing soap. For the preparation of a pill-mass a deep wedgwood or porce- lain mortar, of a form similar to that shown in Fig. 349, is prefer- ably selected. Because of their lightness, and the firm grasp 320 HANDBOOK OF PHARMACY. afforded, pestles having a wooden handle are preferred. Fig. 351 illustrates a form specially adapted for this purpose. After the mass has been formed, it should be given a cylindrical shape with the hands, then placed on a pill tile,* (Fig. 350), and by means of the roller (Fig. 352), which is a piece of hard wood with a smooth surface provided with a handle, or by means of a broad-bladed spatula (Fig. 353), it is rolled out into a long cylinder of the necessary length; then by means of a spatula it is divided into the desired number of parts. Many operators prefer to roll and divide the mass on the pill machine (Fig. 354). This consists of two pieces of hard wood; Fig. 349. Fig. 351. Fig. 352. Pill Mortar. Pill Roller (sectional view). Fig. 350. Fig. 353. Pill Tile. Pill Pestle, f Pill Spatula. the lower board (a) is encased with metal strips to prevent warp- ing, and to protect the raised edges from wear; on the upper end is a hemispherically-grooved brass plate. Corresponding to this is a similar plate on the upper board (6), at either end of which are fastened brass guides, so that the cutting edges of the grooved brass plates may accurately correspond in position. This upper board is provided with handles for operating. * These consist of slabs composed of queensware, porcelain or glass, on one side of which a gradu- ated scale is marked ; queensware is objectionable, because of the frequent cracking of the enamel on the surface, which permits the various substances to penetrate, rendering it after a time unfit for dispensing purposes. Glass is open to the objection that in use the surface becomes rough and scratched. Porcelain answers the best. f Made by Messrs. Whitall, Tatum & Co., New York, SOLIDS—FOR INTERNAL USE. 321 The pill-cylinder, as soon as formed, is laid across the grooves of the lower board ; then the upper board, by means of the guides, is brought upon the surface of the mass with a slight downward pressure, and with a backward and forward movement the pill- cylinder is divided into the desired number of pills. Fig. 354. Pill Machine. To facilitate the formation of the cylinders, in the manufacture of large quantities of pills, the pill (or plaster) press of Liebau (Fig. 355) may be employed. The pill-mass is placed in the cylin- drical hopper (5), which is provided with a double hot water jacket (supplied from a), for the purpose of retaining the mass in Fig. 355. Liebau’s Pill or Plaster Press. soft condition ; then by means of a plunger, operated by a screw, the mass is forced through the apertures in the steel block below, forming cylinders of uniform size. To prevent the mass from sticking to the pill tile or roller, it is usually dusted with rice flour; lycopodium is also used for 322 HANDBOOK OF PHARMACY. this purpose, but offers the slight disadvantage of color, and causes the mass to slip about when rolled. After the cylinder has been cut into the necessary number of parts, these are next rounded and finished by rotating them about with slight pressure, on a level, smooth surface, under the pill finisher (Figs. 356-7). This is made of hard wood, and either of a fixed depth of surface or adjust- able. When the mass is of such a nature that it crumbles readily, it Fig. 356. Pill Finisher. Fig. 357. Pill Finisher, is not only permissible, but preferable, to round the pills by roll- ing them with the fingers. EXCIPIENTS (Fluid). Such excipients as are incompatible with the pill-mass are to be avoided, for instance, confection of rose with iron compounds; also those excipients which render pills too hard or too soft, like- wise those which tend to increase their size unduly. Water.—This is employed in all cases where the mass possesses sufficient inherent adhesiveness capable of being developed with water, as, for instance, pills of aloes, asafoetida, opium, compound cathartic pills, etc. Pills made with water are, however, liable to become exceedingly hard on standing; hence, when they are to be made in large quantities, it is advisable to add a small amount of glycerin. Syrup.—This differs from water in being slightly adhesive. Mucilage or Syrup of Acacia.—While either forms a very adhe- sive excipient, they should be avoided, since they render the pills very hard. Glycerin.—This, alone, is a poor excipient, since it is entirely devoid of adhesive properties. It is, however, excellent when used in combination with other excipients (glycerite of tragacanth, etc.), as it will maintain the pills in a soft condition. Owing to its hygroscopic nature, it should be used very cautiously, other- wise the pills soon lose their shape. SOLIDS—FOR INTERNAL USE. 323 Glucose or Honey.—These form excellent excipients, being adhe- sive and tending to retain the mass in soft condition. Glycerite of Tragacanth*—This forms one of the best general excipients for all sorts of masses. It is adhesive, and does not render the pills hygroscopic. Castor Oil.—This is employed as an excipient in pills of cam- phor, also in the official Plummer’s Pill. General Excipient.—A combination of some of the above excip- ients, possessing their several virtues, forms perhaps the best for general use. Upham’s Formula : Powd. Acacia, 1 drachm. Powd. Tragacanth, 2 “ Glucose (white), 5 “ Glycerin, 3 ounces. Mix the powders in a suitable vessel, and incorporate the glycerin and glucose until a perfectly smooth paste is obtained; then apply sufficient heat until the mass thickens. Remington’s Formula : Glucose (white), 4 oz. av. Glycerin, 1 oz. av. Powd. Acacia, 90 grains. Benzoic Acid, 1 grain. In the glycerin contained in a capsule, heated on a water-bath, dissolve the benzoic acid (or better, replace the benzoic acid by 5 drops of Tr. Benzoin); then add the acacia and glucose, and stir well until they are dissolved. EXCIPIENTS (Solid). Acacia (powdered).—Powdered acacia, by itself, is of but little value, but, when combined with powdered althaea (Hager), it binds well, making a mass of good consistence. Tragacanth (powdered).—This imparts solidity and elasticity to a mass, particularly if the latter tends to crumble. If too much is added, the mass becomes so elastic that it is almost impossible to render the pills round by rolling. Sbcp (powdered).—This is adapted to the formation of pill- masses containing resins, gum-resins, and vegetable powders. In the Pharmacopoeia, it is employed in making pills of aloes, aloes and asafoetida, asafoetida, opium and rhubarb. Water should be added very cautiously to these mixtures, otherwise they become too soft. Soap should not be used in masses which contain metallic salts, acid salts, etc. * Glycerite of Tragacanth, N. F.—Tragacanth, pulverized, 2 troy ounces ; glycerin, 12% fluid- ounces ; water, 3 fluidounces. Triturate the tragacanth with the glycerin, add the water (hot) gradu- ally, and continue trituratinguntil a homogeneous paste results. 324 HANDBOOK OF PHARMACY. Althaea (powdered).—This, with a little water, is quite adhesive. When employed as an absorbent it should not be employed in large quantities, since it renders the mass very bulky and elastic. Powdered Extract of Liquorice.—This forms, with water, an ex- cellent binding material for all sorts of combinations. It should be employed only in masses of dark color. Pilular Extracts.—Such solid extracts, of pilular consistency, as those of Gentian, Taraxacum or Triticum, form a very useful excipient for a great variety of combinations. It should be borne in mind that they should only be employed in masses which are themselves of a dark color. Confection of Rose.—This is useful for combining small amounts of active drugs, but is objectionable because of its bulk. The Pharmacopoeia directs its use in Pills of Aloes and Myrrh. Petrolatum.—This, in conjunction with kaolin as diluent, forms the best excipient for pills containing readily oxidizable sub- stances, such as silver nitrate, potassium permanganate, etc. Suet (Mutton-tallow, benzoinated).—This, with one-third of its weight of white wax, forms the base of all pills which are to be coated with keratin. If the physician directs some particular excipient, this should be employed, if possible; but, if it be not practicable, the dispenser should follow his own judgment. The selection of excipients should be left to the dispenser, as his practical knowledge enables him better to determine this. MASSING* OF VARIOUS MIXTURES. INORGANIC SALTS. Crystalline salts which are soluble in water, should be finely pulverized and made into a mass with glycerite of tragacanth and a little inert powder, and the pills, when completed, should be varnished with tolu. For making the mass, Canada balsam has been recommended; also, a mixture of the salt (2 parts), powdered soap (1.5 parts), cacao butter (1 part), and petrolatum sufficient; also, a mixture of pulverized liquorice root and glucose; also, after dissolving the salt in the smallest quantity of water, to add enough powdered acacia to form a mucilage, then to add sufficient kaolin to form a mass of proper consistence, which is then to be rolled into pills and varnished. Such compounds as iodide or bromide of iron, are mixed with powdered marshmallow or liquorice root and powdered acacia, and massed with glycerite of tragacanth. * By “ massing ” is meant the conversion of powders or other substances, by means of an excipient, into a plastic condition, suitable for moulding into pills. SOLIDS—FOR INTERNAL USE. 325 Exsiccated iron sulphate is usually directed to be combined with vegetable extracts; here a little glycerite of tragacanth should be added in order to prevent the pills from drying out and cracking. Reduced iron may be mixed with a little liquorice and massed with glycerite of tragacanth. When combined with vegetable extracts containing acids (such as citric, tartaric, malic, etc.), the pills soon swell and fall to pieces, owing to the evolution of hy- drogen arising from the action of the acids on the iron. Sensitive salts, such as silver nitrate, potassium permanganate, or gold chloride, require an inorganic basis, because the use of any organic substance, even though it be merely a dusting powder, will cause the reduction of these salts when coming in contact with them. For this purpose an inorganic substance, such as kaolin or infusorial earth, is employed as diluent, the mixture is made into a mass with petrolatum, and the finished pills rolled in powdered French chalk. Another base, consisting of a mix- ture of anhydrous sodium sulphate 1 part, kaolin 2 parts, and water 1 part, has also been recommended. Alkaloids or potent remedies, which are given in very small doses, should be well triturated with a little sugar of milk and powdered marshmallow or liquorice root, then made into a mass with glucose or glycerite of tragacanth. This procedure answers also, for such inorganic potent remedies as arsenous acid, corrosive sublimate, etc. Quinine Sulphate is best massed quickly and rolled out after moistening with a little dilute sulphuric acid. Some employ strong sulphuric acid; but this must be operated rapidly, other- wise the mass loses its plasticity. Another method (Kurssteiner’s) is to mix intimately 5 parts of quinine sulphate, and 1 part each of citric acid, powdered tragacanth, and sugar of milk, then to mass with syrup. Non-adhesive Bodies, such as acetanilid, naphthol, camphor, etc., should be beaten up with one-third of their weight of pow- dered acacia and massed with glycerite of tragacanth or glucose; or 1 part of powdered tragacanth should be mixed with 5 parts of the substance, and the mixture massed with a drop or so of water. Benzoic and Gallic Acids make a fair mass with glycerin or Canada balsam. Croton Chloral or the Valerianates, and very deliquescent salts, should be mixed with a little inert powder, and made into a mass with glycerite of tragacanth. ORGANIC SALTS. 326 HANDBOOK OF PHARMACY. Creosote or Carbolic Acid.—It has been recommended to use pulverized animal charcoal as absorbent and to mass with turpen- tine or Canada balsam. For each minim of either of the above, a mixture of powdered soap (1 part), and powdered liquorice root (5 parts) has also been recommended. Infusorial eartli may also be employed as the absorbent. Another method consists in pre- paring a 50 per cent, jelly, made by melting together gelatin 11 parts, water 24 parts, sugar 5 parts, to which is added creosote 40 parts. This is to be mixed in a slightly warmed mortar with a small quantity of a vegetable powder, and massed. The German Unofficial Formulary directs Creosote 10 parts, Glycerin 2 parts, Ext. Liquorice powd. 10 parts, powd. Liquorice Root 18 parts. The main difficulty experienced with these pills is that most ab- sorbents fail to retain the oily material, but allow it to penetrate to the surface where it is absorbed by the dusting powder or the pill- box. Volatile Oils and Balsams.—Some absorbent powder should be used in connection with a little soap. What has been said of Creosote applies also to the volatile oils. Hager recommends the addition of one-third to an equal weight of yellow wax * (melted); but this should never be done except as a last resort. Resins and Gum Resins.—These should be finely pulverized, and mixed with a little soap, then made into a mass with a few drops of alcohol. When pulverized they may be made into a mass with a little potassium carbonate. Lupulin triturated with ether gives a good mass. Vegetable Powders.—These require adhesive excipients, such as glycerite of tragacanth, or glucose. . Where admissible, certain extracts, for instance those of taraxacum, or gentian, may also be used. Solid Extracts.—These, when hard or in dry powder, should be made up with water, or syrup, a trace of glycerin being added to prevent undue hardening of the pills. When pills are dispensed, they should be strewn with some absorbent inert powder, usually lycopodium, or starch, or in those cases in which an organic powder is not admissible, with powdered French chalk. It is not customary to use more of the dusting powder than necessary to cover the bottom of the box. COATING PILLS. Pills are coated for the purpose of masking their taste or odor, and for the purpose of adding to their permanency. * It is not advisable to make a practice of employing wax in making pills, as they are likely to pass the body in an unaltered state, or to remain a long time in the intestines. Wax contains very little that is soluble in the gastric juice or intestinal fluids, and, besides, its melting point (above 63° C.) is too high, as the temperature of the body is only 37° C. SOLIDS—FOR INTERNAL USE. 327 Silvering and Gilding.—The coating of pills with silver or gold leaf has become somewhat antiquated. Indeed, it is quite rare, at the present time, that the apothecary is required to per- form this. Pills which contain sulphur, or sulphur compounds, should be first varnished with tolu, so as to prevent blackening of the leaf. The pills which should be free from dusting powder and quite hard, are placed in the hollow cylindrical silvering cup (Fig. 358), then moistened with mucilage of acacia (1 drop for a dozen pills), and rotated so as to distribute this evenly over their surfaces. Then the necessary number of gold or silver leaves are added (one for about 6 pills) and the box is shaken with a rotary motion until all the leaf has been taken up by the pills. The pills should not be made too moist, otherwise a larger number of leaves will be necessary and the finish will be dull. Varnishing Pills.—Pills containing easily oxidizable sub- stances, such as Phosphorus, Phosphides, Ferrous Iodide or Bromide, deliquescent salts, etc., are usually coated with a varnish. The pills are placed in a flat-bottomed capsule, then sufficient of the ethereal varnish is poured over them to wet them, the dish is covered and then rotated so as to distribute the varnish equally over their surface. They are then transferred to a pill tile, or any glazed surface, and allowed to dry. As a varnish, the Pharmacopoeia recommends a solution of balsam of Tolu, 10 parts, in 15 parts of ether. Hager recommends mastic, 5 parts, and balsam of Tolu, 15 parts, to be dissolved in a mixture of 25 parts of alcohol and 8 parts of ether. Collodion has also been recommended for this purpose. In this case the coating should be made as light as possible. Sugar Coating.—Sugar coating can only be carried on success- fully on the large scale. This is accomplished in very much the same manner as that employed by the confectioners in coating almonds; a large quantity of pills are rotated in a carefully heated copper kettle with powdered sugar, moistened from time to time with syrup. The smooth coating results from the attri- tion produced. The polish is imparted by rapidly rotating the finished pills with some pieces of wax, or paraffin. For coating small quantities of pills, the following formula of C. Faust yields fair results:— Moisten the pills with a mixture of 1 part of glycerin and 2 parts of absolute alcohol, and throw them into a box containing a liberal supply of a fine powder composed of 4 parts of sugar, 2 Fig. 358. Pill Silverer. 328 HANDBOOK OF PHARMACY. parts of tragacanth and 1 part of starch, and roll them around well. Sift them free of the powder, moisten, and again roll them in the powder. To give a glaze to the pills, moisten them with a mixture of 1 part of glycerin and 2 parts of ether, and roll in a powder consisting of equal parts of talc and calcium carbonate. In making the pills on a large scale the final polish is given by rotating them, after being coated, in a cylindrical vessel with some pieces of hard paraffin. Pearl Coating.—This consists in covering the pills with a thin layer of powdered French chalk. The pills contained in a cylindrical vessel are moistened with sufficient syrup of acacia to dampen their surface after rotating them; then an excess of very fine French chalk is added and the pills rotated until a smooth, polished surface results. It would be well to add a little powdered saccharin, so as to impart a more pleasant taste to the coating material. Gelatin Coating.—Gelatin-coated pills owe their popularity to the elegant appearance and ready solubility of this coating. For coating pills on the large scale, the invention of J. B. Russell, of Detroit, is largely employed. This consists in holding the pills securely upon the ends of small tubes by means of suction. The machine consists of a box to which are attached numerous small tubes; the vacuum caused by the air being exhausted from this produces suction, which attracts and holds the pills in position. The latter are then dipped into the gelatin solution, whereby one- half of their surface becomes coated, then they are quickly dried and reversed and again dipped. Gelatin coating may be readily and quickly imparted on the small scale by using the following gelatin solution:— French Gelatin (so-called Gold Brand), 4 parts. Acacia (select pieces), 1 part. Boric Acid, 0.25 part. Water, 40 parts. The gelatin and acacia are macerated in the water for twelve hours, and then dissolved by heating on a water-bath with the boric acid. The vessel should be kept covered during the heating, so as to avoid loss of water by evaporation and the formation of a scum on the surface. This solution, when cold, solidifies to a jelly. It may be kept in this condition and a portion melted when wanted. The first requisite is that the pill be dry and free from dusting- powder. The simplest form of coater may be made by inserting needles, eye-end down, in a large cork, at a sufficient angle so as not to interfere with one another. The pills are impaled on these, then dipped into the gelatin solution, withdrawn, and then held a moment to allow the superfluous gelatin to collect in the form of a drop, which is removed by touching the surface of the gelatin solution. The cork is then rotated about, so as to permit the gelatin to set evenly over the surface of the pills. SOLIDS—.FOR INTERNAL USE. 329 A very convenient machine for gelatin-coating for the use of the pharmacist, is that devised by Mr. Maynard, of Chicago (Fig. 359). The pills are first rolled into the conical indentations of a plate provided for this purpose. A needle-holder is provided, which consists of a circular plate in which are set a number of needles; on either edge of this plate are placed guiding pins, by means of which the operator is en- abled to accurately center the pills with the needle points. By means of the handle the needle - holder is pressed downward, until the pills are securely impaled on the needlepoints. These are then dipped into the solution, as directed above, and rotated; then, after the gelatin film has become cold and sufficiently hard, the pills are removed by a mechanical device, and set aside on little trays to dry. The gel- atin solution should be kept constantly covered when not dipping. The coater devised by Prof. Patch (Fig. 360) con- sists of wooden strips con- taining 16 needles for im- paling the pills. These strips are provided with adjustable handles, so that as soon as the pills have been dipped they may be rotated by hand sufficiently until they have set; then the strips holding the pills are secured on the wheel, which is made to rotate alternately in both directions, for the purpose of securing uniformity of the coating and facilitating the drying. The pills are removed from the needles by means of a comb attached to the box. Keratin or Salol Coating.—In those instances where it is desired to restrict the action of the medicinal agent (such as naphthalin, Fig. 359. Gelatin Pill Coater (Maynard). Fig. 360. Gelatin-Coating Machine (Patch). 330 HANDBOOK OF PHARMACY. koussin, tannic acid, etc.), to the intestinal tract, it is necessary that the pill be coated with some agent which is not acted on by the acid gastric juices, so that it may pass undissolved through the stomach into the duodenum, where the alkaline secretions cause a solution of the coating and subsequent disintegration of the pill. For this purpose we have two agents, namely Keratin * and Salol.f Keratin Coating.—For coating with keratin, oily excipients should be employed in making the pills; one excipient recom- mended for this purpose consists of a mixture of 3 parts of mutton suet and 1 part of white wax; should other excipients be neces- sary the pills should be first coated with a thin layer of cacao- butter. The coating solution is made by dissolving 7 parts of keratin in 100 parts of concentrated acetic acid, or 1 part of keratin in a mixture of 10 parts each of ammonia water and water. The pills are placed in a large porcelain capsule, 4 or 5 drops of the keratin solution added, and then rolled about every five or ten minutes for half an hour. Then another addition of a few drops of the solution is made and the pills rotated as before. The procedure may be repeated once or twice more. Another method consists in impaling the pills on needles and applying the solution of keratin with a camel’s hair brush. Two applica- tions generally suffice; the first coat should be allowed to dry before applying the second. Salol Coating.—The pills should be impaled on needles (as in coating with gelatin), then dipped into the melted salol contained in a small, deep capsule. The coating hardens almost as soon as the pills are removed from the bath. Such pills have the appear- ance of being sugar-coated. The pin-holes left after removing the pills from the needles should be closed by applying a little melted salol with a brush. This coating may be applied to gelatin capsules as well. A coating of 0.2 to 0.3 Gm. of salol suffices to prevent the pill from being crushed by the pressure of the tongue against the palate. The pills must not be bitten, and not be taken with hot food or fluids. * The Preparation of Keratin.—Dieterich’s modified formula for the preparation of keratin is as follows: Digest 20 Gm. of finely cut goose quills in water for ten hours, and afterward macerate in a mixture of 100 Gm. of ether and 100 Gm. of alcohol for eight days; filter off the liquid, dry the quill, and put it in a large flask containing 200 Gm. of glacial acetic acid ; stopper the flask with a perforated cork, and insert a glass tube in the perforation to serve as a condenser. Boil gently in a sand-bath for 20 to 40 hours, and, when the quill is nearly all dissolved, filter through glass-wool and evaporate the filtrate in a porcelain capsule to a syrup; spread this on clean glass plates and dry. Finally, scrape off the keratin in scales. f Salol is the salicylic ether of phenol, its formula being CflH5C7Hr,O3. It is a crystalline compound which melts at 42° C. In the alkaline secretions of the small intestine it is broken up into phenol and salicylic acid. SOLIDS—FOR INTERNAL USE. 331 TABLETTzE. TABLET TRITURATES. Tablet Triturates consist of the medicine, which, if a dry solid, has been triturated with sugar of milk until a thorough and com- plete division and distribution of it has been made. In the case of pasty or fluid bodies, these are mixed in a wet state with sugar of milk, the whole dried, and then finely subdivided by tritura- tion. The powder in either case is then formed into a pasty mass with varying proportions of alcohol and water, or other suitable menstruum, and afterwards moulded into tablets of uniform size and weight. The formula for each separate combination is arrived at in the following way:— The mould is filled with finely-powdered sugar of milk, which has been wetted to a pasty mass with diluted alcohol. The tablets are then pressed from the mould, thoroughly dried and weighed. This weight is generally sixty-five (65) grains for fifty (50) tablets for the rubber moulds now usually supplied, making a tablet Fig. 361. Rubber Tablet Triturate Mould.* weighing slightly less than one and one-third (1|) grains when filled with plain milk sugar. The weight of the plain sugar of milk tablet is slightly increased with the increased solvent action of the menstruum, as more of the sugar enters solution, making the tablet more compact. The next step is to ascertain how much milk sugar must be omitted from the previously ascertained amount in order to make room for the medicinal constituents. For this purpose one hundred and thirty (130) grains of milk sugar are weighed off, which is equivalent to one hundred (100) finished tablets of plain sugar of milk. From these 130 grains a bulk is taken, equivalent, as nearly as possible, to that of the substance to be incorporated, and its weight noted. The active ingredient, * This consists of two parts, the lower, heavier portion bearing the punch-pins, which number fifty for the regular tablet triturates, and one hundred for the hypodermic size. There are two extra, larger and higher pins at either end, which gauge the mould-plate so that the openings come in line with the punch-pins. The upper portion is the mould proper, consisting of a rubber plate with regularly arranged perforations, corresponding in di vision, size and location of the punch-pins. The mould-plate bears a number which is identical with that upon the plate bearing the pins, and when the tablets are to be pushed through, the two parts must be so adjusted that the ends bearing the num- bers come together, and the face of the mould-plate bearing the number must be turned upward. 332 HANDBOOK OF PHARMACY. if a dry solid, is now mixed with the remaining portion of sugar of milk by thorough trituration. In the case of solid extracts, tinctures and other fluids, these are mixed with the remaining portion of sugar of milk, if necessary, by the aid of water or some other menstruum which dissolves them perfectly, then the mass is dried and powdered. After the mixture has been made, dried and thoroughly tritu- rated, it is wetted with a suitable menstruum, and moulded, care being taken to scrape the mortar as clean as possible in order not to waste any of the material. The tablets are then carefully dried. If there be any mass in excess of that required for the one hundred tablets, it shows that not enough milk sugar has been taken from the original 130 grains. The weight of this excess is generally equal to that of an equal bulk of milk sugar. Hence it will only be necessary, at the next trial, to remove as much more milk sugar as the bulk of this excess amounts to. If there should be less than one hundred tablets, the weight of the number deficient is ascertained by determining the average weight of the finished tablets, and deducting the calculated weight of the missing tablets from the weight of the bulk of the sugar of milk originally separated. At the next trial the amount of milk sugar removed from the original 130 grains should be as much less, as the weight of the missing tablets amounted to. In each case the formula finally found, by actual experiment, to yield a correct result, should be noted in a special book, for the purpose of future reference. It is important that all the ingredients, and the mixture of powders ready for moulding, should be in the finest possible state of subdivision. If they are coarse, the tablets will not show a smooth, finished appearance. In tablets composed nearly all of sugar of milk, if the latter be in coarse powder, it necessitates the addition of more water to the alcohol than is required when the milk sugar is in very fine powder. The menstruum selected should possess a slight solvent action upon one or more of the ingredients, but the latter should not be too freely soluble, since the mass is then moulded with difficulty, and the tablets prepared therefrom will be uneven, sometimes being cracked on the surface and very hard. It should possess sufficient solvent action to make a firm, yet not too hard a tablet, one that will hold firmly together when shaken in a vial, and which should readily disintegrate upon the addition of water. It is, however, impossible to prepare all the various com- binations in such form that they readily dissolve or diffuse upon the addition of water, the rapidity of disintegration depending upon the proportion and soluble character of the constituents. The menstrua generally used are alcohol, absolute alcohol, alcohol and water, and chloroform. For tablets composed nearly entirely of sugar of milk, a menstruum composed of three vol- umes of alcohol and one volume of water is preferable. For SOLIDS—FOR INTERNAL USE. 333 bodies insoluble in alcohol the proportion of water is raised in proportion to the increase of active ingredient. The menstruum must, therefore, be so adjusted that it will dissolve enough of either the milk sugar, or of the active ingredient, to make a suf- ficiently firm tablet. As examples may be quoted: reduced iron, binoxide of manganese, oxalate of cerium, bismuth subnitrate and subcarbonate, and the higher strength calomel tablets. For codeine, podophyllin, leptandrin, aloin, and bodies very soluble in alcohol, it is better to use water exclusively for moulding. For such tablets in which a chemical reaction takes place between the various constituents, with the formation of a new product which is desired, a menstruum must be selected which does not exert a soluble action upon all of the active constituents. For example, we combine sodium bicarbonate with saccharin, in order to increase the solubility, thereby intensifying the sweetness of the latter; as a menstruum for moistening, we employ absolute alcohol, as it exerts a solvent action on the saccharin only, yet binding the constituents to a firm tablet. In the case of fluid extracts and tinctures, thorough trituration with the milk sugar is generally sufficient to produce a homo- geneous mass for drying. Solid extracts produce more difficulties. If water is to be used as diluent, not more than the absolutely required amount should be employed, since any excess will cause the mass to form lumps or large cakes, and render the subsequent drying difficult. After the mass is dried, it must be reduced to a fine powder, previous to being moulded. To form a paste, the best liquid in this case is a mixture of alcohol three volumes and chloroform one volume. Water alone usually renders the mass too sticky, and alcohol alone is not adapted to aqueous or hydro- alcoholic extracts, since the extracts abstract the water from the alcohol, and thus produce an unmanageable adhesive mass. In preparing the powder for moulding, it should be wetted to a pasty consistence, the mould be placed upon a smooth surface, a pill tile answering admirably, and the wetted powder pressed into the spaces with a horn or ivory spatula which is drawn over the mould. Sometimes the mass adheres to the spatula and is drawn from the holes. This is remedied by dipping the spatula in the menstruum used for wetting the mixture before drawing it over the surface. The mould is then reversed by sliding it toward and off the edge of the tile without raising it, the spatula is drawn over the other side of the mould and the latter then again drawn toward and off the edge. The tablets are now pressed out by the punch pin plate and allowed to dry a few minutes upon the punch pins, then shaken off by striking the pin-plate forcibly upon the counter covered with a sheet of paper to receive the tablets. If the tablets are to be finished as speedily as possible, it is advisable to blow heated air over the surface of the side of the mould which comes in contact with the punch pins. This is best accomplished by holding the mould some distance from a gas 334 HANI JOK OF PHARMACY. flame and blowing the upper extremity of the flame towards the mould, the force of the breath carrying considerable heated air with its help to dry the surface quickly. Care should be exercised, if the mould is of rubber, that not too great a heat be directed toward the mould, otherwise it will warp. Moreover, if alcohol has been used for moistening, care must be taken to prevent igni- tion of the vapor. The rubbing of some dry powder (dry milk sugar or lycopodium) over the side of the mould to come next to the punch pins, helps to absorb the excess of moisture and pre- vents the tablets from sticking to the punch pins. The tablets should never be left in the moulds over ten minutes, because if they are allowed to dry in the mould, they cannot be pressed from it without crumbling. The drying process is best completed by placing them upon a sieve which exposes their entire surface, and allows more rapid evaporation of the menstruum. This is particularly necessary when the tablet is colored by the active ingredient, in solution in the menstruum. If such a tablet were dried while lying on a solid surface, the coloring matter would, by the law of capillarity, be deposited near the upper surface, and hence this side would be darker in color than the lower, the evaporation having been entirely from the upper end, while upon the sieve it will be from the entire surface, the color being equally distributed near the entire surface of the tablet, the interior always being lighter in color. In preparing tablets upon a large scale they are allowed to dry upon the punch pins in a draught of slightly warmed dehydrated air. When nearly dry, they are scraped from the punch pins and the drying completed in a hot-air chamber. For hypodermic tablets, sugar of milk is well adapted, and the rules to follow for their preparation are exactly similar to those for the Tablet Triturate. The rubber hypodermic mould, usually sold, makes tablets which weigh about three-quarters of a grain. The menstruum, used for most of the combinations, is three vol- umes of alcohol and one volume of water. In some of the higher strength morphine tablets it is necessary to use diluted alcohol. When solid extracts are to be combined into tablets, the mass should be moistened with a menstruum, composed of a mixture of alcohol three volumes and chloroform one volume. SOLIDS—FOR INTERS.j USE. 335 COMPRESSED TABLETS. Compressed tablets consist of some medicinal substance, or a mixture of substances, compressed to the form of a disc. The substance or mixture which is to be compressed must be in a granular form, either in its original granular condition, or pre- pared in a granular state by aid of a medium, such as cane sugar, or gum arabic, with the aid of water. In the preparation of compressed tablets it is important that the ingredients be brought by trituration to a very fine state of sub- division before being granulated, unless the substance is originally granular, or in a firm, hard crystalline form, from which a granular preparation may be obtained by grinding in a mill or mortar. If the material is compressed in the form of fine powder, it is difficult to be formed into uniform and nicely finished tablets. Not only does the powder not feed well into the mould, but, when pressure is applied, the air confined in the interstices of the powder has no chance of escaping, and is apt to produce tablets of irregular surfaces, edges, and weight, with a tendency to stick to the powders and die. To overcome these difficulties the substance is granulated by adding one-tenth of its weight of cane sugar and one-twentieth of its weight of acacia, thoroughly mixing and moistening with water until it is of such consistence that it can readily be forced through a No. 12 sieve without sticking to it, or clogging it. It is then dried. The finished granulation should always be perfectly dry, as a damp granulation occasions a great deal of trouble by sticking to the dies, and punches. The granulation is now forced through a No. 20 sieve, and the particles which do not readily pass through the meshes are forced through by the aid of a flat pestle. In adding the water to make the granulation, it should be thoroughly and evenly incorporated so that all the particles contain as nearly as possible an equal amount of moisture. The water is best added in small portions at a time. Some substances can be bought already granulated, and these, therefore, require no further preparation, and can be compressed in their original granular condition; for instance, ammonium chloride, potassium bromide, sodium bromide, potassium chlorate, potassium iodide. Some few crystalline salts, if in the form of hard crystals, without having lost any of their water of crystal- lization, can be ground in a mill to granular powder, or may be crushed to a granular form in a mortar; for instance, sodium phosphate and sodium sulphate. Cane sugar is the best material to use for granulating, as tablets prepared with it disintegrate or dissolve more quickly than those prepared with acacia. For beginners, it is better to use the cane sugar and acacia together as directed above, as this mixture is best adapted for granulating almost anything obtainable in a pulverulent condition. 336 HANDBOOK OF PHARMACY. Before the granulation is compressed, it is necessary to add a lubricant. This is a hydrocarbon oil entirely free from odor, the proportion added depending upon the character of the material. Ten to twelve drops is usually sufficient for one pound of the granulation. It is best added by means of a spray, and further mixed by stirring the mixture upon paper, or by dropping the oil into a mortar, adding about one-fortieth of the bulk of the mate- rial, mixing well by rubbing gently so that the granulation may be as little as possible reduced to powder, then adding the remainder of the granulation, and stirring gently. The hydrocarbon oil possesses the property of lubricating the different particles, allowing them to glide by each other freely, easily falling into the mould space, feeding the same amount each time, and thus making the finished tablets equal in weight. While the granulation is undergoing compression, the greater pro- portion of the oil is forced to the surface and edges of the tablet, preventing the sticking of particles of the material to the die and faces of the punches. Finely powdered French chalk is used in connection with the hydrocarbon oil, its properties being likewise that of a lubricant. The proportion used should be just as small as possible, not more than one-fortieth of the weight of the material. It should be added after the oil. Boracic acid is also used as a lubricant in such cases where the tablet is required to form a clear solution. It does not act so well as the French chalk. The more perfect and even the granulation has been prepared, the smaller the quantity of lubricant which it is necessary to use. In the preparation of compressed tablets from solid extracts, fluid extracts and tinctures, the two latter are to be concentrated to a syrupy consistence. A solid extract is best rubbed to a syrupy consistence by the aid of water. In both cases there should be no small particles of undissolved extract, as these would give the finished tablet a mottled or spotted appearance. If the quantity of extract to be contained in a tablet is small, say one-fourth of a grain of extract contained in a tablet weighing two grains, the excess of water may be absorbed by finely pow- dered starch, of which as much as 25 per cent, of the weight of the tablet may be added, if necessary, the principle being to leave the mixture of starch and extract sufficiently wet so that it may exert the required solvent action upon the remaining ingredients to form a proper consistence for granulation. If too much starch has been added, the extra quantity of water required is easily added to the mixture of starch, extract, and other material. When a tablet is to contain two or more grains of extract, the addition of the required amount of starch, so that the product will pass through a No. 12 sieve, would make it too large. Therefore, when the extract is in large proportion, it is a good plan to add to it half its weight of starch after it has been SOLIDS—FOR INTERNAL USE. 337 softened, then to dry the mass upon a steam-bath, and finally to crush it in a mortar, or to grind it in a mill to a No. 20 granu- lation. When a caked mass is to be reduced, by rubbing in a mortar, to a No. 20 granule, the material should be transferred to the sieve at short intervals, in order to separate that portion which has been reduced to the proper fineness ; otherwise, by continued rubbing, the greater portion of the material would be reduced to a fine powder. Extracts may also be incorporated in the form of a dry, im- palpable powder, if the proportion be small, and in such cases it is also a good plan to add some powdered starch to the material and extract; next, sufficient water is added, and well incorporated, the mixture passed through a No. 12 sieve, then dried, and, lastly, forced through a No. 20 sieve. It is not necessary to use any adhesive material, such as acacia or cane sugar, for tablets containing ex- tracts, unless the proportion of extract be very small. Spongy bodies like charcoal must be in impalpable powder, and not less than 25 per cent, of cane sugar should be added for granulation. If the charcoal cannot be obtained in a finely subdivided state, it is a good plan to add the proportion of sugar as above, to wet the mixture to such a state that it forms small cakes, and to dry per- fectly. The cakes are then reduced to very fine powder, moistened with sufficient water to make the mass pass through a No. 12 sieve, the granulation dried, and then reduced to granules, pass- ing through a No. 60 to 80 sieve. The powdered pepsin of the market is of a spongy nature, like charcoal, and is best prepared for compressing by adding one-tenth of its weight of cane sugar, then spraying diluted alcohol over the mixture, mixing thoroughly until all particles have been moist- ened, but are still in about No. 80 powder, then drying and com- pressing. Spongy substances should be fed to the machine in a very finely granular form. The large size granules offer too much resistance to the punches, and the tablet crumbles very easily. Spongy bodies, as a rule, require no lubricant. Scale pepsin and most of the other scale preparations can be compressed by reducing them to No. 30 or 40 granules, and lubri- cating them. Salts containing water of crystallization, organic or inorganic, which cannot be compressed without being first granulated, as, for example, lead acetate, zinc sulphate, alum and quinine sulphate, are best treated in the following manner:— The salt is reduced to a fine powder, mixed with one-twentieth of its weight of powdered gum arabic, moistened sufficiently with water to pass it through a No. 12 sieve, dried, again reduced to fine powder, mixed with one-tenth of its weight of cane sugar, moistened with just enough water to make it pass through a No. 12 sieve, then dried, first without, and lastly by aid of heat. The 338 HANDBOOK OF PHARMACY. mixture is then forced through a No. 20 sieve, lubricated and com- pressed. Bodies which are hygroscopic or deliquescent are best granu- lated with gum arabic exclusively, taking one-tenth of the weight of the substance and water for moistening. Combinations of rhubarb and soda are best granulated by add- ing to them one-tenth of their weight of cane sugar, and granu- lating with a mixture of one volume of glucose, 1 volume of water and three volumes of alcohol, well mixed, this mixture preventing the action of the alkali upon the rhubarb. Glucose is an excellent medium for making tablets hard and tough, so that they will not readily disintegrate, as, for example, lozenges which are intended for slow solution in the mouth. To improve the lozenge, the greater portion of the material should be cane sugar, with 10 per cent, of gum arabic, and the glucose should be diluted with 25 per cent, of water before being added. In tablets to form etfervescing solutions or to form new com- pounds when added to water, the constituents should be granu- lated separately, and mixed in a perfectly dry granular condition just before being compressed. A very important quality which compressed tablets should possess is that of rapid disintegration and solution. This is brought about by adding finely powdered starch, to the amount of from one-twentieth to one-tenth of the weight of material, to the granulated substance ready to be compressed. It is most important for certain insoluble bodies, such as phenacetin, acet- anilid, sulphonal, etc., that they disintegrate rapidly. These are best granulated with one-tenth of their weight of cane sugar, water being used for moistening. As stated before, the addition of acacia retards rapid disintegration and solution; hence it should not be used where cane sugar acts as a sufficiently adhesive agent. Fig. 362 illustrates the simplest form of a compressed tablet machine; this consists of a cast steel cylinder, into the base of which fits a short post with a concave surface. A steel plunger, having a corresponding concave depression on its lower extremity, is used for compression. The granule is introduced into the cylinder, and after inserting the plunger, a quick, sharp blow is struck by means of a wooden mallet, whereby the powder is com- pressed; then, after the cylinder is removed from the base, the plunger is tapped, which forces the tablet out into a proper receptacle. An improvement on this is the tablet machine illustrated in Fig. 363. Its construction is simple, being operated by means of a lever. It is capable of turning out tablets quite rapidly. For the preparation of large quantities of tablets, the larger machines of thd market afford all that is desirable. The pressure used for compressing the tablets should be just as light as possible, for the firmer the pressure the slower the disin- tegration of insoluble bodies, firm pressure not affecting very SOLIDS—FOR INTERNAL USE. 339 soluble substances, since their solution takes place from the surface. The pressure should be regulated so that the tablets may readily be broken in half by the fingers, but should not break to pieces when dropped upon the floor. With a light pressure the material has a greater tendency to stick to the face of the punches. The dies and punches should be of very hard temper and should be kept in good condition. They should be polished from time to time by the aid of finely powdered emery, preferably on a lathe. If this is not at hand, a round smoothened end of a piece of wood answers very well, and is used by dipping the end in oil, then in the emery, and rubbing over the surface of the punches. For polishing the dies, a rounded piece of wood, a little Fig. 362. Fig. 363. Compressed Tablet Mould. Compressed Tablet Mould. (W., T. & Co.) smaller than the bore of the die, dipped in the oil and emery, is well adapted. If the surface of the dies and punches is not kept smooth and polished, the material works into the uneven surface and adheres to it, making a tablet with rough surface and scraped edges, neces- sitating the frequent cleaning of the faces of the punches. If the dies be of soft temper, such bodies as exert considerable friction, as acetanilid, phenacetin, and antipyrin, will wear down the die quickly in that portion where the tablet is compressed, and by the constant wear the die is widened at this spot, especially at the point of the upper and lower surface of the tablet where there is the most wear, hence the tablet is slightly wider than the bore of the remaining portion of die. In being forced upwards 340 HANDBOOK OF PHARMACY. to be expelled from the die, the tablet is forced into a narrower space than that into which it had been compressed, which tends to bend it and loosen the flat or convex upper or lower surface, which may readily be split off by the thumb nail, but which will fall off spontaneously after the tablet has been shaken about some little time. This is termed “ capping.” The best remedy for the “ capping ” is a hard-tempered die; but this is not always at hand. Dampening the granulation very slightly with water will prevent it; but this increases the adhesive qualities, and the material is more liable to stick to the punches. However, if these are smooth and well polished, little trouble will be experienced from the sticking qualities. Reducing the pressure is another remedy; but, if the punches are not in good condition, the material will stick to them. Changing the weight of the tablet is still another remedy, the tablet to be compressed in a portion of the die that is not worn. 341 SOLIDS—.FOR INTERNAL USE. EXTRACTA—{Extracts'). Extracts are solid or semi-solid preparations obtained by the evaporation of solutions of the medicinal principles of drugs. According to the solvent employed in exhausting the drug they are designated as alcoholic, hydroalcoholic, aqueous, ethereal, acetic, or ammoniated extracts. The strength of these preparations bears no definite relationship to the drug, for the amount of solid extract * obtained depends on the nature of the drug, the solvent employed, and the mode of prepara- tion. The more aqueous the menstrua, the greater is the yield of extract, the more alcoholic the menstrua, the smaller the yield. It must be remembered that the activity of most drugs resides, as a rule, in certain definite principles, which generally constitute the smallest portion of the bulk of an extract; the other constitu- ents of the drug, embracing gums, starch, inert extractive, coloring matters, etc., constitute the larger inert portion soluble in water. Hence, the solvent selected for extraction must be such as to take up all the active, with as little of the inert matter as pos- sible. If an unscrupulous manufacturer were to employ water or a feebly alcoholic menstruum for extracting a drug whose active principles are soluble in alcohol only, he would obtain a large yield of inert extractive matter, while his neighbor who employs alcohol only, would obtain a very small yield of a very active pre- paration. If both products were sold in the market at equal rates, the former would be a fraud upon the public. Extracts also vary in consistence. Some are as liquid as honey, others have the consistence of a pill mass, and still others are hard and dry, hence there is not likely to be any uniformity of strength, with such variations as these. Therefore, unless there is some guarantee of intrinsic value based on its alkaloidal strength or physiological activity, no reliance can be placed on the strength of one extract as compared with another. Solid extracts are prepared either— (a) From the dried and powdered drug, by extraction with a solvent, or— (&) From the fresh, moist drug, by expression alone. * Prepared with official menstrua (U. S. Pharmacopoeia, 1880), the yield in extract is, according to J. Lammer, Jr., “Proceed. Amer. Phar. Association,” 1887, p. 35:— Per cent. Extractum Aconiti 12.76 “ Aloes, 91.54 “ Arnicae Radicis, 19.53 “ Belladonna Alcoholicum, . . . 32.23 “ Cannabis Indicae, 16.56 “ Cinchona, 26 40 “ Colchici Radicis, 23.20 “ Colocynthidis, 15.13 “ Conii, 10.73 “ Digitalis, 25.50 “ Euonymi, 18.31 “ Gentian®, 44.60 “ Glyeyrrhiza Purum, 25.32 “ Hamatoxyli, 5.30 Per cent. Extractum Hyoscyami (ale.), 16.64 “ Iridis, 8.90 “ Juglandis, 16.82 “ Kram erise . 8.40 “ Leptandra, 15.97 “ Mezerei, 7.10 “ Nucis Vomicae 6.17 “ Opii, 49.60 “ Physostigmatis, 6.20 “ PodophyTli, 8.31 “ Quassia, 2.24 “ Rhei, 25.66 “ Stramonii 14.02 “ Taraxaci 11.30 342 HANDBOOK OF PHARMACY. (а) When solid extracts are prepared from the dried drugs by extraction, the following rules should be observed:— 1st. Only the best obtainable drug should be employed. Poor drugs cannot be expected to yield active preparations; it is, there- fore, advisable to exercise the greatest care in their selection. 2d. That, whatever process of extraction is employed, it should be carried to as complete an exhaustion of the drug as possible. Extraction is effected by the process of maceration (15-20° C. for 24 to 48 hours), or digestion (35-40° C. for 12 hours) with expres- sion ; or by percolation. 3d. That the menstruum selected will deprive the drug of its active principles with as little inert matter as possible. The vari- ous menstrua directed by the Pharmacopoeia have been selected with this view; hence, an alteration of the menstruum with a view to economy is a reprehensible practice. 4th. The concentration of the liquid extract of the drug should take place as rapidly, and at as low a temperature as possible. Under no circumstances should it be heated over a direct flame. The greatest care is necessary in conducting the evaporation of extracts from such drugs as conium, blackhaw, valerian, etc., for in these the virtues reside mainly in volatile products; hence the slightest degree of overheating destroys their therapeutic value. The temperature of a water-bath or carefully regulated steam-bath is sufficient, while the fluid is being kept constantly in motion; a stirring arrangement, specially adapted for the use of the apothecary is shown in Fig. 97, page 72. The evaporation should be conducted as rapidly as possible to avoid prolonged heat- ing of the fluid. For this purpose the vacuum apparatus is em- ployed (Fig. 106, page 77). The various methods of conducting evaporation are explained in detail under Vaporization. (б) Certain plant drugs, when recently gathered and subjected to expression, yield their juices, impregnated with all their active principles; these juices, when evaporated, constitute a class of extracts generally known as Succi Spissati, or inspissated juices. Among the drugs adapted to this treatment are taraxacum, belladonna, hyoscyamus, and colchicum. The plants should be worked up immediately after being collected, being cut into pieces and bruised until reduced to a pulp. In case the plant is not very succulent, a little water should be added to assist in diluting and extracting the juice. The pulp is then enclosed in a canvas bag and subjected to expression. The juice thus obtained from fresh plants, or leaves, is of a more or less green color, due to the presence of chlorophyll. When heated to about 70° C., the albumen of the juice co- agulates, forming a precipitate which encloses the suspended impurities. These are readily removed by filtration. The sub- sequent concentration is carried out as already explained. SOLIDS—.FOR INTERNAL USE. 343 PHYSICAL CHARACTERS AND PRESERVATION OF EXTRACTS. The Pharmacopoeia recognizes two degrees of consistence—the soft, or pilular, and the hard extract. The pilular consistence should be such that the extract readily admits being rolled into pills, which retain their shape. Twenty-five of the official extracts should be of this consistence. The pilular extracts of the market vary considerably as regards their consistence, many being exceedingly soft, while others are quite hard. The hard extracts, of which seven are official, admit of being reduced to powder. The dispensing conveniences which a pow- dered extract offers, have led to the general introduction of all the various extracts in powder form. The indiscriminate substitution of these powdered extracts in place of the official pilular product is to be condemned, for the heat necessary to reduce the extracts to the proper degree of dry- ness is, in many instances, sufficient to destroy most or all the virtues of the drug contained in them. Again, many extracts cannot be brought, by themselves, to a sufficiently dry condition; hence, they must be mixed with various diluents, such as sugar of milk, starch, the powdered drug itself, etc.; then spread out in thin layers, and exposed in a warm (30-40° C.), dry place; then reduced to a powder, and preserved in well-closed vials. It will be seen from this, that another cause of variation of strength of these powdered extracts is the admixture of inert matter, to which there is no definite limit. Extracts should be preserved in closely covered jars, it being best to place the jar of extract in a canister having a close-fitting lid. Some extracts readily dry out and become very hard. In such cases it is well to moisten the surface with a little glycerin. Other extracts, owing to the presence of deliquescent salts, are quite hygroscopic, and absorb moisture readily. Still others become inert on standing for a long time, due to an alteration of their principles by the action of the air. Many extracts (as those of stramonium, hyoscyamus, bella- donna, etc.), contain numerous crystals of inorganic salts (potas- sium nitrate or chloride, etc.). The presence of these is manifested by the grittiness of the extract when rubbed on a slab under a spatula. Such extracts should always be rubbed with a few drops of water before being combined into ointments or suppositories. The official extracts are 33 in number, 25 being of pilular consistency and 7 dry. According to the menstrua employed for exhaustion, they may be classified thus:— Title. I. ALCOHOLIC EXTRACTS. Dose—Grammes. Extractum Aconiti, 0.006-0.015 “ Cannabis Indicae, 0.008-0.06 “ Cimicifugae, 0.2 -0.3 “ Iridis0.06-2.0 Jalapae,0.1 -0.3 “ Physostigmatis, 0.006-0.03 344 HANDBOOK OF PHARMACY. II. HYDRO-ALCOHOLIC EXTRACTS. Extractum Arnicae Radicis,0.1 -0.3 “ Belladonnas Foliorum Alcoholicum, 0.008-0.05 ‘ ‘ Cinchonae,1. -2.0 “ Colocynthidis,0.03 -0.1 Conii (with acetic acid),0.01 -0.1 Digitalis, 0.008-0.06 “ Ergotae (with acetic acid),0.2 -10 “ Euonymi, 0.06 -0.2 “ Hyoscyami, 0.06 -0.2 Juglandis,0.3 -0.2 Leptandrae0.06 -0 3 “ Nucis Vomicae (with acetic acid),0.01 -0.06 “ Podophylli, 0.06 -0.3 “ Rhei,0.3 -1.0 “ Stramonii Seminis,0.01 -0.2 “ Uvae Ursi,0.3 -1.0 III. AQUEOUS EXTRACTS. Extractum Aloes,0.2 -0.6 “ Colchici Radicis (with acetic acid),0.06 -0.1 “ Gentianae,0.3 -0.6 “ Glycyrrhizae, “ Glycyrrhizae Purum (with ammonia water), . . . . Haematoxyli,0.3 -2.0 Krameriae,0.3 -2.0 “ Opii,0 01 -0.06 “ Quassiae,0.06 -2.0 “ Taraxaci, 0.5 -2.0 IV. COMPOUND EXTRACTS. Extractum Colocynthidis Compositum, 0.3 -1.5 Extractum Nucis Vomicae.—The menstruum selected for the extraction of nux vomica must be of such a character that it will readily take up the alkaloidal principles and yet as little of the fatty oil as possible. The forty-eight hours’ maceration with the acidified menstruum of alcohol, 3 parts, and water, 1 part, is necessary for the softening of the tissues preparatory to extrac- tion. The presence of the acetic acid greatly assists the solution of the alkaloids. As the extract is directed to be reduced to a powder, it is necessary to first remove the fixed oil present. This is accomplished by washing the extract obtained from the con- centration of the percolates with ether. Since some of the alkaloids are associated with the fat which has been removed, it is necessary to remove these by washing the fat with acetic acid and hot water. After completion, a portion of the extract is assayed for alka- loids. In another portion, the amount of water is determined. From these results the total percentage of alkaloids in the dry extract is calculated, enough sugar of milk being added to bring the amount of total alkaloids in the dry extract up to 15 per cent. Example.—A sample of extract of nux vomica, prepared by the process of the U. S. Pharmacopoeia, assayed 16 per cent, of alka- EXPLANATORY. SOLIDS—FOR INTERNAL USE. 345 loids, and contained 22 per cent, of moisture. How much sugar of milk should be added to bring it to the pharmacopoeial require- ment of 15 per cent, of alkaloids when dry ? I. Since the moisture or water which is present has, eventually, all to be evaporated off, it need not be taken into account further than to deduct it from 100, whereby the percentage of dry extract is obtained. The further calculation will have to deal only with this. The extract contains 100 — 22 = 78 per cent, of dry substance. According to the assay, the 100 parts of moist, or 78 parts of dry extract contain 16 parts of alkaloids. The next step will be to ascertain how much of these 78 parts of dry extract will contain 15 parts of alkaloids:— {Equation 1.) 16 : 15 :: 78 : x ; x — 73.125. Since 73.125 parts of the dry extract contain 15 parts of alka- loids, it will only be necessary to dilute these 73.125 parts with sugar of milk to 100 parts in order to convert the 15 parts of alkaloids into percentage :— {Equation 2.) 100 — 73.125 = 26.875. That is, for every 73.125 of dry extract, 26.875 parts of sugar of milk will have to be added. But the original extract contains 78 parts of dry substance. Hence, the amount of sugar of milk required for this (which is equal to 100 parts of the moist extract) will be found by the proposition :— {Equation 3.) 73.125 : 78 — 26.875 : x •, x = 28.667 parts. II. The same result may be arrived at in another manner. The extract contains 100 — 22 = 78 per cent, of dry substance, and this contains 16 parts of alkaloids. Calculated to percentage, this would become:— (.Egwa/ion 4-) 78 : 100 = 16 : a: ; x = 20.513. That is, 100 parts of a dry extract of the same strength as the 78 parts just mentioned, would contain 20.513 parts of the alkaloids. Now, since every 15 parts of alkaloids are augmented in this pro- duct to 20.513 parts, it will only be necessary to dilute the original extract with sugar of milk in the proportion of 15 to 20.513:— {Equation 5.) 15 : 20.513 = 78 of dry extract (= 100 moist) : x. x — 106.667. That is, to every 78 parts of dry extract, or to every 100 parts of moist extract, there will have to be added :— {Equation 6.) 106.667 — 78 = 28.667 parts of sugar of milk. III. Based upon either of the foregoing methods, which are really identical and differ only in form, a general formula may be derived. Let the several values be expressed by letters, as follows:— m = percentage of moisture in the moist extract. a = “ “ alkaloids “ “ “ d = “ “ dry substance “ “ x — amount of sugar of milk required to be added to every 100 parts of the moist extract, to make it contain 15 per cent, of alka- loids, when dry. 346 HANDBOOK OF PHARMACY. Then we have, using equation (3), but substituting in it general terms derived from equations (1) and (2), and remembering that d = 100 — m :— {Equation 7.) - : d = (100 — : x. x — 6.667 a — d. Or, we may derive this value from equations (6) and (5), in a similar manner:— {Equation 8.) IOOji — x . x — 6.667 a — d. The rule, therefore, expressed in words, would be: “ To find the amount of sugar of milk required to be added to 100 parts of moist extract of nux vomica of known percentage of alkaloids and moisture, in order to make it contain 15 per cent, of alka- loids when dry, multiply the percentage of alkaloids found with 6.667, and deduct therefrom the percentage of moisture.” Assay of Extract of Nux Vomica:— Extract of Nux Vomica, dried at 100° C. (212° F.), two grammes, (2 Gm.). Alcohol, Ammonia Water, Water, Chloroform, Decinormal Sulphuric Acid (V. S.), Centinormal Potassium Hydrate V. S., each, a sufficient quantity. “Put 2 Gm. of the dried Extract of Nux Vomica into a glass separator, add to it 20 Cc. of a previously prepared mixture of 2 volumes of alcohol, 1 volume of ammonia water (specific gravity 0.960), and 1 volume of water, and shake the well-stoppered sepa- rator until the extract is dissolved. Then add 20 Cc. of chloroform and agitate during five minutes. Allow the chloroform to separate, remove it as far as possible, pour into the separator a few Cc. of chloroform, and, without shaking, draw this off through the stop- cock to wash the outlet-tube. Repeat the extraction with two further portions of chloroform of 15 Cc. each, and wash the outlet- tube each time as just directed. Collect all the chloroformic solutions in a wide beaker, expose the latter to a gentle heat, on a water-bath, until the chloroform and ammonia are completely dissipated, add to the residue 10 Cc. of decinormal sulphuric acid measured with great care from a burette, stir gently, and then add 20 Cc. of hot water. When solution has taken place, add 2 Cc. of brazil wood T. S., and then carefully run in centinormal potas- sium hydrate V. S., until a permanent pinkish color is produced by the action of a slight excess of alkali upon the brazil wood indicator. Divide the number of Cc. of centinormal potassium V. S. used by 10, subtract the number found from 10 (the 10 Cc. of decinormal acid used), multiply the remainder by 0.0364 and that product by 50 (or, multiplied at once by 1.82), which will give the percentage of total alkaloids in the Extract of Nux Vomica, it being assumed that strychnine and brucine are present in equal proportion, and the above factor being found by taking SOLIDS— FOR INTERNAL USE. 347 the mean of their respective molecular weights rounded off to whole numbers [(334 + 394) 2 — 364.] (U. S. Pharmacopoeia.)” As to the glass separator, the bulbed or pear-shaped form (50 Cc. capacity) as shown in Fig. 296, should be used. The extract readily dissolves in the mixture of alcohol and water, the ammonia water serving to liberate the alkaloids from their combination with igasuric acid ; the chloroform added dissolves the liberated alkaloids. After the chloroform is added, the mixture should be shaken by a rotary motion in order to avoid emulsification. When the chloroform once becomes emulsionized, it is a difficult matter to bring about a separation of the fluids. After the usual number of subsequent extractions, the chloroformic solutions, upon evap- oration, yield an alkaloidal residue consisting of a mixture of strychnine and brucine, assumed to be in equal proportions. Alkaloids, being strong bases, are capable of neutralizing acids in definite proportions. Hence, the usual method of estimating alkalies by means of a standard solution of an acid can be applied to certain alkaloids with a great degree of accuracy. The reaction is as follows:— 2H2SO4 4- 2C21H„N,O, + 2C23H28N2O4 = (C21H22N2O2)2H2SO4 + (C23H26N2O4)2H2SO4 Sulphuric Acid. Strychnine. Brucine. Strychnine Sulphate. Brucine Sulphate. 2 X 97.82 2 X 333.31 2 X 393.17 One molecule of Sulphuric Acid. Strychnine. Brucine. 97.82 = 333.31 + 393.17 = 726.48 total. 1000 Cc. containing 48.91 — 363.24 (J of 726.48) alkaloids. 1 Cc. “ “ 0.04891 = 0.0364 alkaloids. Hence each cubic centimeter of decinormal sulphuric acid is equivalent to 0.364 gramme of total alkaloids.* Since the usual indicators are not sufficiently sensitive in the presence of the alkaloids, the Pharmacopoeia directs the use of Brazil-wood test solution, which strikes a yellow color with acids and a pinkish color with alkalies. When operating with this indicator, it is always advisable to place alongside of the actual test-sample, on a piece of white paper, two beakers, each containing a like volume of water and indicator, to one of which about 1 Cc. of the normal acid has been added, and in the other the equivalent amount of alkaline volumetric solution; with these beakers as a means of comparison, the change of color in the solution for assay can be more conveniently fixed. Example.—The chloroformic residue obtained from 2 grammes of extract, which has been dissolved in 10 Cc. of decinormal sulphuric acid, required 28 Cc. of centinormal potassium hydrate V. S. for neutralization. What percentage of total alkaloids does the extract contain ? We have dissolved the alkaloids in an excess (10 Cc.) of the decinormal acid. In order to ascertain how much of the acid has not been neutralized by the alkaloids, we titrate back with * Assuming them to be present in equal proportions. 348 HANDBOOK OF PHARMACY. centinormal potassium hydrate, and subtract the equivalent amount of the latter from the former, thus: 10 Cc. of H2SO4, minus 1.6 Cc. of KOH (which is the same as 16 Cc. of KOH), leaves 8.4 Cc. of decinormal acid which has been neutralized by N the alkaloids. Then, if 1 cubic centimeter of 10- H2SO4 = 0.0364 Gm. of alkaloid, 8.4 Cc. of the acid = 8.4 X 0.0364 = 0.3057 Gm. of alkaloid. Therefore, there are 0.3057 Gm. of total alkaloids (strychnine and brucine) present. The percentage may be found as usual (0.3057 -h 2 X 100 = 15.28 per cent.), or as directed by the Pharmacopoeia by multiplying by 50 (50 X 0.3057) = 15.28 per cent. SOLIDS—FOR INTERNAL USE. 349 ABSTRACTA {Abstracts). Abstracts are powdered extracts, the strength of which bear a definite and uniform relation to the drug. This class of pre- parations were introduced into the Pharmacopoeia of 1880, but because of their unpopularity* they were dropped from the present Pharmacopoeia of 1890. The strength of the abstracts represents twice that of the drug or of the fluid extract from which they are prepared. The general formula directed by the Pharmacopoeia of 1880 is as follows:— “ Drug, in No. 60 powder, two hundred parts [or four ounces av.] ; Sugar of Milk, recently dried and in fine powder, Alcohol, each, a sufficient quantity, to make one hundred parts [or two ounces av.]. Moisten the drug with eighty parts [or one and three-quarter fluid- ounces] of Alcohol, and pack firmly in a cylindrical glass perco- lator ; then add enough Alcohol to saturate the powder and leave a stratum above it. When the liquid begins to drop from the percolator, close the lower orifice, and, having closely covered the percolator, macerate for forty-eight hours. Then allow the perco- lation to proceed, gradually adding Alcohol, until the drug is exhausted. Reserve the first one hundred and seventy parts [or three and one-half fluidounces] of the percolate, evaporate the remainder to thirty parts [or half a fluidounce] at a temperature not exceeding 50° C. (122° F.) and mix with the reserved portion. Place the mixture in an evaporating dish, and, having added fifty parts [or one ounce av.] of Sugar of Milk, cover it with a piece of thin muslin gauze, and set aside in a warm place, where the temperature will not rise above 50° C.(122° F.), until the mixture is dry. Lastly, having added enough Sugar of Milk to make the mixture weigh one hundred parts [or two ounces av.], reduce it to a fine, uniform powder. Preserve the powder in a well-stopped bottle.” The abstracts recognized by the U. S. Pharmacopoeia of 1880 were Abstractum Aconiti, Belladonnae, Conii, Digitalis, Hyos- cyami, Ignatiae, Jalapae, Nucis vomicae, Podophylli, Senegae, and Valerianae. * It is unfortunate that this class of preparations of definite and uniform strength should not he able to supplant a class characterized by so little uniformity and so great a variation as the solid extracts. 350 HANDBOOK OF PHABMACY. RESINJE—(Resins). These are solid preparations usually obtained by exhausting certain drugs with alcohol and precipitating the resinous prin- ciples by addition of water. The procedure is applied to those drugs whose activity resides in resinous principles. The Pharmacopoeia recognizes four resins, three of which are prepared in the following manner: The drug is exhausted with alcohol; after concentration of this alcoholic extract to a syrupy consistence it is poured slowly, with constant stirring, and in a thin stream, into a large excess of cold water, the precipitate is allowed to subside, washed by decantation, strained off, and dried with a gentle heat. Resin of podophyllum is precipitated with acidulated* water, in order to facilitate its separation, the acid imparting at the same time a brighter yellow color to the resin. The water used in precipitating this resin should be cold, and the resin dried by exposure to air in a cool place. Resin of copaiba, being one of the two constituents of balsam of copaiba, is more readily separated by distilling off the volatile oil. RESIN.E, U. S. P. Title. Preparation. Dose. Resina Copaiba?, .... Product remaining after distillation. 0.3 to 1.5 Gm. “ Jalapae, .... Precipitation. << 0.1 to 0.3 Gm. “ Podophylli, . . . 0.008 to 0.05 Gm. “ Scammonii, . . . u 0.2 to 0.5 Gm. RESINOIDS-(Eclectic). These are a class of resinous powders or medicinal substances obtained by precipitation of the alcoholic tinctures of certain plants or plant-parts, either by means of water alone or aided by heat, or by acids or other agents. If the drug contains an oleoresin, it is necessary, in order to bring the precipitate to a powder form, to mix it with a sufficient quantity of the powdered drug. Such resinoids as hydrastin and sanguinarin are precipitated in water acidulated with an acid or rendered slightly alkaline with ammonia water. These preparations, the names of which generally end in -in, should not be confounded with the similarly sounding alkaloids or other active plant principles. They vary greatly in their activity, owing to various impurities and to the fact that many do not represent all the virtues of the plants from which they are obtained. * Water containing alum is also employed, but yields a product contaminated with alumina. SOLIDS—FOR INTERNAL USE. 351 The following list includes most of these preparations, with their average doses,* such as are given by eclectic authorities:— Obtained from Average dose in Average Obtained from dose in Aconitin, .... Aconite Root, . . . grains. Hydrastin, . . . grains. Goldenseal, 1-2 Aletriii, . . . Star Grass i- 2 Hydrastin Mur., Golden sea 1 (Berber i n a) ll it 1- 3 Alnuin, Tag Alder Bark, . 2-10 Hydrastin Sul., . 1- 2 Ampelopsin, . . American Ivy, . . 2- 4 Hydrastin Nit., . ll ll 1- 2 Apocynin, . . . . Bitter Root, . . . 4- 1 Hydrastin Phos., ll ll 1- 2 Atropin, .... . Belladonna, .... Hyoscyamin, . . Henbane, B- 1 Asclepin, .... Baptisin . Pleurisy Root, . . Inulin, Elecampane, .... 1- 3 Wild Indigo Root, 1- 3 Irisin, .... Jalapin, .... Juglandin, . . . Blue Flag 2- 4 Barosmin, . Btichu, 2- 3 Jalap, 1- 3 Betin, . Beets, 2- 4 Butternut, 2- 5 Bryonin, . . White Bryony, . . 4 2 Leontodin, . . . Dandelion, 2- 4 Caiilophyllin, . . Blue Cohosh, . . . 1- 5 Leptandrin, . . Culvers Root, . . 2- 4 Cerasein, .... Choke Cherry, . . 2-10 Lobelin Lobelia, 1- 3 Chelonin, .... Chiniaphilin, . . . Balmony 1- 2 Lupulin, .... Hops, 1- 2 . Pipsissewa, .... 2- 3 Ly copin, .... Bugle Weed, .... 1- 4 Chionanthin, . . Fringe Tree, . . . 1- 3 Macrotin, .... Black Cohosh, . . . l~ 2 Cimicifugin, . . . See Macrotin, . . 4- 2 Menispermin, . . Yellow Parilla, . . . 1- 4 Collinsonin, . . . . Stone Root, .... 2- 4 Mv ricin, .... Bayberry, ...... Poke Root, 1- 3 Colocynthin, . . . Bitter Apple, . . . Phytolaccin, . . 1- 3 Cornin, . Dogwood, .... 2- 4 Prunin, Wild Cherry 2- 3 Corydalin, . . . . Turkey Pea, . . . 1- 3 Populin, .... Poplar, 2- 4 Cypripedin, . . . Lady Slipper, . . . 1- 3 Podophvllin, . . Mandrake, i~3 Digitalin, . . . . Foxglove, . . 4- I Podophvllin Neut. 4- 2 Dioscorein, . . Wild Yam, .... J- 4 Ptelein, . . Wafer Ash, 1- 3 Ergotin, . . . . Ergot *£1 Rhein, Rhubarb, 1- 4 Erythroxylin, . Coca Leaves, . . . Rhusin, Sumach, 1- 2 Euonvmin, . . . . Wahoo, i-3 Rumin, Yellow Dock, .... 1- 3 Eupatorin (Perf.), Boneset, . . 1- 3 Sanguinarin, . . Blood Root, 1- 3 Eupatorin (Purp.), Queen of Meadow, 1- 4 Scuteliarin, . . . Scullcap, 1- 2 Euphorbin, . . . . Blooming Spurge, . i- 3 Senecin, .... Smilacin, .... Life Root, Sarsaparilla (Hon.), . 1- 3 Eupurpurin, . . . Queen of Meadow, 1- 4 2- 5 Frazerin . American Colombo, 1- 3 Stillingin, . . . Queen’s Root, .... 1- 3 Gelsemin, . . . Yellow Jessamine, 4- 1 Trilliin, . . . Beth Root, Am. Hellebore, . . . 2- 4 Geraniin . Cranesbill 1- 3 Veratrin, .... Gossypiin, . . . . Cotton Root, . . . 1- 5 Viburnin, .... Cramp Bark, .... Hamamelin. . . . Witch Hazel, . . . 1- 3 Viburnin Prunif., Black Haw, 1- 3 Helonin, .... . False Unicorn, . . 2- 4 Xanthoxylin, . . Prickly Ash, .... 1- 2 * These drugs are subject to some variation, according to the manufacturer. CHAPTER XXXV II. FOR EXTERNAL USE. UNGUENTA—(Ointments'). Ointments are soft, unctuous preparations, composed of fats, generally medicated, which are applied to the skin by inunction. An ointment consists of medicinal agents combined with a base, which is generally of the consistence of lard. Base.—The U. S. Pharmacopoeia directs, in most instances, the use of benzoinated lard or simple ointment. Among other bases proposed and in use are petrolatum, wool-fat, diachylon oint- ment ; mixture of yellow wax (3 parts) and olive oil (7 parts), mixtures of such fats as spermaceti, suet or cacao-butter with almond oil; mixture of expressed oil of nutmeg (6 parts), olive oil (2 parts), yellow wax (1 part), etc. The three most popular bases, namely, benzoinated lard, wool-fat, and petrolatum, should not be used indiscriminately. Petrolatum is not adapted for use as an absorbent base. For this reason it should never be substituted where lard or wool-fat is directed. It answers as a bland neutral protective dressing. Wool-fat forms the best basis for dermal medication; it is more readily absorbed by the skin than lard, does not become rancid, and is miscible with aqueous solutions to the extent of its own weight. When inorganic salts are to be combined with it, they should be first dissolved in a little water, and then added to the wool-fat. Lard is not as readily absorbed by the skin as wool-fat, but owing to its cheapness, and the readiness with which it may be purified, it forms the most popular basis. It is often objection- able because of its tendency to rancidity; but, if properly purified and benzoinated, it can, with care, be kept almost indefinitely. Ointments, according to the method of preparation, are made either (1) \yy fusion, (2) by mechanical admixture, or (3) by chemical reaction. 1st. By Fusion.—In preparing ointments by fusion, those sub- stances which have higher melting points should be fused first, then the balance of the fats added, the whole strained, if necessary, well stirred, and, while it cools, such additional substances incor- porated as may be directed. The fats should be melted by the heat of a water-bath, and never directly over the flame. 2d. By Mechanical Admixture.—A large variety of substances are directed to be incorporated into ointments. The admixture may be accomplished either by trituration in a mortar or by 352 SOLIDS— FOR EXTERNAL USE. 353 working the materials, on an ointment slab,* with a spatula (Fig. 364). In handling such materials as iodine, corrosive sublimate, salicylic acid, tannic acid, etc., a steel spatula should not be used, but, in place of it, one of horn or hard rubber should be substi- tuted. When solids are to be incorporated, they should be first reduced to a very fine powder, then intimately mixed with a small portion of the fat, after which the remainder is gradually and thoroughly incorporated, until a perfectly homogeneous mixture is obtained. Solid extracts are first reduced to a smooth, thick paste by addition of a few drops of a solvent (water, alcohol, etc.), and rubbing in a mortar, or on a pill-tile with the spatula; then they are incorporated with the base, as directed above. When comparatively large amounts of dry powders are directed to be incorporated into an ointment, in order to prevent lumping, the powder should be triturated in a warm mortar with a portion of the melted fat. When this is reduced to a smooth, uniform paste, and the fat begins to cool, the balance should be added gradually, and the whole thoroughly mixed. Fig. 364. Ointment Spatula. Soluble salts, such as zinc sulphate, mercuric chloride, silver nitrate, etc., which are prone to crystallize, should be rubbed to a smooth paste with a little olive or almond oil before being incor- porated ; glycerin should not be used for this purpose. No more oil should be employed than is absolutely necessary. Very soluble or deliquescent salts, such as potassium iodide or carbonate, zinc chloride, etc., should be rubbed with a few drops of water. As exception to the above procedure, tartar-emetic should be mixed, in the state of a fine powder, directly with the ointment. Alkaloids should be first dissolved in a little oleic acid before being mixed with the base. Aqueous fluidsf should be combined slowly by trituration: alcoholic liquids are difficult to combine in ointments. If the active constituents in the alcoholic liquid are not volatile, it may be evaporated at a low temperature to the consistence of an extract, and then incorporated in the ointment. * A convenient substitute for this is the so-called Diamond Ointment Pad, made by Fox, Fultz & Webster, of New York. This consists of a block-pad made of parchment-paper, which is impervious to fats and liquids of all kinds. Immediately after use, the soiled leaf is torn off, thus saving the labor and time of cleansing. t Lard will take up mechanically and hold about one-fifth, Petrolatum about one-tenth, and Wool-fat about its own weight of aqueous fluid. 354 HANDBOOK OF PHARMACY. The quantities of fat should be weighed (waxed paper being used), and not guessed at. Immediately after the completion of an oint- ment, the mortar or slab should be cleansed by rubbing it with sawdust, the last traces of fat removed with paper, and the utensil afterward cleaned with soap-suds. 3d. By Chemical Reaction.—There is only one official ex- ample of this, namely, ointment of mercuric nitrate (page 355). PRESERVATION AND DISPENSING. Ointments should be kept in well-closed jars, in a cool and dark place. It is well to cover the surface of the ointment with paper impregnated with Tincture of Benzoin. Never dispense an ointment which has the slightest degree of rancidity. Fresh ointments should never be placed in a jar containing old ointment, even though there be but traces present. Ointments should be perfectly smooth and free from solid particles. Ointments should be dispensed in glass or porcelain jars (galli- pots), imparting a smooth finish to the surface of the ointment before dispensing. Before being refilled, the jars should be thoroughly cleansed. Wooden or lacquered pasteboard boxes should not be used, as the fat quickly penetrates and renders them unsightly. It is often necessary to mask the odor of certain medicinal agents. For this purpose Cumarin, Heliotropin, or the Oils of Rose, Geranium, Neroli, etc., are employed. Ointments of a firm consistence may be spread on linen and preserved in rolls, which forms a very convenient method of dis- pensing them. The U. S. Pharmacopoeia recognizes 23 ointments. Title. Per Cent, of Active Constituent. Base. Unguentum, Lard, 80 % ; Yellow Wax, 20 %. Acidi Carbolici, Carbolic Acid, 5 %. Unguentum. Acidi Tannici, Tannic Acid, 20 %. Benz. Lard. Aquae Rosse, Spermaceti, White Wax, Exp. Oil Almond, Stronger Rose Water, Sodium Borate. Belladonnas, Ext. Belladonna Leaves, 10 %. Benz. Lard. Chrysarobini, Chrysarobin, 5 %. Benz. Lard. Diachylon, Lead Plaster, Olive Oil, Oil Lavender fl. Gallae, Hydrargyri, Nutgall, 20 %. Benz. Lard. Mercury, 50 %. Lard and Suet. Hydrargyri Ammoniati, . Ammoniated Mercury, 10%. Benz. Lard. UNGUENTA, U. S. P. 355 SOLIDS—FOR EXTERNAL USE. Title. Per Cent, of Active Constituent. Base. Unguentum— Hydrargyri Nitratis, . . . Mercuric Nitrate, about Lard Oil. Hydrargyri Oxidi Flavi, . 121 %. Yellow Mercuric Oxide, Unguentum. Hydrargyri Oxidi Rubri, . 10 %. Red Mercuric Oxide, 10 %. Unguentum. lodi, Iodine, 4% (with KI). Benz. Lard. lodoformi, Picis Liquids?, Iodoform, 10%. Benz. Lard. Tar, 50 %. Yellow Wax and Lard. Pl unibi Carbonatis, . . . Lead Carbonate, 10%. Lead Iodide, 10%. Benz. Lard. Plumbi lodidi, Benz. Lard. Potassii lodidi, Potassium Iodide, 12 %. Benz. Lard. Stramonii, Ext. Stramonium Seed, Benz. Lard. Sulpburis 10 %. Washed Sulphur, 30 %. Benz. Lard. Veratrinae, Veratrine, 4 %. Benz. Lard. Zinci Oxidi, Zinc Oxide, 20 %. Benz. Lard. Unguentum Hydrargyri.—On triturating or agitating mer- cury with certain solids or fluids, it will be found that after a time the mercury gradually loses its metallic appearance and assumes a gray color. This mass, on close examination, will be seen to consist of globules of mercury in a very minute state of division. To accomplish this subdivision, or “ extinction,” as it is more properly called, a great variety of substances have been recom- mended, varying according to the use for which the mercurial preparation is intended; that is, internally or externally. The various substances employed act by enclosing each globule of mercury, as rapidly as separated, with a thin coat of material, which prevents it from reuniting with the rest; the presence of a trace of water causes the globules to unite again. Among the extinguishing agents are chalk, honey, fats, oleic acids, resinous tinctures, confection of rose, wool-fat, mercurial ointment, oleate of mercury, etc. Oleate of mercury, as recommended by the Pharmacopoeia, forms perhaps one of the best and most satisfactory extinguishing agents. The triturating should not be accompanied by pressure, but the motion should be light and rapid; then, as soon as the mercury has disappeared and a dull-gray colored magma is formed, the fused and partly cooled fats should be gradually added with continued trituration, until a portion, when spread out in a thin layer on a piece of white paper, does not reveal globules of mercury under a lens magnifying ten diameters. On the large scale this subdivision of the mercury is carried on by “ succussion ” in an apparatus operated by machinery, the mercury being extinguished by means of fused fats or powders. On long standing, mercurial ointment becomes slightly darker, owing to the oxidation of the mercury. Unguentum Hydrargyri Nitratis (Citrine Ointment).—By the action of nitrous acid or mercuric nitrate on the “ drying EXPLANATORY. 356 HANDBOOK OF PHARMACY. oils ” (olive, almond, lard, neatsfoot, etc.), the olein of the oil is converted into an isomer called elaidin, which is characterized by its yellow color and butyraceous consistence. The preparation of citrine ointment depends on the formation of this elaidin, which serves as a vehicle for the mercuric nitrate. The first step of the process is to heat the oil with a portion of nitric acid, which suffers reduction to nitrous acid. The latter, in turn, converts the olein into elaidin. Care should be taken not to raise the temperature above that directed (100° C.). The effervescence produced is not of a violent nature, but proceeds quietly and slowly, the liquid mass assuming thereby an orange (not brown) color. After the addition of the mercuric nitrate the mass should be stirred constantly until cold, by which time it will have assumed a semi-solid consistence and a bright lemon-yellow color. Over- heating causes the ointment to assume a brown color. Either a horn, porcelain, or wooden spatula should be employed for stirring, because of the readiness with which mercuric nitrate attacks metals. SOLIDS—FOR EXTERNAL USE. 357 CER ATA—(Cerates). Cerates (cera, wax) are a class of preparations similar to oint- ments, but of a firmer consistence. They are made by mixing oil or lard with wax, or some other substance having a higher melting point, imparting to them a consistency between that of an ointment and plaster. When applied to the skin they do not melt like ointments, but retain their soft consistence. The materials selected (oil or lard) should be free from all traces of rancidity. The wax or materials of higher fusing point should be first melted on a water-bath, then the oil or lard added in portions; when all is liquefied, the fluid should be stirred constantly while cooling, and those portions which congeal on the sides of the vessel re-incorporated until the whole assumes the proper con- sistence. Cerates should be kept in a cool place, in clean and well-covered jars. Those made with white wax, owing to its incipient rancidity, are liable to become rancid, while those containing yellow wax keep unaltered. Cerates are employed chiefly as dressings for inflamed surfaces. Steatins*—These are a class of preparations which have the consistence of cerates, and contain suet combined with wax or lead plaster as base. The U. S. Pharmacopoeia recognizes 6 Cerates. Title. Composition. Ceratum, White Wax, 300 Gm.; Lard, 700 Gm. Ceratum Camphorse, Camphor Liniment, 100 Gm., White Wax, 300 Gm.; Lard, 600 Gm Ceratum Cantharidis, Cantharides pulv., 320 Gm. ; Yellow Wax, Blistering Cerate, 180 Gm.; Resin, 180 Gm.; Lard, 220 Gm.; Oil of Turpentine, 150 Cc. Ceratum Cetacei Spermaceti, 100 Gm.; White Wax, 350 Gm.; Spermaceti Cerate, Olive Oil, 550 Gm. Ceratum Plumbi Subacetatis, . . Solution of Lead Subacetate, 200 Gm.; Cam- phor Cerate, 800 Gm. Ceratum Resinse, Resin, 350 Gm.; Yellow Wax, 150 Gm.; Lard, Basilicon Ointment, 500 Gm. CERATA. ., U. S. P. * Proposed by Mieleke, Phar. Centralhalle, 1881, Nos. 20-21. 358 HANDBOOK OF PHARMACY. EM PLASTR A—{Plasters). Plasters are compounds of various fusible solids of a melting point higher than that of the human body, being friable when cold, but rendered adhesive by the warmth of the body. Accord- ing to the base employed, they may be designated as Plasters proper, or as Resinous Plasters. Emplastrum Plumbi forms the base of the former class, while the latter consist of various combinations of resins. The Pharmacopoeia recognizes two ready-spread plasters, namely, Emplastrum Ichthyocollae and Emplastrum Capsici. In the preparation of plasters, care should be taken that no higher degree of heat be employed than that of the water-bath, otherwise decomposition of the volatile medicinal constituents might ensue. Some plasters are made by simply fusing the various constitu- ents together; others require the admixture of various solids, which are added to the fused mass either in a state of fine powder, or in the condition of a smooth paste obtained by treatment with a proper solvent. While cooling, the mass should be well stirred to insure uniformity in composition. After preparation, the plaster mass is usually moulded * into sticks or rolls, and wrapped in waxed or paraffin paper. When kept for some time the plaster mass becomes hard and brittle, due to the oxidizing influence of the air; it may be restored to its original plasticity by re-melting it, with the addition of a little oil. Owing to the introduction of the rubber base, the preparation of plasters has almost entirely fallen into the hands of the manu- facturer; it is seldom that the dispenser is required to spread other than cantharides plaster. Spreading of Plasters.—Plasters are usually spread on either muslin or leather (sheepskin), which is cut to the necessary size Fig. 365. Plaster Spatula. and shape, from one-quarter to one inch being allowed all around for a margin. The piece of leather or muslin is then stretched * The Plaster-press, as shown in Fig. 355, page 321, is adapted for this purpose. SOLIDS—FOR EXTERNAL USE. 359 evenly on a smooth surface, being held in position by means of thumb-tacks. Over this is laid the form (Fig. 366), made of thin card-board or heavy paper, cut of the desired shape and size, and this is secured firmly by means of thumb-tacks. Fig. 366. Forms for Spreading Plasters and Cerates. Plasters of an ointment like consistence (like Emp. Cantharidis) may be readily spread in a cold condition by means of a spatula. The plasters proper, because of their friable nature, are first melted and then spread with a hot spatula.* Sufficient of the Fig. 367. Fig. 368 Plaster Block. Plaster Iron. plaster-mass (for the surface required) is selected and cautiously melted in a porcelain capsule over a gas-flame; the melted mass is then allowed to cool until it is of a honey-like consistence and, * The form shown in Fig. 365 is specially designed for this purpose. 360 HANDBOOK OF PHARMACY. by means of a warm spatula blade, quickly and evenly spread over the surface. The mass should not be applied too hot, other- wise it will penetrate the leather or muslin. After the plaster is spread, the surface should appear even and smooth; if it is not, a hot spatula should be quickly passed over it. Care should be taken, while heating the blade, to remove all particles of plaster adhering to it, otherwise the surface of the plaster will become discolored. Before removing the paper, or cardboard frame, the hot edge of the spatula should be passed around the line of con- tact, so that, when the frame is removed, a smooth, sharp edge may be left. For spreading larger numbers of plasters, the operation may be facilitated by the employment of the plaster-block (Fig. 367). This consists of a rectangular block of hard wood, the upper sur- face of which is convex. To one end of the upper surface is attached, by means of a hinge, a sheet-iron frame with an opening of the size desired for the plaster. The muslin or leather of proper size is laid on the convex surface of the block; over this is secured the sheet-iron frame, then the necessary amount of melted and partly-cooled plaster is poured in the center, and by means of a heated (triangular-shaped or round) plaster iron (Fig. 368), it is spread uniformly over the surface, the excess of plaster being forced over on the edges of the frame. Perforation of Plasters.—This is done to permit the escape of exhalations from the skin, also to enable the plaster to adapt Fig. 369. Plaster Perforating Machine. itself better to the skin, and to adhere more firmly. Perforation of plasters is carried on by the manufacturers of plasters on the large scale, by means of specially constructed machinery. For SOLIDS—FOR EXTERNAL USE. 361 the use of the apothecary the perforating machine of Lentz is par- ticularly adapted (Fig. 369). An inexpensive perforating appara- tus has been devised by Professor Remington (Amer. Jour. Phar., 1878, p. 171), which consists of a brass cylindrical wheel studded with steel punches, which is driven with some force across the sur- face of the plaster, resulting in perforating along the line of contact. The employment of a rubber mass, as a base, has practically superseded all others. Its advantages reside in its flexibility and adhesiveness at ordinary temperatures, and in its not requiring any heat in applying or removing. This base consists essentially of a mixture of rubber with certain resins (burgundy pitch and olibanum), variously medicated. This pliable and adhesive rubber base retains its soft consistence indefinitely, and yields its medici- nal constituents readily when applied to the skin. EXPLANATORY. Emplastrum Plumbi (Lead Plaster).—When fats are treated with alkali hydrates or with a number of other metallic oxides, decomposition takes place, the fatty acids combining with the metals forming soaps, while the glycerin is set free. Those soaps whose base is either soda or potassa, are known as the “ soluble,” while those whose base constitutes a metallic oxide, are known as “ insoluble ” soaps. To this latter class Lead Plaster belongs. It may be prepared in either of two ways, viz.:— 1st. By the interaction between soluble soaps and lead salts, (page 287). NaC18H33O2 | p. /C2H3O2 — NaC18H33O2 + rD\C2H3O2 “ rD\CI8H33O2 Sodium Oleate. Lead Acetate. Lead Oleate. 2d. By the process of saponification * (U. S. P. process). 2C3H5(C18H33O2)3 + 3PbO + 3H2O = 3Pb(C18H,,O2)2 + 2CSH5(OH)3 Olein (Olive Oil). Litharge. Water. Lead Oleate. Glycerin. Any oil which consists of nearly pure olein may be used for this purpose. The U. S. Pharmacopoeia recognizes 13 Plasters. EMPLASTRA, U. S. P. Plasters Containing Emp. Plumbi as Base. Emplastrum Ferri, “ Hydrargyri, . . “ Opii, Ferric Hydrate, 90 Gm.; Olive Oil, 50 Gm.; Burgundy Pitch, 140 Gm.; Lead Plaster, 720 Gm. Mercury, 300 Gm.; Oleate of Mercury, 12 Gm.; Lead Plaster, sufficient quantity, to make 1000 Gm. Ext. Opium, 60 Gm.; Burgundy Pitch, 180 Gm.; Lead Plaster,760Gm.; Water, 80 Gm. * In the restricted sense, as employed here, saponification is the separation of fats into their respec- tive acids and glycerin. Here, the fatty acids are liberated by the action of the litharge (in the presence of water)', uniting with the lead and separating out as an Insoluble soap. 362 HANDBOOK OF PHARMACY. Plasters Containing Emp. Plumbi as Base.—Continued. Emplastrum Plumbi, .... “ Resina), .... “ Saponis, .... Lead Oxide, 3200 Gm.; Olive Oil, 6000 Gm.; Water, sufficient quantity. Resin, 140 Gm.; Lead Plaster, 800 Gm.; Yellow Wax, 60 Gm. Soap, 100 Gm.; Lead Plaster, 900 Gm.; Water, sufficient quantity. Plasters—Resinous. Emplastrum Ammoniaci cum Hydrargyro, . “ Arnicse, .... “ Belladonnas, . . “ Picis Burgundicae, “ Picis Canthari- I datum, ... I Ammoniac, 720 Gm.; Mercury, 180 Gm.; Oleate of Mercury, 8 Gm.; Dilute Acetic Acid, lOOOCc.; Lead Plaster, sufficient quantity. Ext. Arnica Root, 330 Gm.; Resin Plaster 670 Gm. Ale. Ext. Belladonna Lvs., 200 Gm.; Resin Plaster, 400 Gm.; Soap Plaster, 400 Gm. Burgundy Pitch, 800 Gm.; Olive Oil, 50 Gm.; Yellow Wax, 150 Gm. Cantharides Cerate, 80 Gm.; Burgundy Pitch, to make 1000 Gm. Plasters—Spread. Emplastrum Capsici, .... Ichthyocollae, . Oleoresin of Capsicum; Resin Plaster. Isinglass, 10 Gm.; Alcohol, 40 Gm.; Gly- cerin, 1 Gm.; Water, and Tincture of Benzoin, each, sufficient quantity. The official Papers consist of paper saturated or covered with medicinal substances. The Pharmacopoeia recognizes only two of these medicated papers. Charta Potassii Nitratis.—This consists of white unsized paper saturated with a solution of potassium nitrate. It is em- ployed in cases of asthma, by burning it, and inhaling the smoke. It is often saturated with fluid extract of belladonna or of stramonium. Charta Sinapis.—The fixed oil present in the black mustard is first removed by percolating with benzin. The solution of india rubber serves as an adhesive coat, firmly retaining the pow- der. The irritating properties of the powdered black mustard depend upon the generation of a vesicating volatile oil, which takes place when the powder is moistened with water. This volatile oil is formed through the decomposition of a glucoside called sinigrin (potassium myronate), caused by the influence of an albuminous ferment myrosin, which does not enter the reaction itself; the reaction being thus:— c10h18kns2o10 = c3h5cns 4- khso4 + c6hI2o6 Sinigrin. Allyl Sulphocyanate Acid Potassium Glucose. (Potassium (Oil of Mustard). Sulphate. Myronate). CIIA RTzE—(Med tea ted Pape rs). SOLIDS—FOR EXTERNAL USE. 363 Hot water causes coagulation of the albuminous ferment, hence no oil will be produced; only lukewarm or cold water should be used to moisten the drug. SUPPOSITORIA—(Suppositories). Suppositories are suitably-shaped masses of medicated fats, which readily fuse when introduced into the body. According to their size and shape, there are three forms, namely, the Rectal (cone-shaped) which should weigh about one gramme (U. S. P.), but which may also be made to weigh as much as two grammes; the Urethral (pencil-shaped) should weigh about one gramme (U. S. P.); the Vaginal (globular or cone-shaped) should weigh about three grammes (U. S. P.), but may also be made to weigh over four grammes. Suppositories are sometimes given a double cone-shape, that is, pointed at both ends. The usual cone- and double cone-shaped suppository is sometimes difficult of retention, because of the peculiar contraction of the sphincter muscles; in view of this, Wellcome (August, 1893) sug- gested a modification of their shape, which, allowing the introduc- tion of the bulbous end first, ensures perfect retention,by the reflex contraction of the sphincter. The base employed should be of such con- sistence as to retain its shape at the ordinary temperature of the air, yet it should be sufficiently soft not to produce any injury on insertion. It should not become rancid and yet be capable of being mixed with most medicinal substances without any lowering of its fusing point. The various bases employed may be designated as fatty (cacao butter), saponaceous (curd soap from animal fat), and gelatinous-, neither of the latter, however, give the general satisfaction that is obtained from the use of cacao butter. The Gelatin Base forms a valuable and service- able substitute where objections are made to a fatty basis. Accord- Fig. 372. Fig. 370. Suppositories (Rectal). Fig. 371. Wellcome’s Improved Suppository. Wellcome’s Improved Bougie. 364 HANDBOOK OF PHARMACY. ing to theory, it is not adapted for administering tannic acid, since they are supposed to form an insoluble compound. These gelatin suppositories are more readily made than those of cacao butter, but present the difficulty of lacking firmness. They are made by moulding. For this purpose the moulds must be thoroughly cleaned and dried, then wiped inside with a piece of flannel impregnated with oil. The base is fused in a capsule on a water- bath, the medicinal ingredients dissolved in a little water and stirred in until thoroughly diffused or dissolved. When of proper degree of consistence the mass is poured into well cooled moulds. The same mass is not applicable to all medicaments, since some render it too hard, others too soft. The gelatin base may be kept almost indefinitely, provided it is poured into bottles and, when cold, covered with alcohol. The following gelatin bases * have been proposed : — I. Gelatin 10 parts, water 40 parts, glycerin 15 parts; evapo- rate to 25 parts. This combination is suitable for hygroscopic drugs, for bougies containing ferric chloride (dissolve 1 part of ferric chloride in 9 parts of water and add to 19 parts of the mass), for tannin suppositories (0.2 per cent.,—not in accordance with theory), and for vaginal pessaries containing such salts as potas- sium iodide or bromide, sodium bromide or salicylate, ergotin, chloral hydrate, etc. II. Gelatin 10 parts, water 40 parts, glycerin 20 parts; evapo- rate to 50 parts. A good base for general use. Phenol or such substances as are soluble in alcohol are first dissolved in a little alcohol, added to 7 parts of glycerin and 50 parts of this mass. Alum bougies are made by adding a hot solution of 7 parts of alum in 10 parts of glycerin, and 5 parts of water to 25 parts of the mass liquefied on a bath with 10 parts of water. The whole is evaporated, under stirring, to 35 parts. III. Gelatin 10 parts, water 40 parts, glycerin 30 parts; evaporate to 60 parts. This mass is adapted as a vehicle for such substances as cupric or zinc sulphate, silver nitrate, extract of opium, mercuric chloride, etc. IV. Gelatin 30 parts, water 120 parts, glycerin 15 parts ; evap- orate to 104 parts. A basis for bougies containing a large per- centage of insoluble drugs. Iodoform bougies (50 per cent.) are made by adding 27 parts of pulverized iodoform to 27 parts of the mass. For a glycerin suppository,)" the following has been recom- mended; glycerin 10 parts, water 5 parts, gelatin 1 to 2 parts ; in order to render the suppositories sufficiently firm, it has been recommended to dip them into melted cacao butter. Cacao Butter Suppositories.—According to their method of * C. H. Oehse, “ Art of Dispensing,” Chemist and Druggist, London. t 'Phis was proposed previous to the appearance of the U. S. P. of 1890, in which “ Suppositoria Glycerini,” made by another process, were made official. SOLIDS—FOR EXTERNAL USE. 365 preparation they may be designated as hand-rolled, moulded, and compressed. Hand-rolled.—The method of forming by hand is very simple, the operation being carried out much in the same manner as that of making a pill mass. The Cacao butter is grated and weighed ; the medicinal agents are reduced to a fine powder in the mortar, or, if they consist of extracts, they should be moistened with a little water and rubbed to a smooth paste; to this is added the cacao- butter and the whole thoroughly incorporated and beaten into a pill mass. In order to impart plasticity, a few drops of castor or olive oil are often added. The mass is then rolled out on a pill tile into a cylinder of the desired thickness and length, finely powdered starch being employed as dusting powder. The cylin- der is then divided into the necessary number of parts, and by carefully rounding one end by rolling on the tile with the spatula or by forming between the fingers, the desired shape is imparted. The hands and all utensils must be kept scrupulously clean. A rusty spatula or a poorly cleansed tile is sufficient to ruin the appearance of the most carefully made suppository. Sometimes, through lack of adhesiveness, the mass crumbles when rubbed. It should then be worked over in the mortar with addition of a drop or two of oil if necessary, and formed into a cylinder with the hands, with sufficient rapidity to avoid undue softening of the mass. Also care should be taken not to incor- porate too much of the dusting powder in the operation of rolling out the cylinder, otherwise the mass will crumble, from lack of adhesiveness. Moulded Suppositories.—The directions of the Pharmacopoeia are as follows:— Take of The Medicinal Ingredient, the prescribed quantity. Oil of Theobronia, a sufficient quantity. Having weighed out the medicinal ingredient or ingredients, and the quantity of Oil of Theobroma required, according to the kind of Suppository to be prepared, mix the medicinal portion (previously brought to a proper consistence, if necessary) with a small quantity of the Oil of Theobroma, by rubbing them together, and add the mixture to the remainder of the Oil of Theobroma, previously melted and cooled to the temperature of 35° C. (95° F.). Then mix thoroughly, without applying more heat, and immediately pour the mixture into suitable moulds. The moulds must be kept cold by being placed on ice, or by im- mersion in ice-cold water, before the melted mass is poured in. In the absence of suitable moulds, Suppositories may be formed by allowing the mixture, prepared as above, to cool, care being taken to keep the ingredients well mixed, and dividing the mass into parts, of a definite weight each, of the proper shape. 366 HANDBOOK OF PHARMACY. Unless otherwise specified, Suppositories should have the fol- lowing weights and shapes, corresponding to their several uses:— Rectal Suppositories should be cone-shaped, and of a weight of about one (1) gramme. Urethral Suppositories should be pencil-shaped, and of a weight of about one (1) gramme. Vaginal Suppositories should be globular, and of a weight of about three (3) grammes. Insoluble substances, when forming the constituents of a sup- pository, should be reduced to a very fine powder; solid extracts should be rubbed with sufficient water to form a smooth paste. This latter point should be carefully observed, because the solana- ceous extracts generally contain numerous minute crystals of potassium nitrate and chloride,which prove very irritating wffien allowed to remain in crystalline condition. Care should be taken not to heat or to continue heating the melted mass after the medicinal ingredients are added, otherwise they will separate in a solid mass from the fused fat. The medi- cinal ingredients are simply in a state of suspension, hence they should be added just before the mass cools, when the cacao- butter is of a syrupy consistence; after these have been added, the mass should be constantly and vigorously stirred, while it is poured into the moulds, otherwise the medicinal constituents will be unevenly distributed, the last suppository receiving more than the others. The moulds should be as cold as possible, so as to secure rapid congelation of the mass, thereby preventing the heavier particles from settling to the bottom. If the moulds are properly cleansed and cooled, the suppository will shrink sufficiently to enable the operator to remove it without any difficulty, hence there is no occasion for the use of dusting powder. Some operators prefer to wipe out the moulds with a piece of flannel moistened with soap liniment. MOULDS. The simplest moulds may be made by rolling glazed or waxed paper into cones of the proper size, placing them into sand or supporting them in holes made in a cardboard box. Among the older forms of moulds are those made of white metal (Fig. 373, c), which are supported in perforations in the lid of a tin box filled with crushed ice or snow. The suppositories are removed from these moulds by inverting them and tapping; after the moulds have been in use some time, which renders them rather difficult to clean properly, particles of the mass are apt to remain adhering to the inside, which tends to interfere with the subsequent removal of the suppositories. The moulds a and b (Fig. 373), are improvements over the first- SOLIDS—.FOR EXTERNAL USE. 367 named form in that they are composed of two distinct parts, which greatly facilitates the removal of suppositories and the subsequent cleaning of the mould. In the form shown in b, the two halves are held in position by means of a rubber band; while in the Wirz mould (Fig. 373, a), the halves are held firmly in position by rings, which are slipped over the handles. The so-called hinged, double Fig. 373. Suppository Moulds. mould of gun metal (Fig. 373, d), because of its compactness and the close fitting of its parts, is one of the most convenient forms made; this is usually so constructed as to accommodate two different sizes of suppositories. The moulds shown in Figs. 374 and 375 are constructed on this same principle, but instead of FIG. 374 Fig. 375. See’s Suppository Mould. Blackmann’s Suppository Mould. opening perpendicularly, as the others, they open horizontally. These forms of moulds have the advantage of size and compact- ness of shape. After the mass has been poured into the mould, ample time should be allowed for the suppositories to contract; then, if on pressing them slightly on top they show that they are 368 HANDBOOK OF PHARMACY. sufficiently loose, the upper half or inside ring of the mould should be carefully detached by raising it equally on all sides, otherwise there would be danger of fracturing the suppositories. Compressed Suppositories.—The preparation of suppositories by the process of melting and moulding is at present being sup- planted by the method of cold compression. This possesses not only the advantage of rapidity, but also yields a perfect, compact suppository at all times without the use of ice. As before stated, some organic bodies, for instance chloral, creosote, phenol, volatile oils, etc., when warmed with cacao-butter, influence its melting- point to such a degree that the mass refuses to harden. This difficulty also arises when they are made cold by hand. Among the earlier forms of these cold-pressure moulds is that devised by Archibald. This is operated by placing the mixture of grated cacao-butter and medicinal substances in a hopper, where the mass is then forced by means of a plunger, operated by a handle-lever, into the mould below. The objection to this form of apparatus is that the removal of the suppositories from the mould is necessarily slow and attended with difficulty. More- over, in order to avoid the fracture of the suppositories, the moulds must be kept very cold and well greased or dusted, so as to pre- vent the mass from adhering to the sides. The necessity of filling the hopper each time is also not a point in favor of this apparatus. These difficulties have all been overcome in the later forms, which are based on the principle of forcing the entire mass, con- tained in a cylinder, under a powerful pressure, by means of a plunger operated by a screw, through small apertures in the bottom of the brass mould secured into the end of a cylinder; the end of the mould resting against a movable plate. One of the older forms constructed on this principle is the mould made by Mr. Knowlson of Troy, N. Y. A later machine of similar construction is shown in Figures 376 and 377. This consists simply of a cylinder swinging in a frame, in which the mould is placed with the small holes up. The mass, previously prepared, is thrown into this cylinder, which at this time is open, as in Fig. 376. The cylinder is then closed, and the screw pressure is applied until all resistance is overcome. Before opening the bed-plate, the screw should be loosened by half a turn, then the bed-plate thrown back (see Fig. 377) and the screw again gently turned downward until the suppositories drop out. After these are secured, the bed-plate is closed and the operation repeated, until the cylinder is emptied of the mass. The small cylindrical pieces which force the suppositories from the moulds, should, of course, be returned to the cylinder at the last working, for conversion into suppositories. In making Urethral or Nasal Suppositories, remove the cap at No. 2, Fig. 377, and screw on the small tube, taking care to have a mould in the cylinder covered with a brass disc, which is SOLIDS—FOR EXTERNAL USE. 369 furnished. The mass is then simply put into the cylinder as be- fore, pressure applied, and the suppositories cut into any length desired. Fig. 376. Fig. 377. When Suppositories are ordered, it is at the option of the Phar- macist to employ either cacao butter, grated on a lemon grater, Perfection Suppository Machine. Fig. 378. Suppository Machine (W., T. & Co.’s). with the extracts in a state of powder, and by means of a slab and spatula to thoroughly incorporate the cacao and extracts to- gether, then to throw the material into the cylinder and to use the screw; or he may take the cacao butter as ordinarily sold in 370 HANDBOOK OF PHARMACY. the market, and work it in with the extracts in the same manner that a pill mass is made, taking care to thoroughly diffuse the active ingredient, and when they are thoroughly mixed to throw the mass into the cylinder, and to operate the screw to compress the suppository. Another new machine is illustrated in Fig. 378. This is of simple construction and easily and quickly operated. Each machine is furnished with a set of moulds for making suppositories of three sizes—15-grain, 30-grain, and vaginal—and with a mould for forming bougies. These moulds are of brass and are screwed into the end of the cylinder. They can be easily and rapidly inserted or removed. In making suppositories the cacao butter mixed with the medi- cinal substance is placed in the cylinder, the mould required being first attached, and the cylinder is put in position with the end of the mould resting against the movable plate at the end of the machine. The mass is then compressed in the forms by turning the wheel and screwing the plunger into the cylinder. After the sup- positories are formed, the end plate is re- moved, and a further turn of the wheel forces them out upon the tray. The operation is then repeated until all the mass has been used. By a special device, the screw on the plunger rod may be released so that the plunger may be pushed into the cylinder or withdrawn from it without the slow process of screwing. BOUGIES are solid cylindrical rods of 2 to four millimeters diameter and from 7 to 15 cen- timeters long, pointed atone end and weighing about one gramme. These are formed by hand, or in special moulds or may be made by cold pressure (Fig. 379). In the absence of moulds they may be moulded by pouring the mass into glass tubing of the proper size (oiled inside). When cold, they are forced out by means of a glass rod, then cut into pieces of the desired size, and pointed at one end. Owing to the brittle nature of the cacao butter,* they are generally made of gelatin. H. Helbingf recommends the following:— “ Gelatin Mass is best prepared from 10 oz. best gelatin, 16 oz. Fig. 379. Bougie Press, * The following formula is proposed by N. Pritzker:— Cacao butter, grains 480 Powd. acacia “ 240 Water, min. 240 Glycerin, “ 120 Po’wd. boric acid sufficient. Melt the cacao butter and triturate it in a warm capsule with the acacia, and add the water previously mixed with the glycerin ; place the capsule in cold water or on ice until the mass has solidified, and set the vessel aside. When required for use, take of the above four drachms, incorporate it with the medicaments and with from 10 to 25 per cent, cacao butter, triturate until intimately mixed, and roll out into 10 bougies. f Proceed. Amer. Phar. Ass’n., 1889, p. 402. SOLIDS—FOll EXTERNAL USE. 371 best glycerin, and sufficient water. The gelatin is dissolved in sufficient water and the glycerin by the aid of a water-bath in a porcelain dish, the water lost by evaporation being compensated for by the addition of more. The ingredients, if not soluble in water, are mixed in a finely powdered condition with the warm and tenacious glue, and the pencils are moulded in moulds simi- lar to those used for making caustic, previously moistened with oil or soap liniment. When cold they are quite elastic, but not sticky. 11 Iodoform Pencils, 33 per cent.—Iodoform, 1 part; cacao butter, 2 parts. “Cocaine Pencils, 2 per cent.—Cocaine hydrochlorate, 1 part; cacao butter, 49 parts. To be cut in pieces containing | grain of the cocaine salt each. “Salol Pencils, 20 per cent.—Dissolve 1 part of salol in 4 parts of the liquefied cacao butter, stir constantly until cool, powder the mass, and form cylinders by the aid of the press. “Opium Pencils, 5 per cent.—Powdered opium, 1 part; cacao butter, 19 parts. Divide into sticks containing 1 grain of opium each. “Thallin Pencils, 5 per cent.—Sulphate of thalline, 1 part; cacao butter, 19 parts. “Mercurial Pencils, 25 per cent.—Made with equal parts of mer- curial ointment and white wax, previously melted. When cool the pencils are pressed out. The following elastic pencils may be made with a mass containing tragacanth, starch, etc.:— “Iodoform Pencils, 33 per cent.—Iodoform, 5j; starch, 5iij ; tragacanth, 5j ; dextrin, 5j; sugar, §ss; water and glycerin, each sufficient. “Salicylic Acid Pencils, 5 per cent.—Salicylic acid, 5j; traga- canth, 5j; starch, 5j; dextrin, 5vij; sugar, 3iij; water and glycerin, each sufficient. These pencils may be polished, if desirable, by rolling them on a porcelain slab with a thin board. “ Urethral Pencils.—Urethral pencils, retaining their shape for some hours, are prepared from cacao butter, 6; beeswax, 5; boric acid (or iodoform, etc.), 2; zinc oxide, 1; and tragacanth, 4 parts. These pencils possess a certain degree of elas- ticity, and are prepared of a conical form. “Caustic Pencils—Dr. De Sinety’s.—Crystal- lized phenol, 0.05 Gm.; tannin, 4.0 Gm.; gly- cerin, 5 drops; tragacanth sufficient.” Suppository Capsules.—These consist of gelatin shells which are filled with the medi- cinal substance, or with a mixture of it and cacao butter. The upper and outer margin of the lower half is moistened with water and the cap slid over it, so as to prevent the two halves from coming apart in handling. Before they are inserted, they should be dipped in water so as to enable them to slip in easily. Fig. 380. Gelatin Suppository Capsules. 372 HANDBOOK OF PHARMACY. Hollow Cacao Butter Suppositories.—These are very con- venient for the dispenser and answer quite well when the medi- cating ingredient is of a neutral nature, but they should never be used when the remedy is in any degree locally irritating. The main object of employing an excipient (cacao butter or gelatin) Fig. 381. Hollow Cacao Butter Suppositories, in a suppository is to secure slow and uniform diffusion of the remedy. The medicinal substance should be well mixed with a little grated cacao butter before it is filled into the cavity, which is then closed by the plug provided for this purpose. Fig. 382. Hollow Cacao Butter Suppositories. GENERAL REMARKS. Suppositories are usually dispensed in partitioned paper boxes, or in wide-mouthed vials. The practice of wrapping them in paraffin paper or foil is not advisable, owing to the possible SOLIDS—FOR EXTERNAL USE. 373 ignorance of many patients, who might use them without removing the wrapper. As in the case of pill masses, the medicinal ingredients should always be thoroughly incorporated with the mass before it is moulded. When such heavy salts as potassium iodide or bromide, or lead acetate are directed to be incorporated in suppositories, they should be made by hand or by cold compression. For, when they are made by the process of fusing, even with the greatest of care and skilled manipulation, the salts, owing to their gravity, will settle and collect at the point of the suppository, which is not only disagreeable but may be dangerous to the patient. For this class of remedies, the gelatin basis is the most advantageous, since the inorganic salt may previously be dissolved in a portion of the water. When iodine is directed to be incorporated in a suppository it should be first powdered with a little potassium iodide, then dis- solved in a small amount of water and added to the gelatin basis. Alkaloids (that is, free alkaloids), should be dissolved in a little oleic acid before being combined with the cacao butter. Green Extracts and Tannin.—When such extracts as those of belladonna, stramonium or hyoscyamus are prescribed with tannin, the suppositories should be made by cold pressure. It is possible, with due care, to prepare these by the warm process; the extract, after having been reduced to a smooth paste with a little water, is combined with the melted fat, then, when the mass is sufficiently cool and ready to pour, the tannin is quickly stirred in. But the slightest degree of overheating causes the tannin to unite with the extract, forming hard lumps. Wax, owing to its high fusing point, should never be added to a suppository mass in any quantity. Suppositoria Glycerini, U. S. P.—This is the only official suppository. It is made by heating stearic acid, glycerin, and sodium carbonate together until effervescence ceases, then pour- ing into moulds. The reaction that takes place results in the formation of sodium stearate, a very hard soap:— 2HC18H35O2 + Na2CO3 = 2NaC18H33O2 + H2O + CO2 Stearic Acid. Sodium Sodium Stearate. Water. Carbon Carbonate. Dioxide. This with the large amount of glycerin present (90 per cent.) forms a firm, stable suppository. According to Thumann * these may also be made from cacao butter rendered liquid at 35° C. and agitated with an equal weight of warmed glycerin (50 per cent.) until the mixture begins to solidify, when it is poured into moulds. Owing to the hygroscopic nature of these glycerin suppositories, they should be dispensed in wide-mouthed vials or glass tubes which are securely corked and sealed. * American Journal of Pharmacy, 1893, p. 368. PART III. CHAPTER XXXVI. THE ART OF DISPENSING. THE PRESCRIPTION. A prescription is a written formula of remedies, with directions to the apothecary for their preparation, and instructions for the guidance of the patient or of his attendant. The word prescription is derived from the Latin word prsescrip- tio, title; order; ordinance, etc., from preescribo “ to write before; to ordain.” For writing prescriptions, the Latin language is almost univer- sal, because, being a language of science, it is generally understood in civilized countries. And being a dead language, it is not sub- ject to the various changes peculiar to modern tongues.* More- over, for various reasons, it is not advisable, as a rule, that the patient be aware of the kind and nature of the remedies admin- istered. The prescription consists of the following parts, thus classi- fied:— (1) The Superscription, . R. (2) The Inscription,Remedy (genitive) ; Quantity (accusative). Repeat for each constituent. (3) The Subscription,Misce (directions to compounder). (4) The Signature,Signa (directions for the patient). (5) This is generally followed by the name of the patient, f and always by the name or initials of the prescriber, with date. 1st. The Superscription (superscribo — to write on top) or Head- ing. The symbol is usually placed at the head of every prescrip- tion. The letter R stands for the Latin word Recipe, the imperative mood of the verb recipio, il to take.” When the prescription is written in English, this letter R is replaced by the words “ take of”; in French, it would be replaced by a P (abbreviation for prenez, take); in German, it would be replaced by the word “nimm” (take). ♦Vernacular names in various languages may vary in different parts of the same country, and are often unintelligible to foreigners. Hence a prescription written in the native language in one part of the country may be unintelligible in another part. f Also written in the upper corner of the prescription. 375 376 HANDBOOK OF PHARMACY. The sign according to some, is derived from the symbol if, the zodiacal sign for the planet Jupiter. In ancient times, it was customary to invoke the blessings of the deity, Jupiter or others, on the remedies to be taken, by a formal prayer at the beginning of the prescription. This was, in time, contracted to simply plac- ing the sign of the respective deity addressed at the head of the prescription. 2d. The Inscription (inscribe = to write upon) includes the names and quantities of the various ingredients. These ought to be arranged, if possible, in a definite manner, somewhat after the following plan :— The Basis—the principal active agent. The Auxiliary (adjuvant)—the ingredients which aid or promote the action of the Basis. For example, the combination of chloral and potassium bromide is more certain as an hypnotic than either alone, hence, while chloral is placed first, potassium bro- mide follows as an auxiliary. With cathartics, the auxiliary, while assisting the action of the base, renders it more manage- able, lessening its liability to irritate, as for example the ad- juvant Myrrh, when combined with Aloes. In conjunction with Quinine, the adjuvants Capsicum and Opium are often pre- scribed for breaking up intermittent fevers. The Corrective.—The ingredient which corrects or modifies the action of the first. For example, the griping tendency of many purgatives is usually overcome by combining them with aro- matics. The Vehicle (excipient or diluent). — The ingredient which assists in imparting proper form, and also in diluting the active constituents. Example. R. Aloes Purificatae, 2 Gm. (ftose). Myrrhae, 1 Gm. (adjuvant). Pulveris Aromatici, 5 Gm. (corrective). Extract! Gentianae, q. s. (excipient). Fiat massa ; divide in pilulas xvi. or R. Quininae Sulphatis,gr. xx (base). Ferri et Ammonii Citratis, .'gr. xl (adjuvant). Acidi Citrici,gr. x (excipient). Syrupi Limonis,fl,?j (vehicle). Aquae purae, . . q. s. ad. fl 5 ij (diluent). Misce. GRAMMATICAL CONSTRUCTION.* The following example is selected as an illustration of Latin construction, as applied in prescriptions: * Only the briefest outlines can be given here. The reader is referred to special text-books, such as Robinson’s Latin Grammar, or “The Prescription,” by Wall. Consult, also: “The Latin Gram- mar of Pharmacy ; ” by Joseph Ince, London. 377 THE ART OF DISPENSING. R. Quininae Sulphatis,drachmam unam (3j) Tincturae Cinchonae Compositae,uncias duas Glycerini,unciam unam et semis- sem (3 iss) Acidi Sulphurici Diluti,quantum sufficiat (q. s.). Aquae,q. s. [quantum sufficiat] ad uncias quatuor (ad £iv). Recipe; Quininae Sulphatis drachmam unam. Take thou of Quinine Sulphate drachm one. K is the symbolic abbreviation for recipe, the imperative mood of the active verb, recipio, recepi, receptum (3d con- jugation), meaning “to take;” its object is drachmam, the accusative singular of drachma, ae; unam is the accusative singular of the adjective unus, a, um, which agrees with drachmam. Thus we have, “take one drachm,”—of what? of sulphate of quinine. This is put in Latin in the genitive (possessive case in English); sulphatis is the genitive of Sul- phas ; quininse is the genitive of Quinina. Recipe Tincturae Cinchonas Compositae uncias duas. Take of Compound Tincture of Cinchona, ounces two. Uncias is the accusative plural of uncia, se, governed by recipe. Duas is the accusative plural (fem.) of the numeral adjective, duo, se, o, and agrees with uncias. Tincturae, noun feminine, genitive, depending on uncias, from Tinctura, se. Cinchonae, noun feminine, genitive, depending on tinctura, from Cinchona, se. Compositae, adjective, feminine, genitive, (from compos itus, a, um), agreeing with tincturae. (The tincture is a “compound tinc- ture.”) Recipe Glycerini unciam unam et semissem. Take of Glycerin ounce one and a half. Glycerini is the genitive of the neuter noun glycerinum,-i, depend- ing on unciam. Unciam is the accusative singular of the feminine noun uncia, se, governed by recipe. Unam, a numeral adjective, accusative singular, agreeing with unciam. Dt,is the conjunction “ and.” Semissem, the accusative singular of semis, gen. semissis, a noun (masc.) meaning “ a half part.” Recipe Acidi Sulphurici Diluti, quantum sufficiat. Take of Acid Sulphuric Dilute, as much as may suffice. Quantum, accusative singular neuter of the interrogative and correlative pronoun quantus, a, um, “ how great, how much ;” the neuter standing here for a noun, “ how great a thing.” There is to be supplied, as object of the verb “ recipe," the de- monstrative pronoun tantum, “ so much : recipe [tantum] quantum 378 HANDBOOK OF PHARMACY. sufficiat, “ take [so much] how much may suffice ” = “ take as much as may suffice.” Sufficiat, third person, singular, present subjunctive, of sufficio, suffeci, suffectum (3d conj.), “ to suffice.” Acidi, genitive singular of Acidum, i, “ the acid.” Sulphurici, genitive singular of the adjective sulphuricus, a, um, “ sulphuric,” agreeing with Acidi. Diluti, genitive singular of the adjective dilutus, a, um, “ diluted,” also agreeing with Acidi. Recipe Aquae ad uncias quatuor: Take of water to ounces four. Aquae is genitive singular of aqua, ae, “ water.” The genitive de- pends on a word (tantum) which must be supplied mentally (see below). Ad, preposition with accusative, “ to, up to.” Uncias, accusative plural of uncia, sc, “ ounce.” Quatuor, indeclinable numeral, “ four.” The sentence is curtailed, since there is apparently no object (accusative) dependent on recipe. In its complete form, the sentence would be: Recipe tantum aquae quantum sufficiat ad uncias quatuor, “ take as much water as [much] would be suffi- cient up to four ounces.” It is rare that the names of the various ingredients are ever written out in full in a prescription, abbreviation being almost a necessity. This should, however, be carefully and considerately done, for such abbreviations can in some instances give rise to serious errors. As examples, a number of such misleading abbre- viations are given here :— May be taken for Acidum Hydrochloricum. “ Hydrocyanicum. Acid. Hydroc. Aq. Chlor. Aqua Chlori. “ Chloroform!. Calc. Chlor. Calcii Chloridum. Calx Chlorata. Chlor. Chlorum (Chlorine). Chloroform. Chloral Hydrate. Extractum Colchici. Colocynthidis. Ext. Col. Calomel. Corrosive Sublimate. Hydrate of Chloral. Hyd. Chlor. Hyd. or Hydr. Hydrargyrum (Mercury). Hydras (Hydrate). Hydrochlorate. Hydrocyanate, etc. Potassium Chlorate. ‘ ‘ Chloride. Pot. Chlor. Potassium Sulphate. “ Sulphite. “ Sulphide. Pot. Sulph. 379 THE ART OF DISPENSING. Sod. Hypo. Sodium Hypophosphite. ‘ ‘ Hyposulphite. May be taken for Sodium Sulphate. “ Sulphite. “ Sulphide. Sod. Sulph. Zinc Phosphate. “ Phosphide. Zinc Phos. The quantity of the various ingredients is very seldom written in full, except perhaps occasionally in metric prescriptions, but is expressed by the various appropriate signs, thus :— Weights. The Ounce (troy), .Symbol 5 Latin Uncia (480 grains). The Drachm, . . ‘‘ 3 “ Drachma (60 grains). The Scruple, . . . “ § “ Scrupulum (20 grains). The Grain, ... “ gr. “ Granum. Measures. The Pint, . . Symbol O Latin Octarius (16 fluidounces). The Fluidounce, “ “ Fluiduncia. The Fluidrachm, “ “ Fluidrachma (60 minims). The Minim, . . “ n£ “ Minimum of a fluidrachm). A half, .... “ ss or11 Semis. Doses.—The doses given in the text-books are either the maxi- mum and minimum, or the average quantity necessary to pro- duce the full effect of the remedy on a healthy adult. These must be diminished for children, females or aged persons, or in other special cases. For children, the dosage may be regulated according to the rule of Dr. Young, viz.: “ Divide the age of the child, in years, by the age of the child plus twelve.” For example, if the age is 6 years, the dose would be 6 + = Ts" = ~3~ the dose for a child of six years is, therefore, one-third of that for an adult. Dr. Cowling’s rule is, “ to add 1 to the age of the child in years and divide by 24.” For example, if the age is 5 years, add 1 which makes 6, and divide by 24, which gives or |. Hence the dose for a child aged 5 years would be one-fourth of that for an adult. 3d. The Subscription.—This includes special instructions to the dispenser for compounding. Since the modern apothecary is pre- sumed to be sufficiently educated to deal with all sorts of com- binations, the physician, as a rule, contracts the directions to a word or even a letter, thus: M. (misce), S. (solve), F. (fiat). Example:— R. Morphinae hydrochloratis, gr. iij Sacchari albi pulveris, 3 iij. M (isee). F(iaf) p(wZr?.s) ; d(whte) i(n) p(artes) aeq(zm7e.s) n(imero) ;rx Mix. Let be powder; divide into parts equal by number 20 made 380 HANDBOOK OF PHARMACY. 4th. The Signature (signatura — label).—The directions for the patient are frequently abbreviated and usually begin with “ Sig.” or “ S.” (= signa, imperative of the verb signo, “to mark; to label ”); sometimes with : “ Misce, detur cum signatura” (mix ; let it be given with the directions ....). Among American physicians, the directions are rarely given in Latin, to avoid any possibility of misinterpretation; also for the sake of the patient, who should fully understand the directions. Hence they are usually written in full, and explicitly, in plain English. 5th. Following the instructions for the patient, the physician signs either his name or initials, with date. The name of the patient should always be written in the upper or lower corner of the prescription, in order to avoid any error on the part of the dispenser or the patient. LATIN TERMS AND ABBREVIATIONS OFTEN USED IN PRE- SCRIPTIONS. Word or Phrase. Usual Contraction. Meaning. Ad, To, or up to. Ad duos vices, . . Ad 2 vic. At twice taking. Ad secundam vicem, . . . Ad sec. vic. For the second time. Ad tertian vicem, . . . Ad 3 tiam vic. For the third time. Adde, Add. Add. A ddantur, Add. Let (them) be added. Addendus, Add. To be added. A dhibendus, Adhib. To be administered. Ad libitum, Ad lib. At pleasure. Admove, Admov. Apply. Admoveatur, .... Admov. Let (it) be applied. Agitato vase, A git. vas. The vial being shaken. Aliquot, Aliq. Some. Alter, Alt. The other. Alternis horis, Alt. hor. Every other hour. Alvus, Alv. The belly. Amplus, Amp. Large. Ampulla, Ampul. A large bottle. Ana, A, or aa, or aa. Of each. Aut, Or. Aqua, Aq. Water. Aqua bullions, ... Aq. bull. Boiling water. Aqua communis, . . . . Aq. com. Common water. Aqua fervens, Aq. ferv. Hot water. Aqua fluvialis, Aq. fluv. River water. Agwa/oniana, Aq. font. Spring water. Aquapluvialis, Aq. pluv. Rain water. Bene, Well. Bibe, Bib. Drink (thou). Biduum, Bid. Two days. Bis, Twice. Bis in die, or bis in dies, . Twice a day. Bolus, Bol. A large pill. THE ART OF DISPENSING. 381 LATIN TERMS AND ABBREVIATIONS OFTEN USED IN PRESCRIP- TIONS. —Contin ued. Word or Phrase. Usual Contraction. Meaning. Bulliat or Bulliant, . . . Bull. Let boil. Calefactus, Calef. Warmed. Caute, Cautiously. Cape, Cap. Take (thou). Capiat, Cap. Let him take. Capsula, Capsul. A capsule. Charta, Chart. Paper. Chart ula, Chartul. A small paper. Cibus, Cib. Food. Cochlear, or Cochleare, . . Coch. A spoonful. Cochleare amplum, . . . . Coch. amp. A dessertspoonful. Cochleare magnum, . . . Coch. mag. A tablespoonful. Cochleare parvum, .... Coch. parv. A teaspoonful. Coctio, Coct. Boiling (noun). Cola, Col. Strain. Colaturse (dative), .... Colatur. To the strained liquor. Collutorium, Collut. A mouth wash. Collyrium, Collyr. An eye wash. Compositus,-a,-um, . . . Comp. Compounded. Concisus,-a,-um, Concis. Cut. Congius, Cong. A gallon. Contusus,-a,-um, . . . . Coutus. Bruised. Cogue; Coquantur, . . . Coq. Boil ; let them be boiled. Cortex, gen. Corticis, . . . Cort. The bark. Cras (adv.) ; Crastinus, (adj), Crast. To-morrow. Cras mane sumendus, . . To be taken to-morrow morning. Cras node, To-morrow night. Cujus, Cujus-libet, .... Cnj. Of which, of any. Cum, C. With. Cyathus, or Cyathus vina- rius, Cyath., C. vinar. A wine-glass. Da; detur, D., det. Give ; let be given. De, Of, or from. Decanta, Dec. Pour off. Decern; Decimus, . . . . Decem. Ten; the tenth. Dein, Thereupon. Deglutiatur, Let be swallowed. Dentur tales doses No. v, . D. t. d. No. v. Let 5 such doses be given. Diebus alternis, Dieb. alt. Every other day. Dilue; Dilutus,-a,-um, . . Dil. Dilute (thou) ; Diluted. Dimidius,-a,-um, . . . Dim. One-half. Dividatur in partes eequales, D. in p. seq. Let it be divided into equal parts. Dosis, D. A dose. Drachma, Dr. or 3. A drachm (60 grains). Eadem (fem.) Ead. The same. Ejusdem, Ejusd. Of the same. Emesis, Vomiting. Et, And. Extende, Ext. Spread. Fac, F. Make. Fiat, Ft. Let be made (sing.). Fiat mistura, .... Ft. mist. Let a mixture be made. Fiat pulvis et divide in Ft. pulv. et div. in Let a powder be made, and chartulas no xii, .... chart, xii. divide it into 12 papers. Fiant, Fnt., or Ft. Let be made (pl.). Fac pilulas duodecim, . . F. pill. xii. Make twelve pills. 382 HANDBOOK OF PHARMACY. LATIN TERMS AND ABBREVIATIONS OFTEN USED IN PRESCRIP- TIONS.—Continued. Word or Phrase. Usual Contraction. Meaning. Fervens, Ferv. Boiling. Filtra, Gargarisma, Filter (thou). Garg. A gargle. Gradatim, Grad. By degrees, gradually. Gutta; Guttse, . . Gtt. A drop; drops. Haustus, Haust. A draught. Hebdomas, Hebdom. A week. Hora, H. An hour. Idem, Id. The same. In dies, Ind. Daily, or from day to day. Inter, ........ Between. Internus,-a,-um, Int. Inner or Internal. Juxta, Near to. Lac, gen. Lactis, .... Lac. Milk, of Milk. Lotio, Lot. A lotion. Macera, Mac. Macerate. Magnus,-a,-um, Mag. Large. Mane, In the morning. Manus, Manus. The hand, Mica panis........ Mic. pan. Crumb of bread. Minimum, M. or min. A minim. Misce, M. Mix. Mitte, Mit. Send. Modicus,-a,-um, Modo prtescripto, .... Modic. Middle-sized. Mod. praesc. In the manner prescribed. Non, Not. Non repetatur, Non repetat. Let it not be repeated. Nox, gen. Noctis, .... Night. Numero, No. In number. Omni hora, Omn. hor. Every hour. Omni mane, Every morning. Omni node, ...... Partitis vicibus, .... Every night. Part. vic. In divided doses. Pastillus; Pastilium, . . . Pastil. A pastille. Per, Through, By. Pilula, Pil. A pill. Poculum, Pocul. A cup. Potus, Praeparatus,-a,-um, . . . Drink (noun). Praep. Prepared. Primus,-a,-um, Primus. The first. Pro.......... For. Pro re nata, P. r. n. Occasionally, as occasion mands. Pulvis, Pulv. A powder. Quantum libet, Quantum sufficiat, .... Q. lib. As much as is desired. Q. s. As much as is sufficient. Quaque (abl.), Qq. Each, or Every. Quartus,-a, -um, Quatuor, Quart. Fourth. Quat. Four. Quinque, Quinq. Five. Quintus,-a,-um, Quint. The fifth. Quotidie, Quotid. Daily. Recipe, B. Take. Reliquus,-a,-um, Remaining. Repetatur, Rept. Let it be repeated. Saturatus,-a,-um, .... Sat. Saturated. Scatula, Scat. A box. THE ART OF DISPENSING. 383 LATIN TERMS AND ABBREVIATIONS OFTEN USED IN PRESCRIP TIONS.—Continued. Word or Phrase. Usual Contraction. Meaning. Scrupulum, ...... Scrap., or 9- A scruple (20 grains). Secundem artem, .... S. A. According to art. Secundus-a,-um, Second. Second. Semis, gen. Semissis, . . . Ss. A half. Septem, Sept. Seven. Sex, Six. Signa, Sig. Write, or Mark (thou). Simul, Together. Sine, Without. Solve, Solv. Dissolve. Somnus, Somnus. Sleep. Statim, Stat. Immediately. Same, ......... Sum. Take (thou). Supra, . . . . . . Above. Tails, Tai. Such a one. Ter, Thrice, or Three times. Ter in die, or Ter die, . . T. i. d., or T. d. Thrice daily. Tere, Rub (thou). Tertius,-a,-um, Tert. Third. Tres, Three. Triduum, Trid. Three days. Tussis, . Tus. A cough. Ultimo preescriptus, . . . Ult. praesc. The last ordered. Una, Una. Together. Uncia, Unc. or 5. An ounce. Ut dictum, Ut. Diet. As directed. Vas vitreum, Vas vit. A glass vessel. Vel, Or. Vinum, Vin. Wine. Vires (plus.), Vir. Strength. Vitellus, Vitel. Yolk. Vitreus,-a,-um, Vitr. Made of glass. FOREIGN PRESCRIPTIONS. German prescriptions offer some differences of nomenclature, particularly in the use of the adjective, thus:— From R. Kali hydrojodici, 5.0 (Kalium Hy droj odicum). Aquae camphoratae, 50.0 (Aqua cam- phorata). Syrupi, 120.0 (Syrupus). Rendered into Anglo-Latin: Potassii lodidi, 5.0 Aquae Camphorae, 50.0 Syrupi, 120.0 Thus Natrium aceticum is written for Sodii Acetas; Ferrum jodatum for Ferri iodidum ; Ferrum sulfuricum for Ferri Sulphas, etc. A few physicians of the old school still employ some cabalistic 384 HANDBOOK OF PHARMACY. signs* (Fig. 383) derived from alchemistic times; and certain obsolete terms are occasionally employed to designate well known Fig. 383. Aqua. V Aqua fontana. V7 Aqua pluvialis. Aurum. (£) Argentum. J) Camphora. Crystallum. \ X Cuprum. Q Destillatus. Ferrum. Poison. Hydrargyrum. Nitrum. Phosphorus. Plumbum, p Precipitatus. Tfg Pulvis. Saccharum. Acidum. + Sal. Q Spiritus. Spiritus Viui rectificatus. Spiritus Viui rectificatissimus. Stannum. 2|_ Stibium. Omni hora. Sublimatum. -n- Sulphur. Tartarum. Vitriolum. Vitrum. Volatile. remedies. The following table will explain a number of such terms.! For Acetum plumbi ‘ ‘ “ saturninum ‘ ‘ Aqua saturni “ “ phagedaenica “ “ fbntana ‘ ‘ Aquila alba “ Flores benzbes “ “ naphae “ “ zinci “ Gummi mimosae ‘ ‘ Lapis iufernalis “ Magisterium bismuthi ‘ ‘ Mercurius “ Natrum carbonicum acidulum “ Natro-kali tartaricum “ Nihilum album “ Oleum anthos “ Protojoduretum hydrargyri “ Saccharum saturni ‘ ‘ Sal amarum “ “ mirabile “ Sapo viridis “ Spiritus Mindereri “ Tinctura thebaica “ Acidum phenylicum ‘ ‘ Aqua amygdalarum amararum “ Calcaria usta “ Cortex chi use ‘ ‘ Chininum read Liquor Plumbi subacetatis. “ “ “ “ dilutus. “ Lotio hydrargyri flava. “ Aqua pura. “ Hydrargyri subchloridum. ‘ ‘ Acidum benzoicum. “ Flores aurantii. “ Zinci oxidum. ‘ ‘ Acacia. “ Argenti nitras. 1 ‘ Bismuthi subnitras. 1 ‘ Hydrargyrum. “ Sodii bicarbonas. ‘ ‘ Potassii et sodii tartras. “ Zinci oxidum. “ Oleum rosmarini. “ Hydrargyri iodidum viride. “ Plumbi acetas. ‘ ‘ Magnesii sulphas. “ Sodii sulphas. “ Sapo mollis. “ Liquor ammonii acetatis. ‘ ‘ Tinctura opii. “ Acidum carbolicum. “ Aqua laurocerasi. 1 ‘ Calx. “ Cinchona. “ Quinina. * Real-Encyclopeedie der Pharmacie, by Geissler and Moeller, Vol. I, p. 23, Wien. f Selected (with alterations) from “ The Art of Dispensing,” Chemist and Druggist, London. THE ART OF DISPENSING. 385 For Flores cinte “ Gutti “ Hydrargyrum amidato-bichlorat. ‘ ‘ Kalium “ Kali “ Linimentum volatile “ Radix liquiritiae “ Liquor ammonii caustici “ Natrium “ Natrum ‘ ‘ Stibium “ Semen strychni “ Tartarus depuratus “ “ natronatus “ “ sti hiatus “ Tinct. opii benzoica “ Vinum stibiatum read Santonica. ‘ ‘ Cambogia. “ Hydrargyrum ammoniatum. “ Potassium. “ Potassa. “ Linimentum ammoniaj. ‘ ‘ Glycyrrhiza. “ Liquor Ammonite. “ Sodium. “ Soda. “ Antimonium. “ Nux vomica. ‘ ‘ Potassii bitartras. “ Potassii et sodii tartras. “ Antimonii et potassii tartras. ‘ ‘ Tinctura opii camphorata. “ Vinum antimonii. The quantities ordered are always understood weight, unless specially specified. The metric system being employed exclus- ively by the Continental countries, a few typical examples are given. (See also Typical Prescriptions.) B. Apomorph, mur. cryst., 0.04 04 Morph, mur., 0.02 02 Aquae amygd. amar., 5.0 or 5 Elix. pectoralis, 20.0 20 Aqu. destill., 30.0 30 B. Ammonii Chloridi, 10 Gm. Ext. Glycyrrh. Fid., 10 Gm. Aquae Foeniculi, 250 Gm. B. Morphinae sulphatis, 0.001 Gm. Sacchari, 1.5 Gm. French Prescription. B. Kermes mineral, 0.10 gramme. Gomme arabique, q. s. Eau destillee, 150 grammes. Teint. d’aconit, 6 gouttes. Sirop diacode, 30 grammes. “TABLE OF TERMS LIKELY TO OCCUR IN FRENCH AND GERMAN PRESCRIPTIONS”* A, Fr., to, or ; Trois it quatre paquets (three or four powders). Abendessen, Abend-brod, -mahlzeit, -tisch, Ger., supper. Drei von diesen Pillen vor dem Abendessen. (Three of these pills before supper.) Acide azotique, Fr., nitric acid. Aetz - Ger., caustic. Aetzstein, Ger., caustic potash. Alcohol sulphuris, Ger. Lat., carbon bisulphide. Alcohol de soufre, Fr., carbon bisul- phide. Al tschaden wasser, Ger., lotio flava, yellow wash. Aqua calcaria, G. L., lime water. Aqua chlorata, G. L., chlorine water. Arsenige Saure, Ger., arseuious acid. Arsensa ure, Ger., arsenic acid. Augenstein, Ger. lapis divinus. Azotate, Fr., nitrate. Barbotine, Fr., santonica. Baudruche, Fr., goldbeater’s skin. Bissen, Ger., bolus. Sechs Bissen im Tage zu nehmen auf drei Gaben ver- theilt. (Six boluses to be taken daily, divided into three doses.) Blauholz, Ger., logwood. Bleiessig, Ger., liq. vplumbi subacetatis. Bol, Fr., bolus. A prendre six bols par ♦Selected from “ The Art of Dispensing,” Chemist and Druggist, London.—Ger. Lat. or G. L. means “ German-Latin,” that is modern Latin, as employed in Germany and some other European countries. 386 HANDBOOK OF PHARMACY. jour en les partageant en trois doses. (Six boluses to be taken every day, dividing them into three doses.) Bourdaine, Fr., Rhamnus Frangula. Calcaria, G. L., calx or calcium. Carboneum, G. L., carbon. Carbonicus,-a,-um, G. L., carbonas, or carbonate. Cautere potentiel, Fr., caustic potash. Chamomilla vulgaris, G. L. ; Matricaria chamomilla, L. Chaux, Fr., lime. Chinin, Ger., quinine. Chininum, G. L., quinine. Chloratus,-a,-um, G. L., chloride. Chlorsaures, Ger., chlorate. Cinchoninum, G. L., cinchonine. Citricus,-a,-um, G. L., citrate. Coccionella, G. L., cochineal. Colla piscium, G. L., ichthyocolla. Coton carde, Fr., wadding, cotton wool. v Coucher, Fr., bed-time, going to bed. A prendre deux pilules avant le coucher. (Two pills to be taken at bed-time.) Cyanatus,-a,-um, G. L., cyanidum, cy- anide. Cuilleree & cafe, Fr., teaspoonful. Une cuilleree it cafe, au cas d’Une attaque de toux. (A teaspoonful to be taken if the cough comes on.) Cuilleree & soupe, Fr., tablespoonful. Prenez une cuilleree a soupe toutes les deux heures. (One tablespoonful every two hours.) Dower’sches Pulver, Ger., Dover’s powder. L’effet voulu, Fr., the desired effect. Une cuilleree & cafe toutes les demi- heures jusqu’tl l’effet voulu. (A tea- spoonful every half hour till it acts.) Einspritzung, Ger., injection. Eisessig, Ger., glacial acetic acid. Emplastrum adhresivum anglicum, G. L., court plaster. Emplastrum picatum, G. L., pitch plaster. Essen, Ger., meal. Essig, Ger., vinegar. Esslbffel, Ger., tablespoon. Alle zwei Stunden einen Esslbffel-voll. (A tablespoonful every three hours.) Ferrocyanatus,-a,-um, G. L., ferrocyan- ide. Flasche, Ger., bottle. Schiitteln Sie die Flasche. (Shake the bottle.) Fois, Fr., time. Prenez en quatre fois a une demi heure d’intervalle. (To be taken in four portions at intervals of half an hour.) x Gouttes, Fr, drops. A prendre dix gouttes trois fois par jour. (Ten drops to be taken thrice daily.) Clas, Ger., glass, tumbler. Hirschtalg, Ger., mutton suet. Hollenstein Ger., silver nitrate, lunar caustic. lodure de formyle, Fr., iodoform. Kohlensaure, Ger., carbonic acid. v Kummel, Ger., caraway. A jeun, Fr., fasting. Prenez deux ou trois de ces pilules & jeun. (Take two or three of these pills fasting.) Latwerge, Ger., electuary. Lavement, Fr., enema. Limonade sfeche, Fr., effervescent saline. Liquiritia, G. L.. glycyrrhiza. Mai, Ger., time, portion. Auf vier Mai in halbstundigen Zwischenraumen zu nehmen. (To be taken in four portions at intervals of half an hour.) Mittagsessen, Ger., dinner (properly ‘mid-day meal’). Dieses Pulver un- mittelbar vor dem Mittagsessen zu nehmen. (This powder to be taken immediately before dinner.) Natrium, G. L., sodium ; Natrum, G. L., soda, sodium oxide. Nuchtern, Ger., sober, fasting. Vieroder sechs von diesen Pillen nuchtern zu nehmen. (Four or six of these pills to be taking fasting, or before break- fast.) Oblate, Ger., wafer. Ein Pulver vor der Mahlzeit in einer Oblate zu nehmen. (A powder to be taken in a wafer before meals.) Ordonnance, Fr., prescription. Ouate, Fr., wadding, cotton wool. Pain azyme, Fr., wafer. Un de ces paquets ;i prendre dans du pain azyme avant le repas (One of these powders to be taken in a wafer before meals.) v Paquet, Fr., a packet, powder. A pren- dre un paquet toutes les deux heures. (One powder to be taken every two hours.) On prend un de ces paquets peu de tempsavant 1’attaque defievre. (One of these powders to be taken shortly before the fever fit.) Pasta gummosa, G. L., pate de guimauve Fr. Marshmallow paste. s Pastilles, Fr., lozenges. A prendre de quatre i six pastilles par jour. (Four to six lozenges to be taken daily.) Pastillen, Ger., lozenges. Man nimmt von diesen Pastillen auf einmal nur eine alle zwei Stunden. (One only of these lozenges to be taken every two hours.) Pierre A cautfere, Fr , caustic potash. Pillen, Ger., pills. Zwei Pillen jeden Abend vor dem Zubette-gehen. (Two pills every evening before going to bed.) Pilules, Fr., pills. Deux pilules chaqne soir avant le coucher. (Two pills every evening before going to bed.) 387 THE ART OF DISPENSING. Pincee, Fr., a pinch. Infusez une pincee de ces herbes avec un demi-litre d’eau bouillante pour faire une tisane. (Infuse a pinch of these herbs in half a pint of water to make a draught.) Potasse la chaux, Fr., caustic potash. Potion, Fr., mixture, potion. Poudre, Fr., powder. Matin et soir une poudre dix minutes avant le repas. (One powder every morning and evening, ten minutes before meals.) Poudre alexitfere Fr., Dover’s Powder. Poudre anodine, Fr., Dover’s Powder. Poudre diaphoretique, Fr., Dover’s Powder. Poudre gazeuse, or Poudre gazifere pur- gative, Fr., Seidlitz powder. Poudre gazogene, Fr., effervescent or gazogene powder. Poudre gazogene neutre, Fr., soda powder. Poudre gazogene laxative, Fr., Seidlitz powder. Poudre Savory, Fr., Seidlitz powder. Poudre sudorifique, Fr., Dover’s Pow- der. Priser par le nez, Fr., to snuff. Pour priser par le nez cinq ou six fois par jour. (To be snuffed five or six times daily.) Pulver, Ger., powder. Ein Pulver jeden Morgen und Abend zehn Minuten vor dem Essen. (One powder every morn- ing and evening, ten minutes before meals.) Man nimmt ein Pulver kurz vor Fieberanfall. (A powder to be taken shortly before the fever fit.) Pulvis aerophorus, G. L., effervescent powder, gazogene powder, soda pow- der. Pulvis aerophorus laxans, G. L., Seidlitz powder. Pulvis gummosus, G. L., pulvis traga- canth® co. Raucherkerzchen, Ger., fumigating pas- tilles. Raucheressig, Ger., toilet or disinfecting vinegar. Repas, Fr., meals. Rezept, Ger., prescription. Riechessig, Ger., aromatic vinegar. Saindoux, Fr., lard. Saure, Ger., acid. Schlafengehen, Ger., “ going-to-bed,” bed-time. Vor dem Schlafengehen zwei Pillen zu nehinen. (Two pills to be taken at bed-time.) Schnupfen, Ger., to snuff. F'unf bis sechs Mai im Tage zu schnupfen. (To be snuffed five or six times daily.) Schwarzes Wasser, Ger., black wash, lotio nigra. Schwefel, Ger., sulphur. Schweflige Saure, Ger., sulphurous acid. Schwefelsaure, Ger., sulphuric acid. Sebum, G. L., sevum, suet. Sei de lait, Fr., milk sugar. Soufre vegetal, Fr., lycopodium. Stibium, G. L., antimonium. Sucre de Saturne, Fr., lead acetate. Sulfuratus,-a,-um,G. L., “sulphurated,” sulphidum, sulphuretum, sulphide. Sulfuricus, a,-um, G. L., “sulphuric,” sulphas, sulphate. Table, Fr., stable. Se mettre a table. (To dine.) A prendre deux de ces pilules en se mettant h table. (Two pills to be taken before dining.) Taffetas d’Angleterre, Fr., court plaster. Tartarus boraxatus, G. L., soluble tartar, potassium boro-tartrate. Tartarus depuratus, G. L., potassium acid tartrate, cream of tartar. Tartarus natronatus, G. L., Rochelle salt, potassium and sodium tartrate. Tartarus stibiatus, G. L., tartar emetic, antimonium tartaratum. Theeloffel, Ger., a teaspoon. Ein Thee- loffelvoll, a teaspoonful. Tisane, Fr., draught, medicated drink. Tisch, Ger., table. Zu Tische gehen. (To take a meal.) Man nehme zwei von diesen Pillen wenu man zu Tische geht. (Take two pills before eating.) Trifolium fibrinum, G. L., Menyanthes trifoliata, buckbean. Tropfen, Ger., drop. Drei Mai des Tages zehn Tropfen zu nehmen. (Ten drops to be taken thrice daily.) Verordnung, Ger., prescription. Verre, Fr., glass, tumbler. Un verre d’eau sucree. (A tumbler of sugar and water.) Wasserstoff, Ger., hydrogen. Weinsteinsaure, Ger., tartaric acid. Wirkung, Ger., action, effects. Ein Theeloffelvoll alle halbe Stunden bis zur Wirkung zu nehmen. (Take a tea- spoonful every half-hour until it acts.) 388 HANDBOOK OF PHARMACY. Homoeopathic medicines are prepared in the form of:— Solutions in water, alcohol, or a mixture of these, or, very rarely, in ether, glycerin, or syrup. Triturations with sugar of milk. Liquid Attenuations.—Pilules and globules are merely forms of dispensing the liquid attenuations. The mother tinctures are of the strength of 10 per cent., based on a percentage of dry plant. Should the fresh plant be employed, the amount of moisture is estimated and a corresponding quan- tity taken. The process of attenuation (dilution) begins from a point termed “zero,” which is marked. This represents usually the pure medicinal substance. The strong or mother tincture is marked The first decimal (lx) attenuation contains 10 per cent, of the tincture; it is made by adding 10 parts of mother tincture to 90 parts of the diluent. Or, it may be made as follows: Select a clean half-ounce bottle with a good tight-fitting cork; then put in 20 minims of the mother tincture and 180 minims of alcohol of the same strength; cork the bottle and shake. This constitutes the first decimal attenuation, and should be marked lx. Each subsequent attenuation is prepared in like manner from the one preceding it, and should be marked in order, 2x, 3x, etc. This constitutes the decimal scale. The centesimal attenuations are prepared in the same way, but are diluted in the proportion of 1 in 100 instead of 1 in 10, and are generally marked in figures 1, 2, 3, etc. HOMEOPATHIC DISPENSING. Hahnemann published minute directions for making tritura- tions, and his method is still adhered to, with the small alteration of the quantity of sugar of milk used at each stage of the pro- cess. He recommends that 1 grain of the substance be triturated with 99 grains sugar of milk for one hour. It is, however, recommended in the Homoeopathic Pharmacopoeia to use the proportion of 1 to 9, as it is found that a better and more perfect mixture results. The substance is to be first triturated in a clean Wedgwood mortar with an equal amount of sugar of milk, a horn or ivory spatula being occasionally used to scrape the mixture from the sides of the mortar. This completes the first stage of the process. The second stage consists in adding and mixing, as before, three times the amount of sugar of milk used in the first stage. The third stage consists in adding and mixing, as before, five times the amount first used, when the trituration is regarded as com- pleted, and can be transferred to a perfectly clean, dry bottle, carefully corked and labeled lx. This constitutes the first deci- HOMOEOPATHIC TRITURATIONS. THE ART OF DISPENSING. 389 mal attenuation, containing 1 part of the substance in 10. For making subsequent triturations, 1 part of the first trituration and 9 parts of sugar of milk in fine powder are mixed in two stages in a manner similar to that employed in making the first decimal trituration. It should be noted that coarse sugar of milk is used in the first and second stages of the first trituration and fine sugar of milk in all subsequent triturations. The method of medicating pills and globules consists in putting a suitable quantity in a clean, dry bottle, and pouring over them a sufficient quantity of tincture (of the strength required) to thoroughly saturate them, shaking the bottle in a circular direction so as to insure them all being equally saturated, and then drying them by allowing the spirit to evaporate. Tincture triturations are a form of powder now used, and for the preparation of which definite instructions are given in the Homoeopathic Pharmacopoeia. Briefly, they are prepared by pouring successive quantities of tincture on sugar of milk, con- tained in a mortar, thoroughly mixing, and allowing the mixture to dry after each addition of tincture, so that the strength of the powder ultimately obtained represents 1 minim of tincture in each grain:— R. Tinct. Nucis Vomicae, 6x, -l52- Aquae destill.,vj. M. Ft. mistura, cujus capiat cochlearia duo magna tertiis horis. Twelve drops of the sixth dilution are prescribed. R. Nucis Vomicae, f Sacch. Lactis, q. s Ft. pulvis. Mitte vj. Two grains of the third dilution are triturated with sufficient Sugar of Milk and made into powders. R. Pil. Chamomillae, Direct a pilule to be taken every three hours. Three pilules saturated with tincture of the twelfth attenuation. R. Tinct. Belladonnae, 3x, Aquae destill., Ft. Misce. Dessertspoonful every six hours. Tinct. Pulsatillae 0,ryx Aquae dest., The Tincture of Belladonna should be the third attenuation. The Tinct. of Pulsatilla should be the mother tincture (10 per cent). R. Trit. Mercurii sol., 6x,gr. J Mitte tales chart, xij. This should be diluted with a little Sugar of Milk before dividing. The trituration of Mercurius Solubilis is prepared from Suboxide of Mercury (Hg2O). 390 HANDBOOK OF PHARMACY. SOLUBILITIES. In the compounding of prescriptions, an acquaintance with the general rules of solubility is of great value to the dispenser. For this purpose the general table of solubilities in water (normal temperature), as compiled by Prof. Attfield, is given:— Acetates.—Soluble. Arsenates and Arsenites.—Insoluble, except those of alkali metals. Bromides.—Soluble, except Hg(ous) and Ag.—Sb, Bi, with water form insoluble Oxysalts. Carbonates.—Insoluble, except those of alkali metals. Chlorides.—Soluble, except Hg(ous) and Ag.—Pb sparingly. Citrates.—Soluble, except those of Mu, Hg(ous), Ag, Sr—Al, Ba, Bi, Cd, Cu, Pb, Zn, sparingly soluble. Cyanides.—Insoluble, except Hg (ic), and those of alkali metals and earths. Hydrates.—Insoluble, except Ba, Sr, alkali metals.—Sr, Ca, Pb, sparingly soluble. Iodides.—Soluble, except Sb, Bi, Au.—Pb, Hg(ic), Hg(ous), and Ag, sp’r soluble. Oxalates.—Insoluble, except alkali metals—Sb, Cr, Fe(jc), (ous), Sn(ic), sparingly soluble. Oxides.—Insoluble, except Ba, Sr, Ca, and alkali metals. Nitrates. — Soluble. Sulfates.—Soluble, except Ba, Sr.—Ca. Sb, Hg(ous) sparingly soluble. Sulfites.—Soluble, except Al, Sb, Bi.—Fe(ous), Ca, Mn, Ag, Zn, sparingly soluble. Tartrates.—Soluble, except Sb, Ba, Bi.—Ca, Fe(ous), Pb, Mu, Hg(ic), (ous), Sr, Zn, sparingly soluble. Certain chemical compounds, when brought together under favorable conditions, either give rise to violent reaction, or favor the formation of new bodies which explode on the application of mechanical force. To give rise to such violent or explosive reactions all favorable conditions must be fulfilled, hence, in order to operate with such bodies with safety we must avoid these con- ditions as much as possible, by such precautions as previous dilu- tion of the active agents, avoiding pressure or force, heat, etc. The following list * is a general classification of such bodies as are liable to give rise to such difficulties. Explosive Bodies and MixTUREs.f I. Spontaneously Inflammable Bodies. Phosphorus (also subsulphide). Compounds of methyl and ethyl with Al, Zn, B, As, Sb, etc. II. Bodies Which Explode on Heating. Ammonium nitrate (when suddenly or strongly heated). Chlorine monoxide (C12O), trioxide (C12O3), tetroxide (C12O4). Mercurous oxalate. EXPLOSIVE MIXTURES. *See on this subject: “ Explosive Bodies and Mixtures,” by Dr. Chas. Rice, New Remedies, 1878, pp. 165-196. Another paper on this subject is by C. D. Lippincott, Proceed. Penn. Phar. Ass’n., 1886 ; see also “ Art of Dispensing,” London, Chemist and Druggist. fOnly the better known bodies are given here; for a more complete list, consult Dr. Rice’s article, New Remedies, 1878, pp. 165-197. THE ART OF DISPENSING. 391 Urea nitrate (suddenly heated). Most organic nitro-substitutioii compounds, containing the group NO2. Picric acid explodes when quickly heated in a confined space. Picrates when strongly heated, especially in a confined space. Hypophosphites (also in solution) when heated too high. Silver Chlorite (AgC102) explodes at 105° C. Silver oxalate, citrate, fumarate, malate. Ammonium iodate and periodate. Chlorates explode when heated in presence of combusti- ble bodies. Methyl and ethyl nitrate; their heated vapor explodes. Permanganic acid. III. Bodies ivhich Explode on Percussion or ivhen Triturated. Substances which contain carbon and oxygen with nitrogen in a feeble state of combination with the entire amount or a portion of the oxygen. When ex- plosion takes place, the nitrogen is set free, and the oxygen unites with the carbon present to form carbon monoxide and dioxide. If hydrogen is present, it forms water in the shape of greatly expanded vapor. Certain nitrogen oxides when substituted in place of hydrogen, may form very explosive compounds, such as nitroglycerin or the hexanitrocellulose (gun cotton). Chlorates should never be prescribed in powder, mixed with organic or inorganic combustible or oxidizable bodies. Some of these mixtures should never be mixed, but dispensed separately or in solution. When it is necessary that such be mixed, the greatest caution should be observed, and only small quantities should be operated on at a time, with the precaution of pulverizing each ingredient separately and mixing without pressure. Commercial potassium chlorate, if it contains organic impurities, will explode on tritur- ation. Tannic and Gallic Acids, Antimony Sulphides, Amorphous Phosphorus, Charcoal, Catechu, Lycopodium, Glycerin, Sulphur, Iodine, Oxalic Acid, Sugar, Hypophosphites, Starch, Phenol, Salicylic Acid, Morphine, Shellac. Chlorates* with Organic Substances in Gen- eral, as for Exam- ple :— ♦The preparation of colored fires is attended with much danger, as they generally contain potassium chlorate or nitrate and various easily combustible bodies. Each of the ingredients should be dried and powdered singly, then the whole mixed with a wooden spatula, with great care. 392 HANDBOOK OF PHARMACY. Chlorates, Bromates, and Iodates when rubbed or heated with iodine, sulphur, reduced iron, sulphides, etc. Fulminates are exceedingly explosive. Glonoin (nitroglycerin). Nitrogen Chloride, produced by the action of chlorine on a solution of ammonium chloride. Nitrogen Iodide, generated by bringing together iodine and ammonia. Even the vapor of ammonia on com- ing in contact with iodine may produce it. Nitric Acid (fuming), with readily oxidizable substances, such as glycerin, alcohol, tinctures, volatile oils, resins, sugar, phos- phides, etc. With straw or sawdust it is liable to ignite. Permanganates with organic extracts, organic powders, organic acids, fats and oils, hypophosphites, reduced iron, sulphur, or sul- phides, glycerin, alcohol, etc. These react in very dilute solutions in causing a reduction (decolorization) of the permanganate to manganate; when triturated or even mixed with many organic compounds, they give rise to violent reactions or explosions, due to the extremely loose state of combination of their oxygen. Oxide and nitrate of silver, when made into pills with saccharine or other reducing agents, do not usually explode with violence, but cause the pills to swell up rapidly and to fall to pieces. Mixtures from which a gas is evolved, should not be corked until the evolution of the gas has ceased, unless it is especially desired to confine the gas together with the liquid, in which case the necessary precautions must be taken. The following combinations are dangerous, some of them hav- ing caused serious accidents:— R . Potassii Chloratis, Should not be triturated together, nor Acidi Tannici. mixed together and dispensed in dry M. form. Dispense the powders separately. R. Potassii Chloratis, -n- i • at. ! Acidi Tannici Dissolve the tannin in the glycerin, rivccrini ’ and chlorate in the water, and then (’ mix. Do not rub the chlorate, tannin M. Ft. Sol. and S1ycerin together. R. Potassii Chloratis, The two salts must not be rubbed Sodii (or Calcii) Hypophosphitis, together or an explosion will result. Aquse. They should be dissolved separately in M. Ft. Sol. water and mixed. R. Potassii Chloratis, . . . 5ss-?i Tr , , . .. . Tincture Ferri Chloridi, iss-.?ij ™ed’ the mixture « liable to Glycerini,3ss-£iij. explode' R. Olei Terebinthinae, These should be cautiously mixed in Acidi Sulphurici or Acidi Nitrici. an open vessel, as the reaction is quite violent. This. dwi11 bur?.t. <>n standing, Extract! Gentians. owing to the decomposition of the silver M Ft Pill oxide by the organic extract. THE ART OF DISPENSING. 393 R. Potassii Chloratis, . . . . gr. iij Sulphuris Precipitati, . . gr. v Zinci Valerianatis, . . . . gr. j This should not be dispensed. When Sacchari,gr. xx. carelessly mixed it is liable to explode. M. Ft. pulvis. Dentur tales doses No. x. R . Potassii Permanganatis, . . 5 j These, on being brought together, will Glycerini, fgss. cause an explosion. R. Acidi Chromici,gr. x rm.* • j i i • Glycerini, . . ’f|j. This is dangerously explosive. R . lodi,f 3 ss This mixture has given rise to an ex- Linimenti Camphorse Co., plosion, owing to the formation of Saponis, . nitrogen iodide, from the presence of M. Ft. linimentum. the ammonia in the Lin. Camph. Co. R. Acidi Nitrici, This mixture is liable to explode a few Tincture Nucis Vomic®, aa f 3 ij. hours after bein" mixed- R. Acidi Nitromuriatici, . . . f?ss . ... . . Tincture Cardamomi, . . ffj. Thls mixture W1U exPlode’ 394 HANDBOOK OF PHARMACY. INCOMPATIBLES. Incompatibility, that is, the incongruity among the constituents of a prescription, or their interference with each other, may be of three kinds, viz.: 1, chemical; 2, pharmaceutical; 3, therapeu- tical. Chemical Incompatibility.*—This arises when a chemical change takes place with the formation of one or more new com- pounds which were not expected or intended to be produced by the prescriber. A prescription may be chemically incompatible, and yet be just what the physician desires. For instance, acids are generally said to be incompatible with alkalies, yet they are prescribed together, in many instances intentionally, so as to produce the corresponding salts. Liquor calcis is chemically incompatible with mercuric or mercurous chloride, yet the pro- ducts of the reaction with either one of these chlorides are actually intended to be produced, as they are the therapeutic agents wanted. The dispenser, with a little experience, can readily distinguish a case of intentional from one of unforeseen in- compatibility. Examples. Alkalies (caustic or carbonated) are incompatible with alkaloids in aqueous or weak alcoholic solutions; also, with acids, metallic salts, ammonia salts, etc. Alkaloids (aqueous or weak alcoholic solutions) are precipitated from their solutions by liquids containing albumen, tannin, mercuric chloride, free iodine, Donovan’s solution, Lugol’s solu- tion, double iodides, alkalies or alkali carbonates, picric acid, auric or platinic chloride, and many other compounds. Acacia in solution forms a jelly with tincture of ferric chloride, borax, alcoholic or ethereal solutions, solution of lead sub- acetate, etc. Arsenous Acid, with tannic acid, salts and oxide of iron, lime and magnesia, is rendered insoluble. Antipyrin is incompatible with carbolic acid, nitric acid, ammonia alum, syrup of ferrous iodide. With spirit of nitrous ether or amyl nitrite, it produces a bright-green colored solution, due to the formation of isonitroso-antipyrin; with ferric salts, it develops an intensely red-colored solution. Like the alkaloids, it is incompatible (precipitated) with all solutions containing tannic acid (such as infusions, certain fluid extracts, tinctures, etc.), tincture of iodine, mercuric chloride, Lugol’s solution, etc. Bromides are subject to nearly the same reactions as the iodides. Bismuth Subnitrate or Subcarbonate is incompatible with tannin, sulphides, mercurous and mercuric salts, etc. * Consult typical prescriptions given under this head. THE ART OF DISPENSING. 395 Calomel is decomposed by alkalies, alkaline earths, their carbon- ates, sulphides, solution of lime, iodides, iodine, soap, acids, salts of lead, iron and copper, silver nitrate, etc. Chlorides are incompatible with silver salts and mercurous salts, lead salts, etc. Chloral is incompatible with alkalies (CHC13 being liberated), sulphites, ammonia water, calomel; in alcoholic solution chloral alcoholate (see Prescription No. 84) is formed; in aqueous solu- tion it slowly undergoes decomposition, etc. Chlorates. See page 391. Chlorine Water is incompatible with silver, lead, and mercurous salts, organic substances, emulsions, hyposulphites, etc. Corrosive Sublimate is incompatible with alkalies, alkali carbon- ates, solution of lime, the iodides or bromides, alkaloids (in aqueous solution), sulphides, reduced iron, silver nitrate, albu- men, gelatin, tannic acid, etc. Hydrogen Peroxide is incompatible with vegetable tinctures, alkali citrates and tartrates, ferrous salts. It sometimes liberates iodine from iodides. This is due to the presence of iodates, the iodine being liberated by the action of the small amount of acid pre- sent in the hydrogen peroxide. Iodine is incompatible with ammonia or its salts, starch, metallic salts, fatty or volatile oils, emulsions, chloral, solutions contain- ing alkaloids, sodium hyposulphite, etc. Iron (reduced) is incompatible with vegetable extracts (containing organic acids), metallic salts, acids, mercuric chloride, potassium permanganate, etc. Iron Salts are incompatible with alkalies and the alkali carbon- ates, solutions containing tannic acid, mucilages, emulsions, solutions of the iodides or bromides, etc. Iodides. The alkali iodides, also ferrous iodide, are incompat- ible with the strong mineral acids, many alkaloids, metallic salts, silver nitrate, potassium chlorate, chlorine water, hydro- gen peroxide (see Hydrogen Peroxide), etc. Lime-water is incompatible with acids, ammonia compounds, salts of the metals, soluble carbonates, etc. Lead Acetate is incompatible with iodides, bromides, chlorides and sulphates, alkalies and their carbonates, lime-water, soap, sul- phides, acids, acacia, tannin, etc. Lead Subacetate (Goulard’s Extract) is incompatible with the alkali carbonates, alkalies, alkali earths, sulphuric or hydrochloric acids, sulphides, solution of acacia, solutions containing tannin, also most vegetable coloring matters, albumen, etc. Pepsin, when combined with alkalies or alcoholic liquids, or tan- nates, loses its digestive activity. 396 HANDBOOK OF PHARMACY. Potassium Permanganate is incompatible with all organic com- pounds. Quinine Sulphate gives rise to many complications. When or- dered in a mixture, it should not be dissolved (by,aid of an acid) unless so ordered by the physician ; it is far more in- tensely bitter in solution than when simply suspended. Qui- nine and its salts can be dispensed in a suspended condition in combination with various incompatibles without inconve- nience, but when it is first dissolved before combining, then many difficulties arise. Thus we may suspend the quinine in a mucilaginous mixture with such incompatibles as tannin, alkalies, salicylates, etc., without giving rise to the unsightly insoluble mass which is formed when these are added to its solution. Strychnine when in solution combined with bromides is generally deposited, on standing, as insoluble strychnine bromide. When any of these alkaloidal precipitants is prescribed in a solu- tion with an alkaloid, the former should be slowly added in a well diluted condition to the latter in solution, in order to obtain the insoluble precipitate in as finely divided condition as possible, so that, when shaken, it readily remains suspended. Such incompatible combinations are admissible in mixtures containing quinine, and in many others in which the total amount of alkaloid is small. Combinations which contain larger amounts of active and powerful alkaloids, such as strych- nine or morphine, as insoluble precipitates, should under no circumstances be dispensed, since the patient may receive the whole of the precipitated alkaloid at one dose. Silver Nitrate is incompatible with chlorides, iodides, bromides, cyanides, alkali and earthy carbonates, sulphides, organic bodies, etc. Salicylic Acid is incompatible with iron compounds, alkali iodides; salts of salicylic acid likewise with iron compounds, also with alkaloids, acids, etc. Tartar Emetic is decomposed in solution by the addition of acids, alkalies, soap, calomel, tannin, acacia, opium, etc. Tannin and all solutions containing it, are incompatible with all metallic salts, gelatin, albumen, alkali carbonates, alkaloids, etc. Pharmaceutical or Mechanical Incompatibility.*—Many substances or solutions cannot be brought to the state of a clear * For example:— The addition of resinous tinctures or fluid extracts (as tinctures of guaiac, benzoin, etc.), to aque- ous solutions. The combination of emulsions with alcoholic liquids or acids, or solutions of liquorice or glycyr- rhizin with acids or acid salts, tincture of iron with mucilage of acacia, infusions with ferric salts, etc. Volatile or fixed oils with aqueous liquids. Compound infusion of gentian with infusion of wild cherry or compound infusion of cinchona. Alcoholic tinctures and fluid extracts, with aqueous preparations, etc., etc. THE ART OF DISPENSING. 397 uniform mixture, the production of such being a violation of correct pharmaceutical procedure. In many cases it is impossible to combine the ingredients of a prescription to a clear mixture, owing to the insolubility of one or more of the substances present.* While there are cases in which it is proper or even necessary to separate such insoluble matters by filtration, there are many others in which this would be inadmissible, and would defeat the intentions of the prescriber. It is impossible to provide rules for all these cases. Each pre- scription has to be considered by itself. In general a prescription may be pronounced effectively incompatible, if any of its constituents would suffer changes which weaken or destroy the intended effect, or which produce effects not intended. Therapeutic Incompatibility.—This occurs where there is an antagonism of physiological action, one ingredient being, as it were, an antidote to the other. Difficulties that arise in this connection do not concern the apothecary, but lie solely within the power of the physician to correct. GENERAL OBSERVATIONS. It is important that the dispenser possesses an accurate knowl- edge of chemical reactions, solubilities and doses, in order that he may be able intelligently to compound the great variety of combinations prescribed, and discover any serious errors of judg- ment on the part of the prescriber. Physicians are rarely good chemists, hence the dispenser should be accordingly qualified. Before attempting to compound a mixture, the dispenser should first satisfy himself that no error has been committed on the part of the writer, in prescribing doses of powerful remedies, that is, excessive quantities which would result in endangering the life of the patient. In such instances the physician should be consulted. In cases of chemical incompatibility, the question that first arises is, whether this incompatibility is intentional or was un- foreseen on the part of the prescriber. For example, it will be seen at once that in mixture No. 85 the incompatibility was intentional, hence it is the duty of the dispenser to compound this to the best of his ability. In the case of the prescriptions No. 37, 48, 59, etc., the dispenser will perceive that the incompatibil- ity was unforeseen by the prescriber through his deficiency of knowledge concerning chemical reactions. Now an unforeseen incompatibility should not, under all circumstances, lead the dis- penser to refuse compounding a prescription; for in such cases as prescriptions No. 63, 79, the mixture should be dispensed with cer- tain precautions—as, to be shaken well before using. However, there are many cases in which the presence of a precipitate of a potent nature or other substances which have been set free in * Consult typical prescriptions given under this head 398 HANDBOOK OF PHARMACY. the mixture (for instance, iodine, bromine, chlorine, etc.), would lead the dispenser to refuse compounding it, because it is liable to endanger the life of the patient; as examples of such, consult prescriptions Nos. 46, 64, 68, 83, etc. The prescriber should not be troubled unless the prescription presents difficulties which the dispenser cannot overcome. Under no circumstances should the dispenser attempt substitution. In the compounding of various mixtures, precipitation is of very frequent occurrence. The question naturally arises, shall these precipitates be removed or not. Precipitates should not be removed, unless the solution is intended as an application to the eye or inflamed surfaces, for in such instances the particles of solid matter might prove a source of irritation. In mixtures intended for internal use, precipitation may arise from a variety of causes,* but such precipitates should not be removed, for as a rule we de- prive the mixture of a portion, or in some cases, of its entire activity. For example, should we filter such mixtures as No. 55, 56, 86, etc., we would obtain a clear inert solution. So also if the precipitate which results from the admixture of alcoholic solutions of resinous substances with aqueous liquid, be removed, we deprive the mixture of the greater part of its activity. In other cases, the precipitate resulting is inert, yet it may, when removed, retain active matter which is retained mechanically. Mixtures which contain precipitates of active or potent sub- stances are a source of danger, because, unless the mixture be shaken before using, so that the precipitate will become uni- formly suspended, the last doses may contain a poisonous quan- tity. In such instances the prescriber should be consulted. Some precipitates cannot be evenly distributed by shaking; examples are Nos. 28, 74, etc. Insoluble powders should never be added directly to a mixture, but they should be put in a mortar and reduced to the condition of a smooth paste with a portion of the mixture (syrup or muci- lage, if ordered), and then transferred to the bottle by washing the mortar with the remainder of the liquid. When such mix- tures are dispensed, the proper direction regarding the necessity of shaking the bottle should be given. Soluble salts should be powdered if necessary, and dissolved in a suitable amount of the most appropriate liquid constituent of the prescription, before the remainder of the ingredients is added, the liquid which dissolves the salt the least being added last. For example, if the salt is readily soluble in aqueous and but little soluble in alcoholic liq- uids, it should first be dissolved in one of the aqueous constituents, and the alcoholic ones added last. And if it be more soluble in alcoholic liquids, the aqueous constituents should be added last. Potent substances, such as poisonous alkaloids or their salts, should always be in solution before being added to the mixture. * See Precipitation, page 156. TYPICAL PRESCRIPTIONS. 399 TYPICAL PRESCRIPTIONS WITH EXPLANATORY NOTES. No attempt has been made to give the names of the ingredients in strictly pharmacopoeial Latin. As the prescriptions here quoted have been taken from promiscuous sources, the original phraseology or nomenclature has been preserved. (1) General Examples. R. Potassii Permanganatis, . . gr. xxx Auri et Sodii Chloridi, . . . . gr. iss Misce et fiant pilulae No. xl. 1. Organic matter should not be em- ployed in making these pills. Use infusorial earth, or kaolin, with petro- latum. 2. R . Liquoris Ammonii Acetatis, . . 60 Cc. Tincturse Ferri Chloridi, ... 30 Cc. Syrupi,q. s. ad 150 Cc. If the spirit of Mindererus be alka- line, and the ferric chloride free from excess of acid, a precipitation of ferric carbonate will occur. It is necessary to make sure that the former is at least slightly acid, or to render it so by the addition of a little acetic acid. 3. R. Pulv. Camphorae, Chloral Hydratis, ... aa 5 Gm. Cocainae Hydrochloratis, . . 5 Dg. M. Apply externally. These should be triturated together until a thick, clear fluid results. R . Hydrargyri Chloridi Corrosivi, gr. xvj Collodii, f 5 ss M. Ft. sol. 4. The mercuric chloride should be triturated in a small glass mortar with just sufficient alcohol for solution, then this added to the collodion. 5. R. Lupulini, 5.00 Pulveris Camphorae, 1.00 Terebinthinae Venetae, 8.00 M. Fiant pilulae No. cxxv. The lupulin should be rubbed in a mortar until a crumbly mass results, then the powdered camphor and tur- pentine added, and massed with mag- nesia. 6. R. Asafoetidae, 5j Aquae, M. F. enema. The asafoetida, in tears, should be reduced to a mass, and then triturated with a little water until a smooth paste results ; then the remainder of the water should be added, and the mixture finally strained. 7. R . Olei Terebinthinae, f 3 iss Syrupi Simplicis, Aquae Cinnamomi f 3 ij Olei Limonis, Tqyiij M. Sig.—Teaspoonful as directed. In this instance it would be advis- able for the dispenser to add powd. acacia (45 grains) sufficient to emulsify the oils. 400 HANDBOOK OF PHARMACY. 8. R. Copaibae, 10 Cc. Liquoris Potassae, 3 Cc. Olei Gaultheriae, 0.5 Cc. Glycerini, 15 Cc. Aquae Cinnamomi, .... 60 Cc. M. Sig.—Teaspoonful. Mix the liquor potassae with double its volume of cinnamon water in a bottle, then add gradually, with con- stant agitation, the copaiba and oil of Wintergreen, next the glycerin and re- mainder of the w7ater. The solution of potassa does not emulsify, but saponifies the copaiba. 9. R. Chloroformi, Acidi Nitrici, Creosoti, aa f 3 v M. For cauterizing. The nitric acid should be first added to the creosote and the mixture al- lowed to cool before the chloroform is added, otherwise the latter would be volatilized by the heat generated by the reaction of the other two in- gredients. 10. R. Sodii Biboratis, 3 iv Chloralis, 3 ij Atropinae, gr- iv Spiritus Vini Rectificati, . . . . Aq. Sambuci, . . . . q. s. ad M. Ft. lotio. This should be kept in a cool place, and well-stoppered, for chloroform will be developed by the action of the borax on the chloral. 11. If the acid be added to the chlorate followed by the water, a yellowish colored solution will result, which contains free chlorine. If the chlorate be dissolved in the water and the acid added last, a colorless solution will result. It is best to consult the phy- sician as to which is desired. R. Potassii Chloratis, 3 ij Acidi Hydrochlorici, f 3 ij Aquae, f £ viij M. Ft. gargarisma. R. Potassii Cyanidi, gj Morphinae Sulphatis, .... gr. ij Acidi Citrici, ijiss Syrupi, q. s. ad f § viij M. Ft. sol. Sig.—Coch. parv. t. i d. Hydrocyanic acid is developed ac- cording to the equation : 3KCN + H3C6H5O7 =3HCN + K3C6H6O7. 195 81 If 195 grains of KCN are capable of yielding 81 grains of HCN, then 60 grains of KCN will yield approxi- mately 2.5 grains of HCN, which is equivalent to about 130 minims of the official dilute hydrocyanic acid, leaving about two minims to the dose. The mixture may, however, be dispensed. 12. 13. R. Tincturae Ferri Muriatici, . . . Spiritus JEtherisNitrosi, . . . f£iv Mucilaginis Acaciae, fj|j Syrupi,q. s. ad When mixed in the order written, the mixture forms a jelly-like mass. If each of the constituents be diluted with an equal quantity of the syrup, and then mixed, a clear mixture will result. 401 TYPICAL PRESCRIPTIONS. 14. R . Extract! Buchu Fluidi, Extract! Cubebae Fluidi, . aa Olei Terebinthinae, f 3 ij Tincturae Hyoscyami, ... . Mucilaginis Acaciae, . . q.s. ad fsjiv Mix the fluid extracts, tincture and oil of turpentine ; then add this slowly to the mucilage, agitating constantly; a precipitate forms but can be readily diffused by agitation. Should we add the mucilage of acacia to the other mixed ingredients, the gum is pre- cipitated in a lumpy condition. 15. Solutions containing alkaloids are incompatible with alkalies or their carbonates, but in this case the in- compatibility may be neglected. There is about of a grain of strych- nine in the solution and this is precipitated by the sodium salt. But inasmuch as the alkaloid strychnine is soluble in 6700 parts of water, it will here remain in solu- tion, as there are over 9000 parts of water to each part of liberated alkaloid. R. Liquoris Strychnia), B. P., . . Sodii Bicarbonatis, gr. xv Aqua;, ad f R. Acidi Sulphurici, Acidi Nitrici, aa 10.00 Olei Terebinthinae, 30.00 Alcoholis, 50.00 M. Ft. sol. Owing to the violent reaction which ensues on mixing these acids with oil of turpentine great caution should be observed to prevent accidents. The mixed acids should be added to the oil slowly and cautiously. The dish containing the mixture should be placed in the open air and at least at arm’s length from the operator. After the mixture has cooled the alcohol may be gradually added. 16. 17. R. Acid. hyd. dil., Syrupi, fgij Here is an ambiguous abbreviation ; the dispenser would be at a loss as to whether hydrobromic, hydriodic, hy- J|drochloric or hydrocyanic acid was intended. The prescriber should be consulted before dispensing. R. Acidi Sulphurici Aromatici, . 8.00 Tincturae Cinchonae Composite, 30.00 Glycerini, ' 30.00 Aquae Destillatae 60.00 Quininae Sulphatis, 2.00 M. Ft. sol. Sig.—Cochleare parvum ter in die. 18. The quinine salt should be added to the compound tincture of cinchona in a graduate, and dissolved in the latter with the aid of the aromatic sulphuric acid, under stirring. Then the gly- cerin should be added and lastly the water. The glycerin prevents the formation of a precipitate from the tincture, when it is afterwards mixed with water. 19. R. Acidi Salicylici, Sodii Bicarbonatis, aa Aquae, f£vj M. Ft. sol. Sig.— 3j 3 t. d. The two substances may be mixed in a large mortar, and the water gradu- ally added, under stirring, until effer- vescence ceases. Or, the sodium salt may be mixed in a large capsule, on a water-bath, with the larger por- tion of the water, and the acid added until effervescence ceases. The solution will be of a dark color, due to the excess of alkali present at the close of the reaction :— NaHCO3 + HC7HSO3 = NaC7KsO, + CO2 + H2O 83.8 137.6 159.6 402 HANDBOOK OF PHARMACY. If the acid and the sodium salt were in molecular proportions, darkening of the solution could be prevented by dissolving the acid in boiling water (or adding it to boiling water, if there is too much to be dissolved), and then gradually adding the sodium salt to saturation. 20. The phosphoric acid must be free from “meta” or “ pyro ” acid or precipitation of iron will occur. If sufficient phosphoric acid is added, the red ferric chloride changes into colorless acid ferric phosphate. The quinine salt is dissolved in the tinc- ture, the strychnine salt in some of the water ; these are added to the syrup, followed by the balance of the water and lastly the acid. After a time the phosphates of the alkaloids will precip- itate. The mixture should be dispensed with a ‘ ‘ shake label. ’ ’ R. Tincturae Ferri Chloridi, . . . 10.00 Acidi Phosphoric! Diluti, . . 10.00 Quininae Suiphatis, 3.00 Strychninae Suiphatis, .... 0.10 Aquae Destillatae, 100.00 Syrupi Limonis, 80.00 M. Sig.—Dose, a teaspoonful. 21. R. Copaibae, 20.00 Tincturae Lavandulae Composite, Spiritus JEtheris Nitrosi, . . aa 10.00 Olei Gaultheriae, 0.50 Mucilaginis Acaciae, .... 30.00 Aquae Destillatae, . q. s. ut ft. 250.00 M. sec. art. Sig.—Coch. mag. t. i. d. To the mucilage contained in a bottle add the copaiba and oil in small por- tions at a time, shaking well after each addition. Then add the greater part of the water, next the tincture and spirit, all in portions, and lastly the remainder of the water. The balsam and oil are made into a sort of emul- sion with the mucilage, and the alco- holic liquids are added last. 22. R. Olei Jecoris Aselli, £3 viij Olei Amygdalae Amarae, Olei Gaultheriae, aa rrj_x Pepsini pulv., gj Pancreatini 3j Pulveris Acaciae, . .... 5 j Glycerini, f£j Syr. Hypophosphitura, .... f.Aj Acidi Phosphoric! Diluti, . . . f,5ss Aquae Destillatae, . q.s. ut ft. M. Ft. emulsio sec. art. Sig.—Coch. mag. t. i. d. Triturate one-half of the cod-liver oil and the essential oils with the pep- sin, pancreatin and acacia ; add at once one-half of the water, and triturate rapidly until an emulsion results. To this add gradually the remainder of the cod-liver oil, using a little water to prevent the emulsion from separ- ating (“ cracking ”)• Next incorpor- ate the syrup and the remainder of the water, leaving room for the acid, which is to be added last. (2) Pharmaceutical Incompatibility. 23. R. Tincturae Ferri Muriatici, ... Decocti Uvae Ursi, f 3 vj M. Signa.—Coch. mag. t. i. d. 24. R. Extracti Buchu Fluidi, Extracti Cubebae Fluidi, . aa f £ iss Aquae Cinnamomi, f 3 iij M. Sig.—To be well shaken. The tannin of the Uva Ursi forms an inky mixture (tannate of iron) with the ferric chloride. This forms a very unsightly mixture, owing to the separation of the resinous and oily matter when the fluid ex- tracts are added to the cinnamon water. TYPICAL PRESCRIPTIONS. 403 25. R . Tincturae Ferri Chloridi, ... f 3 iij Tincturae Guaiaci Ammoni- atae, Tincturae Aloes, f.?ss Syrupi, q. s. ad. fjjiv This forms a black mixture, the tincture of guaiac being pharmaceuti- cally incompatible with the ferric chlor- ide. Also both resinous tinctures pre- cipitate on coming in contact with an aqueous solution, in this case the syrup. 26. The chloral should be dissolved in the syrup, and the camphor, reduced to fine powder, be gradually mixed by trituration with the syrup, so that it may remain in suspension. The mix- ture should be directed to be well shaken before being used. B • Chloral Hydratis, gr. xl Camphorae, gr. x Syrupi Zingiberis, fjjij Aquae, q. s. ad. f ij B. Ferri et Quininae Citratis, . . 10.00 Acidi Phosphorici Diluti, . . 10.00 Tincturae Cardamomi Com- posite, 30.00 Syrupi Limonis, 20.00 Aquae, 100.00 27. The scale salt is dissolved in the water, followed by the syrup, tincture and acid in order. The mixture will not be clear because of the separation of the resinous matter of the carda- mom. The quinine phosphate which is formed, owing to its comparative insolubility, will generally precipitate. 28. B • Tincturae Guaiaci Ammoni- atae, Mucilaginis Acaciae, ... aa Potassii lodidi, Qij Tincturae Hyoscyami, Aquae Cinnamomi, . q. s. ad. . f 3 iij This forms an unsightly mixture, o wing to the separation of the resinous matter of the tincture of guaiac, which adheres to the sides of the bottle. 29. R. Copaibae, Spiritus yEtheris Nitrosi, . aa f£ iss Extracti Cubebae Fluidi, Tincturae Cinnamomi, . . aa f£iv Mucilaginis Acaciae, M. If the copaiba is emulsified by the mucilage, the addition of the alcoholic liquids will cause the gum to separate in a solid mass. As it stands it cannot be dispensed. R. Extracti Buchu Fluidi, Extracti Cubebae Fluidi, Mucilaginis Acaciae, . . . . aa Olei Terebinthinae, f 3 j Tincturae Hyoscyami, .... M. 30. The mucilage of acacia is intended to emulsify the turpentine. This emul- sion is, however, destroyed by the addition of the fluid extracts and tincture, the alcohol of which coagu- lates the acacia. R. Potassii Bromidi, 3 vj Aquae Camphorse, f 3 vj M. Ft. solutio. 31. The addition of soluble salts to cam- phor water causes the separation of the camphor, which floats on the sur- face of the mixture. The mixture should be well agitated before being taken. The addition of soluble salts to any of the medicated waters causes a separation of most of the volatile constituents. 404 HANDBOOK OF PHARMACY. li. Extracti Cannabis Indicae Fluidi, fgj Copaibae, Tincturae Guaiaci, f 3 ij Spiritus Terebinthinae, .... f 5 ij Tincturae Camphorae, fgss Syrupi Zingiberis, . . . q.s. ad. M. Ft. mistura. 32. Upon mixing the first five ingredi ents a clear or nearly clear solution will result. Upon adding this to the syrup, the resinous matters, camphor, copaiba and oil will separate, render- ing the mixture unsightly. R. Acidi Carbolici, 10.00 Collodii, 90.00 M. Ft. sol. 33. On mixing these, a jelly will be produced. (3) Chemical Incompatibility. 34. R. Argenti Nitratis, gr. v Tincturae Opii, f 3 iss Aquae Cinnamomi, . . q.s. ad Silver nitrate, when brought into contact with organic substances, suf- fers reduction to metallic silver. 35. R. Argenti Nitratis, 1.50 Sodii Chloridi, .60 Aqua, 200.00 Sig.—Use as a wash. There is sufficient sodium chloride present to decompose the entire amount of argentic nitrate. The pre- cipitate that forms being argentic chloride. The solution is practically inert. The reaction is as follows ; AgNO3 + NaCl = NaNO3 + AgCl. R. LiquorisPlumbi Subacetatis, . . Mucilaginis Acaciae, Aquae Destillatae, . . q. s. ad. f5 iv M. Ft. lotio. 36. The Goulard’s Extract produces a heavy white precipitate with the muci- lage of acacia. The mixture is incom- patible and should not be dispensed. 37. R . Strychnii Nitratis gr. ij Sol. Fowleri, M. Sig.—Gtt. v, t. i. d. This would prove to be a dangerous mixture if dispensed as written, for the alkalinity of the Fowler’s solu tion will cause the precipitation of the strychnine. The addition of a few drops of dilute nitric acid sufficient to retain the strychnine in solution would remove the difficulty. 38. R . Lithii Salicylatis, 3 ij Ferri et Ammonii Citratis, ... 3 iv Syrupi Limonis, Aquae, aa On bringing together the solutions of the first two ingredients, a reddish- brown precipitate of ferric, salicylate will form. The prescriber should be notified, if possible. If this is impos- sible, directions to shake the bottle should be added. 39. R. Cocainae Hydrochloratis, ... 2 Gm. Sodii Biboratis, 5 Dg. Aquae Destillatae, 100 Cc. M. Ft. sol. Sig.—Apply, as directed, to the eye. The cocaine is precipitated by the borax. Boric acid should have been used. TYPICAL PRESCRIPTIONS. 405 40. This mixture should not be dis- pensed, because the mercuric chloride will be entirely decomposed by the alkali hydrate and carbonate present in the aromatic spirit of ammonia, and the whole of the mercury be pre- cipitated ; part of which as ammoni- ated mercury. R. Hydrargyri Chloridi Corrosivi, . gr. iij Tincturae Cinchonae Compositae, f 5 vij Spiritus Ammoniae Aromatici, . M. Ft. sol. 41. R. Aluminis, gr. xxx Ammonii Carbonatis, . . . . gr. lx Tincturae Belladonnae, f 3 ij Glycerini, f J iij Infusum Senegae, . . q.s. ad On adding the solution of the am- monium salt to that of the alum, a precipitate of aluminum hydrate will fall, carrying with it the coloring matter and activity of the tincture of belladonna and infusion of senega. It is not advisable to dispense this. 42. R. Potassii Permanganatis, .... 3j Glycerini, fgj Aquae, f§ij The glycerin (being organic) causes decomposition of the permanganate ; instead of a bright, red-colored solu- tion, a colorless liquid with a dark precipitate (of manganic oxide) will result. R. Quininae Sulphatis, 1.30 Sodii Salicylatis, 15.50 Acidi Hydrobromici Diluti, . 30 Cc. Aquae, q. s. ad 250 Cc. 43. No matter how compounded, this mixture will contain a heavy precipi- tate of salicylic acid caused by the decomposition of the sodium salicylate by the hydrobromic acid. 44. R. Liquoris Hydrargyri Perchloridi, npx Potassii lodidi, gr. x Decocti Cinchona?, . . . q. s. Liquor Hydrargyri Perchloridi is official in the British Pharmacopoeia. It contains 10 grs. each of HgCl2 and NH4CI in 1 pint (Brit.) of water. The addition of potassium iodide to this will produce the reagent known as Mayer’s, which causes a precipitate with the alkaloids of the decoction of Cinchona to form. To render this as diffusible as possible it is best to add the solution of the mercury salt to a portion of the decoc- tion, and to dissolve the potassium iodide in another portion, then to mix the two gradually. 45. R. Ferri et Quininae Citratis, . . . 2.00 Potassii lodidi, 5.00 Syrupi, Aquae Destillatae, aa 30.00 Potassium iodide and the scale salt are incompatible, hydriodate of qui- nine being precipitated ; should the solution become warm, the precipitate would form a sticky mass. 46. R . Liquoris Ferri Perchloridi, . . . Potassii Bromidi, gr. xxx Aquae, fgij This mixture would not be safe to dispense if the ferric chloride contains an excess of acid, because of the libera- tion of bromine ; however, if the liquor be nearly neutral no difficulty will occur. 406 HANDBOOK OF PHARMACY. 47. R. Strychnin® Sulphatis, .... 0.065 Potassii Bromidi, 25.000 Aqu®, q. s. ad 250 Cc. M. Ft. sol. The strychnia sulphate is dissolved in a portion of the water, and the bro- mide in the remainder; a clear solu- tion will result. On standing over two days, crystals of strychniae hydrobro- mate will gradually separate. If one fluid ounce of alcohol be used in place of water, no precipitate will appear. 48. R. Tinct. Guaiaci Ammoniatae, . . 3 ij Mucilag. Acaciae,gij Quin. Sulph., gr. viij Acid. Sulph. Dil., giv Potass. Bicarb., Aquae,q. s. ad §iv The potassium bicarbonate being in excess will precipitate the quinine, and the resin of the ammoniated tinct- ure of guaiac; will be thrown out by the water. The mixture is hopelessly incompatible. 49. R. Acidi Carbolici,5.00 Sodii Bicarbonatis,20.00 Sodii Biboratis, 30.00 Glycerini, 360.00 On mixing these, active efferves- cence follows. Glycerin reacting with borax (sodium biborate) combines with part of the boric acid to form glyceryl metaborate (C3H5BO8) and sodium metaborate (NaBO2). The glyceryl metaborate, in presence of water, resolves itself into glycerin and boric acid ; the latter reacts with the sodium bicarbonate liberating carbon dioxide. 50. R. Quininae Bisulphatis,£ss Extracti Eucalypti Fluidi, ... Aquae,f£ij M. Ft. sol. Sig.—Cochleare parvum omni hora suma- tur. The tannic acid of the fluid extract unites with the quinine to form the insoluble quinine tannate, which sepa- rates in the form of an insoluble pre- cipitate. 51. R. Potassii lodidi, J)j Syrupi Ferri lodidi, .... f3 iv Aqua;, q. s. ad Syrup of Ferrous Iodide generally gives with potassium iodide a precipi- tate of ferrous, quickly changing to ferric carbonate or hydrate, because the KI is usually slightly alkaline. The addition of a little citric acid to the solution of the iodide will keep the mix- ture clear. 52. R. Plumbi Acetatis, T)j Tincturae Opii,ffi ij Syrupi, Aquae,q. s. ad M. Ft. lotio. The lead salt should be dissolved in an excess of the water and added to the diluted tincture. The precipitate formed should not be filtered off. 53. R. Argenti Oxidi,gr. vj Creosoti,gtt. vj Pulveris Radicis Glycyrrhizae, q. s. M. Fiant pil. No. vj. Silver oxide parts with its oxygen with great facility and often with explosive force when combined with organic substances. TYPICAL PRESCRIPTIONS. 407 R. Potassii lodidi, 12.0 Tr. Digitalis, 8.0 Extract! Erythroxyli Fluidi, . . 30.0 Sp. JEtherisNitrosi, 30.0 Glycerini, 30.0 Aquae, q. s. ad 125.0 54. When the ingredients are mixed in the order given and shaken, efferves- cence will occur, with evolution of nitrous fumes. Preparations contain- ing tannic acid react with nitrous ether, resulting in its decomposition. The spirit of nitrous ether should be added last and in portions, and the mixture should be allowed to stand uncorked for at least five hours for the escape of nitrous fumes. 55. R. Liq. Plumbi Subac. Dil., . . . Extract! Opii Aquosi, .... gr. xx M. Ft. lotio. The extract of opium, if not already in powder, should be reduced to a fine powder and triturated with the “lead water” gradually added. The turbid mixture should not be filtered. 56. R . Hydrargyri Chloridi Corrosivi, gr. j Liquoris Calcis, f§viij M. Ft. lotio. This forms the well-known “Yel- low Wash.” The yellow precipitate formed consists of mercuric oxide. This should not be filtered off. 57. R. Potassii lodidi, 3 iss Tincturae Ferri Perchloridi, . . fsjss Aquae, q. s. ad fgiv M. Signa.—Cochleare parvum ter in die. This mixture should not be dis- pensed, because of the presence of free iodine, liberated by the action of ferric chloride :— Fe2C16 + 2KI = I2 + 2FeCl2 + 2KC1. 58. R. Caffeinae Citratae, Ammonii Carbonatis, . . . . aa Q ij Elixir Guaranae, M. Signa.—Cochleare parvum p. r. n. The alkali carbonate precipitates the caffeine from both of the other ingre- dients. The patient should receive caution to shake the bottle before using. 59. On pulverizing these two together, the mixture will acquire a dark color, due to the separation of metallic mer- cury, mercuric bromide being formed at the same time. The powders should not be dispensed. R. Potassii Bromidi, gr. x Calomelanos, gr. iij M. Ft. pulv.; mitte tales vj. 60. R. Bismuthi Subnitratis, £j Sodii Bicarbonatis, .... gr. xxx M. Fiantpil. No. xx. These pills, after being made, swell considerably and disintegrate. This is due to the evolution of carbonic acid gas, caused by the reaction be- tween the subnitrate and the bicar- bonate. R. Potassii Bitartratis, £j “ lodidi, 3j Spiritus JEtheris Nitrosi, ... f £ iv Syrupi Aurantii, f o iv Aquae, q. s. ad f 61. The following reaction takes place, resulting in the decomposition of the nitrous ether and the liberating of free iodine from the iodide : KHC4H4Ofi+ C2H5NO2 + KI = K2C4H4Oe 4- C2H5- OH + NO + I. The mixture should not be dispensed. 408 HANDBOOK OF PHARMACY. R. Morphinae Acetatis, 0.05 Potassii lodidi, 2.00 Ferri Sulphatis, 1.00 Aquae, 50.00 M. Ft. sol. Sig.—Cochleare parvum omnibus noctibus. 62. The addition of potassium iodide to such metallic salts as iron or copper sulphate gives rise to the precipitation of the iodide of the metal as well as the liberation of free iodine. The mixture is incompatible and should not be dispensed. 63. R . Calcii Sulphidi, gr. xv Liquoris Hydrargyri Perchloridi, 3 vj Potassii lodidi, gr. xj Potassii Bicarbonatis, 3 iij Aquae Chloroformi, . . q. s. ad 5 viij If the calcium sulphide he added to the solution of the mercuric chloride, the latter will be decomposed with formation of mercuric sulphide. If the potassium bicarbonate be added to the mercuric chloride, mercuric car- bonate or oxychloride will be thrown down. However, as the amount of mercury salt present in the mixture is comparatively small, the mixture might be dispensed, with directions to shake the bottle. 64. R. Potassii Chloratis, 3 ij Syrupi Ferri lodidi, Vini Antimonii, f’3 ss Spiritus Chloroformi, .... f 3 ij Aqua*, q. s. ad. f§viij The addition of the potassium chlo- rate to the solution containing the ferrous iodide causes a liberation of free iodine. Under the circumstances the mixture would be dangerous to dispense. R. Liquoris Strychnin® Hydrochlor- atis, Liquoris Arsenicalis,rq, Ixx “ Potass®, Spiritus Vini Rectificati, . . . f§ iij 65. The strychnine is precipitated by the alkali, but redissolved by the alcohol. In compounding, add the liquor potassae last. 66. R. Tincturae Myrrhae, f 3 ij Morphinae Acetatis, gr. j Acidi Tannici, 3 ss Syrupi Zingiberis, M. Ft. sol. The tannin unites with the mor- phine, forming an insoluble precipi- tate. The tinct. of myrrh precipitates its resin when added to the syrup. A hopeless case of chemical and pharma- ceutical incompatibility. 67 There is an insufficient amount of alcohol for dissolving all of the iodine ; hence to the powdered iodine mixed with the alcohol, the oil of turpentine is slowly added. Ignition would result if the iodine and turpentine were brought together directly. R. lode mStallique, 10 Gm. Alcool, 30 Gm. Essence de t6r6benthine, . . 200 Gm. (To be used as spray). TYPICAL PRESCRIPTIONS. 409 68 R. Strychninae Hydrochloratis, . . gr. j Tincturae Cinchonae, Liquoris Ferri Dialysati, . . . f 3 iv Liquoris Potassii Arsenitis, . . f 3 ij Syrupi, Aquae,q. s. ad. M. Ft. solutio. Signa.—Capiat cochleare parvum post prandium. The dialyzed iron forms an insol- uble inert compound with the Fow- ler’s Solution. There is also danger of the strychnine being thrown out of solution by the alkali of the Fowler’s Solution, which would render the mixture dangerous to dispense, as the whole of the strychnine might possibly be given with the last dose. R. Liquoris Ferri Dialysati, . . . 25.00 Liquoris Potassii Arsenitis, . . . 4.00 Hydrated oxide of iron will separate, produced by the action of the alkali carbonate of the Fowler’s Solution. This ferric hydrate combines to the inert insoluble ferrous arsenate, with the arsenous acid of the Fowler’s Solution. Dialyzed iron is employed as an antidote for arsenical poisoning. 69. R. Potassii Cyanidi, Chloralis, &a 10.0 Unguenti, 30.0 On bringing the chloral and potas- sium cyanide in contact, decomposi- tion takes place at once, with the disengagement of hydrocyanic acid. In this case immediate reaction may be prevented by triturating the substances separately with a portion of the oint- ment. However, the ointment will turn brown in a short time, with disengagement of hydrocyanic acid. 70. 71. R. Zinci Phosphidi Potassii Permanganatis, . . aa gr. x Extracti Taraxaci, ... q. s. M. Ft. pil. cxx. The phosphide and permanganate should not be triturated together. Zinc phosphide, when combined with many organic extracts, gives oft’ phos- phoretted hydrogen (PH3), while potassium permanganate is immedi- ately decomposed under the same circumstances. This should not be dispensed. 72. R. Liquoris Arsenicalis (Fowl.), . . Hydrargyri Perchloridi, . . . . gr. j Aquae,q. s. ad f§iv M. Ft. mist. Sig.—f 3 iJ t- i- d- The alkali carbonate of the Fowler’s solution decomposes the mercuric chloride which has been dissolved in the water, with formation of mercuric carbonate or oxychloride. The pre- scriber should have chosen Liquor Acidi Arsenosi. If circumstances are such that the mixture must be dispensed at once without consulting the prescriber, the patient should be instructed to shake the bottle, in order to avoid the risk of taking the entire precipitate with the last dose. 73. The alkali carbonate of the Fowler’s solution precipitates a portion of the iron first as ferrous carbonate, which soon loses its CO2, and eventually changes to ferric hydroxide. The iodine liberated unites with the potassium. The intentions of the physician are defeated by this incompatibility, hence he should be consulted. Otherwise nothing R. Syrupi Ferri lodidi, Liquoris Potassii Arsenitis, aa f 3 ij Syrupi Tolutanae, . . q. s. ad 410 HANDBOOK OF PHARMACY. would be left for the dispenser to do but to compound the mixture by diluting each of the active ingredients with half of the Syrup of Tolu and mixing gradually. The proper precautions in regard to shaking before using should be observed. R. Quinin® Sulphatis, . . . . 2.0 Gm. Tinctur® Cantharidis, ... 3.5 Cc. Spiritus Rosmarini, . . . 15.0 Cc. Infusi Salvi®,120.0 Cc. M. Ft. lotio. Sig.—Apply to scalp as directed. 74. The tannic acid in the infusion forms an insoluble mass with the quinine. The mixture is unmanage- able. 75. Spirit of nitrous ether effervesces quite violently when added to fluid extract of buchu or uva ursi, or any preparation containing tannin. The potassium citrate, when alkaline, causes the decomposition of the nitrous ether. R. Extracti Bnchu Fluidi, . ... f,5j Potassii Citratis, 3 iij Spiritus JEtheris Nitrosi, ... Syrupi Limonis, . . q. s. ad 76. R. Hydrargyri lodidi Rubri, . . . 0.20 Potassii lodidi, 12.00 Ext. Cinchona: Fluidi, . . . .20.00 Syrupi, 150.00 M. Ft. sol., cujus aeger cap. coch. parvum ter in die in cyatho vinario aq. frig, postjentac., prand. et cenam. The mercuric iodide and potassium iodide are dissolved in the smallest possible amount of water, replacing an equal bulk of syrup. Next the fluid extract is gradually added. The whole of the cinchona alkaloids contained in this will be precipitated by the po- tassio-mercuric iodide. A “shake” label should be attached. 77. R. Plumbi Acetatis, gr. xl Bismuthi Subuitratis, 5 ss Acidi Sulphurici Aromatici, . , Quininas Sulphatis, gr. xx Aquae Anisi, .... q. s. ad f iv M. Ft. sol. Upon addition of the aromatic sul- phuric acid to the solution of the lead salt, lead sulphate will be precipitated. As this would be likely to be all taken with the last dose, and as it is, more- over, liable to remain for a long time in the digestive organs, and apt to cause lead-poisoning, the mixture should not be dispensed without the prescriber being consulted. If this be impossible, the lead sulphate should be removed by filtration. 78. R. Alu minis,£j Plumbi Acetat.,3 v Aquae Destillatae, M. Ft. lotio. Each of the salts is dissolved in a separate portion of water. On mixing these solutions a heavy precipitate of lead sulphate falls, resulting from the reaction between the aluminum and potassium sulphate and the lead acetate. Unless the prescriber directs otherwise, the lead sulphate should not he removed by filtration, but directions to shake the mixture before use should be attached. TYPICAL PRESCRIPTIONS. 79. 411 R. Acidi Tannici, gr. x Quininae Sulphatis, gr. iij Acidi Sulphurici Diluti, .... tqj’j Aquae, q s. ad f§j The quinine salt should be dissolved in one-half of the water by aid of the dilute acid ; to this add slowly the solution of the tannic acid in the re- mainder of the water ; a light floccu- lent precipitate of quinine tannate will result. Dispense with a shake label. 80. R. Olei Morrhuae, Aquae Calcis, f.?iv Solve et. adde :— Syrupi Ferri lodidi, f 3 iv Olei Cinnamomi, f 3 ss Syrupi, f 3 xij The lime-water serves the purpose of emulsionizing, or, rather, partially saponifying, the cod-liver oil. But on bringing this mixture in contact with the ferrous iodide, ferrous hydrate will be precipitated, while the iodine will combine with the calcium. 81. R . Liquoris Arseni et Hydrargyri lodidi, * . . 10 Cc. Potassii lodidi, 5 Gm. Quininae Sulphatis, 2 Gm. Acidi Sulphurici Diluti, . . . q. s. Aquae, q. s. ad 300 Cc. The Donovan’s Solution forms with the quinine an insoluble compound which precipitates. The quinine solution should be added last and in small portions to the mixture in order to obtain the precipitate in as finely subdivided a condition as possible. 82. R. Sodii Salicylatis, 8 Gm. Quininae Sulphatis, 5 Dg. Liquoris Ammonii Acetatis, . 10 Cc. Syrupi Zingiberis, . . q. s. ad 60 Ce. M. Sig.—Teaspoonful in water. The two salts are dissolved in the solution of ammonium acetate, which, for this purpose, must be neutral. The solution is then mixed with the syrup. If the spirit of Mindererus were acid, some of the salicylic acid would be thrown out of solution. On diluting the finished, clear mixture with water, insoluble quinine salicylate precipitates. 83. R. Liquoris Acidi Arsenosi, ... 1’5 j Hydrargyri Bichloridi, . . . . gr. j Strychnin® Sulphatis,gr. j Spiritus Vini Rectificati, . . . . fsjj Aqu®,fgj When strychnine and mercuric chloride are brought together in solu- tion in the presence of hydrochloric acid, a dense precipitate of strychnine chloro-mercurate is thrown down. This is insoluble in water, but soluble in alcohol. In this mixture there is not sufficient alcohol to effect solution. dispensing this, or, in fact, any mixture which contains a potent substance in the form of an insoluble precipitate, a great risk will be incurred by the dispenser, for any carelessness on the part of the patient, in omitting to shake the bottle, may be attended with serious results. R . Potassii Bromidi, Chloralis Hydrat., . . . . aa 10 Gm. Tincturae Opii Camphoratae, Syrupi Zingiberis, . . . . aa 50 Cc. 84. On standing, chloral-alcoholate will separate as oily drops. Certain salts, as KBr, NaBr, NaCl, MgSO,, etc., cause the formation of chloral alco- holate (CC13COH,C2H6O) in hydro- 412 HANDBOOK OF PHARMACY. alcoholic solutions with chloral. While this chloral alcoholate acts as an hypnotic, it is harsh in its action, leaving unpleasant secondary effects. Alcoholic prepara- tions should not be prescribed with chloral, especially not in connection with the bromides of sodium and potassium, because, if the solutions used are at all con- centrated, the chloral will separate as alcoholate, float on the surface, and a great risk will be incurred of giving a large overdose if the patient is not very careful to shake the bottle before taking a dose. This forms an unsightly and in- compatible mixture, yet should be dispensed unfiltered. The zinc sul- phate and lead acetate* react, produc- ing the insoluble lead sulphate. Lead acetate is incompatible with the wine of opium and tincture of catechu. The zinc sulphate and lead acetate should each be dissolved in two ounces of water and mixed, and the wine of opium should be diluted with an ounce of water and added, followed by the tincture of catechu, likewise diluted. This yields a brownish colored liquid, holding a fine precipitate in suspension. R. Zinci Sulphatis, Plumbi Acetatis, aa gr. x Vini Opii, Tinctures Catechu aa f 3 ij Aquae, q. s. ad M. Ft. sol. 85. R . Hydrargyri Chloridi Corrosivi, gr. iij Aquae Destillatae, f3 iss M. ft. solutio et adde : — Albuminis Ovi, f3iss Aquae Destillatae, . . . ql s. ad f 3 v Misce, cola, et adde :— Aquae destillatae, . . . q. s. ad f3 x 86. On adding the solution of the mer- curic chloride to the solution of the egg albumen, an insoluble compound forms, which, when the mixture is strained, removes the entire amount of mercuric chloride, resulting in an inert solution. 87. R . Hydrargyri Chloridi Corrosivi, Ammonii Chloridi, .... ail gr iij Aquae Destillatae, f 3 iss M. ft solutio et adde : — Albuminis Ovi, fjiss Aquae Destillatae, . . . q. s. ad f 3 v Misce. cola, et adde : — Aquae Destillatae . . . q s ad f 3 x The ammonium chloride assists the solution of the mercuric chloride in the water. It also prevents the for- mation of the insoluble compound of the mercuric salt with the albumen * Lead Acetate is incompatible with such preparations as contain organic acids, as it forms insoluble compounds with these. In the above instance it unites, forming an insoluble compound, with the meconic acid of the opium and the catechuic acid of the catechu. Lead Subacetate, being of an alkaline reaction, precipitates alkaloids, organic acids, solutions of gummy and coloring matters, tannins, albumen, etc. CHAPTER XXXVII. VOLUMETRIC QUANTITATIVE ANALYSIS. Volumetric Analysis is the method by which we determine the quantity of certain substances by means of the volume of selected reagents which are required to perform a given reaction. The process of adding the liquid reagent from graduated mea- sures is called Titration. The strength of a volumetric solution as compared with that of another, or, in other words, its ratio to the latter, is called its Titer. A Volumetric or Standard Solution is a solution of definite strength, which is made by dissolving a given weight (in grammes) of a reagent, in a definite volume (in cubic centimeters) of water. These solutions are usually made by dissolving the molecular weight of a reagent in grammes or a fraction thereof in 1000 cubic centimeters (one liter) of water. The following abbreviations are in use: N or j (normal). “Volumetric solutions are designated as N normal ( -) when they contain in 1 liter the molecular weight of the active reagent, expressed in grammes, and reduced to the valency corresponding to one atom of replaceable hydrogen or its equivalent. “ Thus, hydrochloric acid, HC1 = 36.37, having but one H atom replaceable by a basic element, has 36.37 Gm. of HC1 in 1000 Cc. of the normal volumetric solution; while sulphuric acid, H2SO4 = 97.82, having two replaceable II atoms, contains only one-half this number, or 48.91 grammes of H2SO4 in 1000 Cc. of its normal solution. Potassium hydrate, KOH = 55.99, has but one K to replace one H in acids, hence its normal solu- tion contains 55.95 grammes of KOH in one liter.” 1T (decinormal) — Solutions which contain in one liter one-tenth of the quantity of the active reagent in the normal solution. 156 (cen^normad) = Solutions which contain in one liter one hun- dredth of the quantity of the active reagent in the normal solution. N (double normal) = Solutions which contain in one liter twice the quantity of the active reagent in the normal solution. N 2 (semi-normal) = Solutions which contain in one liter one-half of the quantity of the active reagent in the normal solution. 413 414 HANDBOOK OF PHARMACY. An indicator is a substance which is added to the solutions, dur- ing titration, for the purpose of showing, by a change of color (or other visible change), the exact point at which the reaction is com- plete. The principal indicators employed are:— (1) Solution of Litmus (Test solution, U. S. P.). This turns red with acids and blue with alkalies. (2) Alcoholic Solution of Phenolphtalein (Test solution U. S. P.). —This is colorless with acids and turns deep red with alkali hydrates and carbonates; bicarbonates and most other salts do not produce this color. It is not reliable when alkaline salts of ammonium or phosphoric acid* are present. (3) Solution of Methyl- Orange (Test solution U. S. P.).—This solu- tion acquires a yellow color in contact with alkali hydrates, car- bonates, or bicarbonates. With the inorganic acids the solution acquires a crimson color. It is indifferent to carbonic acid and should not be used with organic acids. (4) Solution of Rosolic Acid in diluted alcohol (Test solution U. S. P.).—The solution turns violet with alkalies and yellow with acids. (5) Decoction of Brazil- TFbod (Test solution U. S. P.).—This is a very sensitive indicator, especially adapted in the estimation of alkaloids. The solution turns purplish-red with alkalies, and yellow with acids. (6) Tincture of Cochineal (Test solution U. S. P.).—The solution turns violet with alkalies and yellowish-red with acids. It is employed as an indicator when ammonia or alkaline earths are present. (7) Starch Mucilage (Test solution U. S. P.).—The cold solution turns blue in the presence of free iodine. (8) Solution of Potassium Chromate (Test solution U. S. P.).—The solution gives a red color with silver nitrate. When any halogen salts are present, the red color does not appear until every trace of the halogen has combined with the silver. (9) Solution of Potassium Ferricyanide (Test solution U. S. P.).— This gives a blue color or precipitate with ferrous, and only a clear brown solution with ferric salts. This indicates that all of the ferrous salt has been oxidized to ferric, when it ceases to impart a blue color to the solution. INDICATORS. * Excepting in case of an orthophosphate M2HP0<—See Estimation of Phosphoric Acid. VOLUMETRIC ANALYSIS. 415 APPARATUS EMPLOYED. Measuring Flasks and Cylinders.—For the preparation of volumetric solutions we employ accurately graduated flasks or cylinders. The flasks (Fig. 384) are made of various sizes, usually of the capacity of 250, 500 and 1000 cubic centimeters (at 15° C. or 59° F.), which is indicated by a mark on the neck. Graduated cylinders (Fig. 385) are also employed for this purpose. Pipettes.—These are instruments (see page 164) graduated to deliver definite volumes of fluids. They are constructed to hold, Fig. 385. Fig. 384. Measuring Flasks. Measuring Cylinder. when the fluid is drawn up to the mark indicated on the stem, various volumes, as 1 cubic centimeter or fraction thereof, 5, 10, 15, 20, 25 or 50 cubic centimeters. Burettes.—These are long tubes, usually of a capacity of 25, 50 or 100 cubic centimeters, and graduated into divisions of 1 Cc. or fractions thereof (one-fifths or one-tenths). These are employed for measuring out standard solutions. They are gradu- ated between two points on the cylinder, the upper one (0) begin- ning a short distance below the upper extremity, the lower one (50 or 100 Cc.) being situated a short distance above the point where the tube begins to narrow toward the outlet; the fluid can be measured only between these points (0 and 50, Fig. 387). The 416 HANDBOOK OF PHARMACY. burettes are usually fitted below with a pinch-cock arrangement (Fig. 386), or with a glass stop-cock (Fig. 388, a-6); the former, when pressed, or the latter when turned, allows the fluid to flow out at any speed desired. The pinch-cock arrangement is applied to the simpler forms of burettes in which a short heavy piece of rubber tube is slipped over the narrow neck (a, Fig. 386) of the lower end of the burette, and tied, if necessary (6, Fig. 386). Into the other end of the rubber tube is slipped a short piece of glass tubing (d, Fig. 386) of small caliber, drawn to a fine orifice; between the extremities of the rubber, a pinch-cock* (c, Fig. 386) is placed, Fig. 387. Fig. 388. Burettes with Glass Stop-Cocks. Burette Operated with Pinch-Cock. Device for Dropping from Burette. and by pressing the two tips it is caused to open and permit the flow of liquid from the burette. Fig. 387 illustrates the same form, in which the pinch-cock is replaced by a small glass marble, or short rounded piece of glass rod of sufficient size so that when it is inserted inside the tube, it will retain its position and not permit the liquid to pass through. It is operated by pressing the rubber tube slightly together at this point, forming a narrow channel, which permits the fluid to flow out at any rate desired. Beginners find it at first somewhat difficult to read off the height of the column of fluid correctly. On holding the burette so that the surface of the fluid is on a level with the eye, it * See also page 90, Figs. 138, 139. 417 VOLUMETRIC ANALYSIS. will present an appearance like unto that shown in Fig. 389, this being known as the meniscus. It is a matter of some differ- ence, whether the height of the meniscus is read off on a line parallel with the upper edge o or the lower one at u. But if we begin by reading off from one of these edges, we must use the same height in all our other readings. To facilitate the accuracy of read- ing, various devices have been proposed; one of the simplest (for clear liquids) is that shown in Fig. 390, in which a piece of paper half black and half white is held against the back of the burette, the upper edge of the black portion being held a few millimeters below the level of the liquid; the lower concave curve of the meniscus then appears as a sharp black line which enables the operator readily to note the height of the fluid. Fig. 389. Fig. 390. Meniscus. Reading of Meniscus. Some burettes are specially constructed for the purpose of facili- tating reading, being provided with white enameled sides and dark blue background (Fig. 391); the reflection of the dark line in the background with the meniscus produces an appearance as shown in Fig. 392. The point of the narrowest portion cor- responds to the middle of the meniscus, which can be read off with great accuracy. A very convenient instrument for avoid- ing the meniscus altogether, and which can be employed with accuracy for all kinds of fluids, is the Erdmann float (Fig. 393). This consists of a small cylindrical closed tube, sufficiently weighted so that it will float upright, around the middle of which a line is scratched ; this is placed in the fluid in the burette and the height is read off by comparing the ring (scratch) on the float with the divisions on the burette. 418 HANDBOOK OF PHARMACY. In the operation of titrating, the substance to be titrated, if in dry or concentrated form, should always be dissolved in, or diluted with water. Beakers or flasks, placed on a sheet of white paper, or a porcelain dish should be employed for holding the solution; the operation should be conducted with as much light as possible, in order to distinguish clearly the change of color, etc., which denotes the end point of the reaction. In the begin- ning of the operation, the standard solution may be added rapidly under constant stirring; towards the end it should be added more cautiously, and finally only in drops. Thus in adding a standard solution of an alkali to an acid (diluted), with phenolphtalein as indicator, each drop of the alkali solution will produce a red color which almost immediately disappears. To- Fig. 391. Fig. 392. Fig. 393. Effects produced by Meniscus. Erdmann Float. ward the end of the reaction, however, tliis red color disappears less rapidly; then the operator should proceed very cautiously. Just sufficient of the reagent should be added to produce the desired color (not too intense), or to cause decolori- zation, as the case may be. With such indicators as phenol- phtalein or litmus, which produce marked changes in color, little difficulty is experienced in distinguishing the end-point of the reaction. Other indicators, however, such as methyl- orange, brazil wood, cochineal, etc., cause considerable difficulty for the inexperienced, the change of color being often very gradual and sometimes indistinct. It is best for the operator to take two beakers or test tubes containing the same bulk of water as there is fluid for assay, acidulate one with the standard acid solution, and render the other alkaline to an equal degree ; then add to both an equal amount of the indicator. On placing these Burette (Enameled Sides). VOLUMETRIC ANALYSIS. 419 beside the sample to be assayed the change of color can be accur- ately noted by comparison. Fig. 394. Fig. 395. Burette Stand. Burette in Position. PREPARATION OF STANDARD SOLUTIONS, WITH EXERCISES. As before stated, these solutions are prepared by dissolving a given weight, that is, usually, the molecular weight of the reagent, expressed in grammes, in 1000 Cc. of water. Thus in order to prepare a standard normal solution of hydrochloric acid, we should weigh off (assuming that we had an acid of the exact strength required) an amount containing 36.37 Gm. of the 420 HANDBOOK OF PHARMACY. absolute acid, place it into a flask, and dilute it with water to one liter. Then if 1000 Cc. of the solution contain 36.37 Gm. of absolute HC1. 1 Cc. “ “ “ “ 0.03637 “ “ “ “ From the equation. HCl + NaOH = NaCl + H2O Hydrochloric Sodium Sodium Water. Acid. Hydrate. Chloride. 36.37 39.96 we learn that 36.37 Gm. Hydrochloric Acid is equivalent to 39.96 Gm. of Sodium Hydrate ICc. or 0.03637 Gm. “ “ “ “ “ 0.03996 Gm. of “ a; Cc. of “ “ “ “ x X 0.03996 Gm. of “ “ If we know the number of cubic centimeters of normal acid solution, the amount of alkali is readily calculated. The second clause of the definition of Volumetric Solutions reads thus, “ and reduced to the valency corresponding to one atom of replaceable hydrogen or its equivalent.” When we desire to prepare a normal sulphuric acid solution we weigh off an amount equivalent to 48.91 Gm. (| of 96.82) of the absolute acid, and dilute it to one liter; here we have taken one- half of the molecular weight, for sulphuric acid, being bivalent, corresponds to two atoms of replaceable hydrogen. Thus H2SO4 4- 2NaOH = Na,SO4 + 2H2O Sulphuric Sodium Sodium Water. Acid. Hydrate. Sulphate. 97.82 2 X 39.96 One molecule (97.82 p.) of Sulphuric Acid is equivalent to two molecules (2 X 39.96 p.) of Sodium Hydrate. One-half of a molecule (48.96 p.) of Sulphuric Acid is equivalent to one molecule (39.96 p.) of Sodium Hydrate. 1000 Cc. (N V. S.) containing 48.91 Gm. Sulphuric Acid = 39.96 Gm. of Sodium 1 Hydrate. 1 Cc. “ “ 0.04891 Gm. Sulphuric Acid = 0.03996 Gm. of So- dium Hydrate. x Cc. of normal Sulphuric Acid Solution = x X 0.03996 Gm. of Sodium Hydrate. The estimation of acids or alkalies is known as Acidimetry and Alkalimetry. In order to prepare the various standard solutions, we must select some substance which can be readily had in pure and undiluted form. For this purpose crystallized oxalic acid answers best. Its solution must be carefully and accurately prepared, for upon this all other normal acid and alkaline stand- ard solutions are based ; hence any inaccuracy in this standard would be carried over into all others. (1) Normal Oxalic Acid Volumetric Solution. H2C2O4 4- 2H2O = 125.7 62.85 Gm. in 1 Liter. Weigh 62.85 Gm.* of pure oxalic acid ih crystals and transfer * “ This is frequently rounded off to 63 Gm. when a delicate balance and exact weights are not at hand.” VOLUMETRIC ANALYSIS. 421 it without loss to a measuring flask or cylinder of one liter capac- ity, add enough distilled water to dissolve it, then, maintaining the temperature at or near 15° Cc. or 59° F., add water to make the volume measure exactly 1000 cubic centimeters. One Cubic Centimeter of Normal Oxalic Acid V. S. is the equivalent of: Gramme. Oxalic Acid, crystallized, H2C2O4 + 2H2O 0.06285 Ammonia Gas, NH30.01701 Sodium Hydrate, NaOH 0.03996 Potassium Hydrate, KOH 0.05599 Potassium Permanganate, KMnO40.03153 (a) Estimation of Alkali Hydrates. Exercise.—In about 30 Cc. of water 0.4 Gm. of Soda were dis- solved, with phenolphtalein as indicator; 9 Cc. of normal oxalic acid V. S. were required to neutralize it (sufficient to discharge the pink color): What was its percentage in pure NaOH ? According to the equation. H2C2O4 + 2H2O + 2NaOH = Na.2C2O4 + 4H2O Oxalic Acid. Sodium Hydrate. Sodium Oxalate. Water. 125.7 2 X 39.96 1000 Cc. (— V. S.) containing 62.85 Gm. of Oxalic Acid are equivalent to 39.96 Gm. 1 of Sodium Hydrate. 1 Cc. “ “ 0.06285 Gm. of Oxalic Acid is equivalent to 0.03996 Gm. of Sodium Hydrate. 9 Cc. of the normal Oxalic Acid, V. S. = 9 X 0.03996 = 0.3576 + Gm. of So- dium Hydrate. That is, 0.4 Gm. of the Soda taken contains 0.3576 Gm. of pure substance, hence 0.4 : 0.3576 — 100 : x; x — 89.4 per cent. (2) Decinormal Oxalic Acid Volumetric Solution. H2C2O4 + 2H2O = 125.7. 6.285 Gm* in 1 Liter. Dissolve 6.285 Gm.* of pure oxalic acid in enough water to make, at or near 15° 0. (59° F.), exactly 1000 Cc. One Cubic Centimeter of Decinormal Oxalic Acid V. S. is the equivalent of:— Gramme. Oxalic Acid, crystallized, H2C2O4 + 2H2O 0.006285 Ammonia Gas, NH3 0.001701 Calcium Hydrate, Ca(OH)2 0.003691 Potassium Hydrate, KOH 0.005599 Potassium Permanganate, KMnO4 0.0031534 Sodium Hydrate, NaOH 0.003996 The decinormal solution is generally preferred to the normal, because the stronger solution has the tendency to crystallize at the point of the burette, in consequence of which particles of the solid matter are liable to drop into the solution to be assayed. * “ Generally rounded off to 6.3 Gm., when a delicate balance and exact weights are not available.” 422 HANDBOOK OF PHARMACY. ALKALIMETRY. Any of the normal or decinormal acid solutions may be em- ployed for estimating the strength of alkalies or alkaline solutions. The substance or fluid is quickly weighed, dissolved or mixed with the necessary volume of water, then a few drops of phenol- phtalein solution are added, or in presence of carbonates, methyl- orange solution, and the standard acid solution then added until the red color of the former just disappears or the yellow color of the latter changes to red. Great care must be employed not to add any more of the reagent than just necessary to produce or discharge a given color. Exercise.—50 Cc. of Solution of Lime (Lime Water), with phen- olphtalein as indicator, required 20 Cc. of decinormal oxalic acid V. S., for complete neutralization (sufficient to discharge the pink color). What percentage of Calcium Hydrate does the solution contain? According to the equation :— H2C2O4 + 2H2O + Ca(OH)2 = CaC2O4 + 4H2O Oxalic Acid. Calcium Hydrate. Calcium Oxalate. Water. 125.7 73.83 125.7 parts of Oxalic Acid are equivalent to 73.83 parts of Calcium Hydrate 62.85 parts of Oxalic Acid are equivalent to 36 91 -j- parts of Calcium Hydrate. 1000 Cc. (-2L V. S.) containing 6.285 Gm. of Oxalic Acid are equivalent to 10 3.691 4- Gm. of Calcium Hydrate. 1 Cc. “ “ “ 0.006285 Gm. of Oxalic Acid is equivalent to 0.003691 Gm. of Calcium Hydrate. 20 Cc. of the decinormal Oxalic Acid, V. S. = 20 X 0.003691 + = 0.07382 + Gm. of Calcium Hydrate. That is, 0.07382 4- Gm. of Calcium Hydrate is contained in 50 Cc. (about 50 Gm.) of Solution of Lime, hence 50 : 0.0738 = 100 : x ; x — 0.14 per cent. True percentage by weight would require that the specific gravity of the solution be taken into consideration. In this case, where it is practically identical with that of water, it may be neglected. Inasmuch as sulphuric acid varies in strength, and the accurate weighing of quantities corresponding to definite amounts of absolute acid is next to impossible, the strength of a diluted acid is adjusted by means of a standard solution of potassium hydrate, which in turn owes its accuracy to having been standardized by oxalic acid (see Normal Potassium Hydrate V. S., page 426). The Pharmacopoeia gives the following directions:— (3) Normal Sulphuric Acid. H2SO4 = 97.82. 48.91 Gm. in 1 Liter. “ Carefully mix 30 Cc. of pure, concentrated sulphuric acid (of specific gravity 1.835) with enough water to make about 1050 Cc., and allow the liquid to cool to about 15° C. (59° F.). Place 10 Cc. of this liquid (which is yet too concentrated) into a flask, add VOLUMETRIC ANALYSIS. 423 a few drops of phenolphtalein T. S., and afterwards, from a burette, normal potassium hydrate V. S., shaking after each addition, and regulating the flow to drops towards the end of the operation, until the red color produced by its influx no longer disappears on shaking, but is not deeper than pale pink. Note the number of Cc. of potassium hydrate V. S. consumed. Then dilute the sul- phuric acid solution so that equal volumes of this and of normal potassium hydrate V. S. exactly neutralize each other. Example.—Assuming that 10 Cc. of the acid solution first pre- pared had required exactly 11.2 Cc. of normal potassium hydrate V. S., each 10 Cc. of the former must be diluted to 11.2 Cc., or each 1000 Cc. to 1120 Cc. After the liquid is thus diluted, a new trial should be made in the manner above described, in which 50 Cc. of the acid solution should require for neutralization exactly 50 Cc. of potassium hydrate V. S. If necessary, a new adjustment should be made to render the correspondence perfect.” One Cubic Centimeter of Normal Sulphuric Acid is the equivalent of: Gramme. Sulphuric Acid, absolute, H2SO4 0.04891 Ammonia Gas, NH3 0.01701 Ammonium Carbonate, (NH4)2CO3 0.042935 Ammonium Carbonate [U. S. P.], NH4HCO3.NH4NH2CO2 . . 0.05226 Lead Acetate, crystallized, Pb(C2H3O2)2 + 3H2O 0.18900 Lead Subacetate, assumed as Pb2O(C2H3O2)2 0.13662 Lithium Benzoate, LiC7H5O2 (to be ignited), 0.12772 Lithium Carbonate, Li2CO3 0.036935 Lithium Citrate, Li3C6H5O7 (to be ignited), 0.0698566 Lithium Salicylate, LiC7H5O3 (to be ignited), 0.14368 Potassium Acetate, KC2H3O2 (to be ignited), 0.09789 Potassium Bicarbonate, KHCO3 0.09988 Potassium Bitartrate, KHC4H4OB (to be ignited), 0.18767 Potassium Carbonate, anhydrous, K2CO3 0.068955 Potassium Citrate, cryst., K3C6H5O7 + H2O (to be ignited), . 0.10786 Potassium Hydrate, KOH 0.05599 Potassium and Sodium Tartrate, KNaC4H4O6 4~ 4H2O (to be ignited), 0.14075 Sodium Acetate, NaC2H3O2 + 3H2O (to be ignited), 0.13574 Sodium Benzoate, NaC7H5O2 (to be ignited), 0.14371 Sodium Bicarbonate, NaHCO3 0.08385 Sodium Borate, crystallized, N’a2B4O7 + 10H2O 0.19046 Sodium Carbonate, anhydrous, Na2CO3 0.052925 Sodium Carbonate, crystallized, Na2CO3 + 10H2O 0.142725 Sodium Hydrate, NaOH 0.03996 Strontium Lactate, Sr(C3H5O3)2 (to be ignited), 0.13244 Exercise.—Exactly 1.7 Gm. of Stronger Ammonia Water was diluted with water, rosolic acid added as indicator, and normal solution of sulphuric acid added until the violet-red color gave way to yellow, 28 Cc. of the normal solution having been con- sumed. What is the percentage strength in ammonia gas? H2SO4 + 2NH3.H2O = (NH4)2SO4 + 2H2O Sulphuric Acid. Ammonia Water. Ammonium Water. 97.82 2 X 17 Sulphate. 424 HANDBOOK OF PHARMACY. 1000 Cc. (N V. S.) containing 48.91 Gm. of Sulphuric Acid are equvialent to 1 17 Gm. of Ammonia Gas. 1 Cc. “ “ “ 0.04891 Gm. of Sulphuric Acid is equivalent to 0.017 Gm. of Ammonia Gas. 28 Cc. of normal Sulphuric Acid V. S. = 28 X 0.017 = 0.476 Gm. Ammonia Gas. Since 1.7 Gm. of Ammonia Water has been taken, then 1.7 : 0.476 = 100 : x; x = 28 per cent. (6) Estimation of Alkali Carbonates. Exercise.—Let it be assumed that two samples of sodium bicar- bonate, each of 0.85 Gm. are to be assayed, to determine the per- centage of pure salt. Here it should be stated that two methods are available for assaying alkalies in presence of carbonic acid. One is the cold method, with methyl-orange as indicator, since this is not sensi- tive to carbonic acid. The other is the hot method, with phenol- phtalein as indicator, which will not strike a pink color with alkalies, until all the carbonic acid has been expelled by heat. Let it now also be assumed that we used the cold process, with methyl-orange, on one sample, and the hot process, with phenol- phtalein on the other, and that, in both cases, 10 Cc. of normal sulphuric acid were required to produce neutrality. (1) Cb/d Process.—The procedure is the same as in all solutions heretofore explained. H2SO4 + 2NaHCOs = Na2SO4 + CO2 + H2O Sulphuric Acid. Sodium Sodium Carbonic Water. 97.82 Bicarbonate. Sulphate. Acid Gas. 2 X 83.85 1000 Cc. (— V. S.) containing 48.91 Gm of Sulphuric Acid are equivalent to 1 83.85 Gm. of Sodium Bicarbonate. 1 Cc. “ “ “ 0.04891 Gm. of Sulphuric Acid is equivalent to 0.08385 Gm. of Sodium Bicarbonate.. 10 Cc. of normal Sulphuric Acid, V. S. = 10 X 0.08385 = 0.835 + Gm. pure Sodium Bicarbonate. That is, 0.850 Gm. of the Sodium Bicarbonate taken contains 0.835 Gm. of pure substance, hence 0.850 : 0.835 = 100 : x ; x = 98.2 per cent. (2) Hot Process.—When phenolphtalein is used as indicator, the solution will have to be boiled after the addition of each in- stalment of the standard acid solution in order to expel the car- bonic acid. The end of the reaction is recognized from the fact that the red color produced by the indicator with alkalies ceases to reappear after several minutes boiling. (c) Estimation of Organic Salts of the Alkalies and Alkaline Earths. The organic salts of potassium, sodium, lithium, strontium, etc.; are examined by weighing out a small amount in a platinum or porcelain crucible, then heating slowly to redness (uncovered) until no further gases are given off and a charred mass remains. The crucible is allowed to cool, and its contents treated with boiling water and filtered into a flask or porcelain dish. The crucible is washed out with boiling water, and the washings passed through VOLUMETRIC ANALYSIS. 425 the filter, until the filtrate ceases to turn red litmus blue. To the filtrate, which should be clear, a sufficient amount of the indicator is added, and the alkali carbonate present estimated as directed above. This method is directed by the U. S. Pharmacopoeia to be carried out with Lithium Benzoate, Lithium Citrate, Lithium Salicylate, Potassium Acetate, Potassium Bitartrate, Potassium Citrate, Potassium et Sodium Tartrate, Sodium Acetate, Sodium Benzoate and Strontium Lactate. POTASSII BlTARTRAS. *2KHC4H4O6 = K2CO3 + 5C + 2CO2 + 5H2O Potassium Potassium Carbon. Carbonic Water. Bitartrate. Carbonate. Acid Gas. 2 X 187.67 138 h2so4 + k2co3 = k2so4 + co2 + h2o Sulphuric Potassium Potassium Carbonic Water. Acid. Carbonate. Sulphate. Acid Gas. 97.82 138 1000 Cc. — V. S. containing 48.91 Gm. of Sulphuric Acid is equivalent to 69 Gm. of Potassium Carbonate. 1 Cc. “ “ “ 0.04891 Gm. of Sulphuric Acid is equivalent to .069 Gm. of Potassium Carbonate. One molecule (138 parts) of Potassium Carbonate is obtained from two molecules (2 X 187.67 parts) of Potassium Bitartrate, hence one-half of a molecule (69 parts) of the former is obtained from one molecule (187.67 parts) of the latter. Then each 1 Cc. of normal Sulphuric Acid V. S. is equivalent to 0.069 Gm. Potas- sium Carbonate, which in turn represents 0.187 + Gm. Potassium Bitartrate. POTASSII ET Soon TARTRAS. t2(KNaC4H4O6 + 4H2O) = 2KNaCO3 + 5C + CO2 + 12H2O Rochelle Salt. Potassium Carbon. Carbonic Water. 2 X 281.5 Sodium Acid Gas. Carbonate. 2 X 122 KNaCO3 + H2SO4 = KNaSO4 + CO2 + H2O Potassium Sulphuric Potassium Carbonic Water. Sodium Acid. Sodium Acid Gas. Carbonate. 97.82 Sulphate. 122 1000 Cc. (— V. S.) containing 48.91 Gm. of Sulphuric Acid are equivalent to 61 Gm. of Potassium Carbonate. 1 Cc. “ “ “ 0.04891 Gm. of Sulphuric Acid is equivalent to 0.061 Gm. Potassium Carbonate. One molecule (122 parts) of Potassium Sodium Carbonate is obtained from one molecule (281.5 parts) of Rochelle Salt. Then each 1 Cc. of normal Sulphuric Acid V. S. is equivalent to 0.061 Gm. Potassium Sodium Carbonate, which in turn represents 0.1407 + Gm. of Rochelle Salts. * The reaction may also be written thus: 2KHC4H406 + 5O2 = K2C03 + 7CO2 + 5H2O. f The reaction may also be written thus: 2KNaC4H4O6.4H2O + 5O2 = 2KNaCO3 + 6CO2 + 12H2O 426 HANDBOOK OF PHARMACY. Sodii Benzoas. 2NaC7H5O2 + 5O2 = Na2CO3 + 5H2O + 3CO2 + 5C2 Sodium Oxygen. Sodium Water. Carbonic Carbon. Benzoate. Carbonate. Acid Gas. 2 X 143.71 138 H2SO4 + Na2CO3 = Na2SO4 + CO2 + H2O 97.82 138 One Cc. of normal Sulphuric Acid V. S. containing 0.04891 Gm. of Acid is equivalent to 0.069 Gm. of Sodium Carbonate. One molecule (138 parts) of Sodium Carbonate is obtained from two molecules (2 X 143.71 parts) of Sodium Benzoate, or one-half of a molecule (69 parts) of the former is equivalent to one mole- cule (143.71 parts) of the latter. Then 1 Cc. of normal Sulphuric Acid V. S. is equivalent to 0.069 Gm. of Sodium Carbonate, which in turn represents 0.1437 + Gm. of Sodium Benzoate. (4) Normal Hydrochloric Acid Solution is made after the same principle and is in every respect equivalent, in neutralizing power, to normal Sulphuric Acid. It may be employed in all instances given under the latter. H2C2O4 + 2H2O = H2SO4 = 2HC1 Oxalic Acid. Sulphuric Acid. Hydrochloric Acid. 125.7 97.83 2 X 36.37 1 L. of ~ V. S. containing 62.85 Gm. Oxalic Acid = 1 L. containing 48.91 Gm. of 1 H2SO4. 1 Cc. “ “ “ 0.06285 Gm. Oxalic Acid = 1 Cc. containing 0.4891 Gm. N of H2SO4. 1 L. of ' Sulphuric Acid = 1 L. containing 36.37 Gm. Hydrochloric Acid. lCc. ““ “ “ = 1 Cc. “ 0.03637 Gm. “ “ (5) Normal Potassium Hydrate Volumetric Solution. KOH — 55.99. 55.99 Gm.* in 1 Liter. “Dissolve 75 Gm. of potassium hydrate [Potassa, U. S. P.] in enough water to make, at or near 15° C. (59° F.), about 1050 Cc., and fill a burette with a portion of this liquid. Put 0.6285 Gm.f of pure oxalic acid into a flask of the capacity of about 100 Cc., and dissolve it with about 10 Cc. of water. Add a few drops of phenolphtalein T. S., and then carefully add, from the burette, the potassium hydrate solution, frequently agitating the flask, and regulating the flow to drops toward the end of the operation, until the red color produced by the influx no longer disappears on shaking, but is not deeper than pale pink. Note the number of Cc. of the potassium hydrate solution con- sumed, and then dilute the remainder of the solution so that exactly 10 Cc. of the diluted liquid shall be required to neutralize 0.6285 Gm.f of oxalic acid. Example.—Assuming that 8.0 Cc. of the stronger solution of potassium hydrate first prepared had been consumed in the trial, * “ This figure is frequently rounded off to 56 Gm.” t This figure may be rounded off to 0.63 Gm., if a delicate balance and exact weights are not available. VOLUMETRIC ANALYSIS. 427 then each 8.0 Cc. must be diluted to 10 Cc., or the whole of the remaining solution in the same proportion. Thus, if 1000 Cc. should be still remaining, this must be diluted with water to 1250 Cc. After the liquid is thus diluted, a new trial should be made in the manner above described, in which 10 Cc. of the diluted solution should exactly neutralize 0.6285 Gm.* of oxalic acid. If necessary, a new adjustment should then be made to render the correspond- ence perfect. Note.—Solutions of caustic alkalies are very prone to absorb carbon dioxide from the atmosphere, and thereby become liable to occasion errors when used witli litmus T. S. or phenolphtalein T. S. as indicators (methyl-orange T. S. is not affected by the presence of carbonic acid). Hence the volumetric solutions should be preserved in small vials provided with well-fitting corks or rubber stoppers, or, better still, they should have tubes filled with a mixture of soda and lime attached to their stoppers, so as to absorb the carbon dioxide and prevent its access to the solution. In place of potassium hydrate V. S., sodium hydrate V. S. may be used, in the same manner and in the same quantity. Potassium hydrate V. S., however, is preferable, since it foams less, and attacks glass more slowly and less energetically.” One Cubic Centimeter of Normal Potassium Hydrate V.S. is the equivalent of : Gramme. Potassium Hydrate, KOH 0.05599 Sodium Hydrate, NaOH 0.03996 Ammonia Gas, NH30.01701 Ammonium Chloride, NH4C1 0.05338 Acetic Acid, absolute, HC2HSO2 0.05986 Citric Acid, crystallized, H3C6H5O7 -p H2O 0.06983 Hydrobromic Acid, absolute, HBr 0.08076 Hydrochloric Acid, absolute, HC1 0.03637 Hydriodic Acid, absolute, HI 0.12753 Hypophosphorous Acid, HPH2O2 0.06588 Lactic Acid, absolute, HC3H5O3 0.08979 Nitric Acid, absolute, HN03 0.06289 Oxalic Acid, crystallized, H2C2O4 -p 2H2O 0.06285 Phosphoric Acid, H3PO4 (to form K2HPO4 ; with phenolphtalein), 0.0489 Phosphoric Acid, H3PO4 (to form KH2PO4; with methyl-orange), 0.0978 Potassium Dichromate, K2Cr2O7 0.14689 Sulphuric Acid, absolute, H2SO4 0.04891 Tartaric Acid, crystallized, H2C4H4O6 0.07482 ACIDIMETRY. The necessary amount of fluid (acid) should be weighed off in a fared and stoppered weighing flask, in order to avoid injury or corrosion of the balances. It is not always advisable to attempt ♦This figure may be rounded off to 0.63 Gm., if a delicate balance and exact weights are not available. 428 HANDBOOK OF PHARMACY. to weigh off a definite amount of the fluid, as this is attended with considerable difficulty. It is better to measure a quantity of the fluid, by means of a pipette, into a flask and then weigh the amount. The amount of acid selected depends upon its strength. For this purpose the Pharmacopoeia tabulates a list of various acids, stating the amount to be taken. Any weight approxi- mately near that given may be selected. It is best to avoid taking large amounts of the acids, as this would result in the useless waste of a large volume of the standard alkali solution. After weighing off the acid, the contents of the weighing flask are carefully rinsed out into a beaker or other flask preparatory to titrating. Then a few drops of the indicator are added, and titra- tion carried out with normal alkali solution until the fluid turns faint rose red (with phenolphtalein), or blue (with litmus), or yellow (with methyl-orange), or faint violet red (with rosolic acid), etc. The following equations will explain the various equivalents of the acids. (a) KOH 4- HC1 = KC1 + H2O 55.9 36.37 0.0559 Gm. of Potassium Hydrate (1 Cc.) are equivalent to 0.03637 Gm. of absolute Hydrochloric Acid. (&) KOH + HC2H3O2 = KC2H3O2 + H2O 55.9 59.86 0.0559 Gm. of Potassium Hydrate (1 Cc.) are equivalent to 0.05986 Gm. of absolute A A (c) 2K0H + H2SO4 = K2SO4 + 2H2O 2 X 55.9 97.82 55.9 p. = 48.91 p. 0.0559 Gm. of Potassium Hydrate (1 Cc.) are equivalent to 0.04891 Gm. of absolute Sulphuric Acid. (d) 2K0H + H2C4H4O6 = K2C4H4O6 + 2H2O 2 X 55.9 149.64 55.9 p. = 74.82 p. 0.0559 Gm. of Potassium Hydrate (1 Cc.) are equivalent to 0.07482 Gm. of crys- tallized Tartaric Acid. (e) 3KOH + H3C6H5O7 + H2O = K3C6H5O7 + 4H2O 3 X 55.9 209.5 55.9 p. = 69.83 p. 0.0559 Gm. of Potassium Hydrate (1 Cc.) are equivalent to 0.06983 Gm. of crystal- lized Citric Acid. (/) 2K0H + H3PO4 = K2HPO4 + 2H2O 2 X 55.9 97.8 55.9 = 48.9 In the case of phosphoric acid, with phenolphtalein as indi- cator, neutralization is attained when potassium orthophosphate (K2HPO4) is formed, which requires two molecules of alkali. 0.G559 Gm. of Potassium Hydrate (1 Cc.) are equivalent to 0.0489 Gm. of Phos- phoric Acid. (y) KOH + H3PO4 = KH2PO4 + H2O 55.9 97.8 With methyl-orange as indicator, neutralization is attained VOLUMETRIC ANALYSIS. 429 when acid potassium phosphate (KH2PO4) is formed, which requires one molecule of alkali. 0.0559 Gm. of Potassium Hydrate (1 Cc.) are equivalent to 0.0978 Gm. of Phos- phoric Acid. (6) Centinormal Potassium Hydrate V. S. containing 0.5599 Gm. to the liter, or 0.0005599 Gm. to the cubic centimeter, is employed in conjunction with decinormal sulphuric acid V. S. (containing 0.004891 Gm. in the cubic centimeter) in the estima- tion of total alkaloids in Extract of Nux Vomica. N N 10 Cc. Potassium Hydrate (0.005599 Gm.) is equivalent to ICc. Sulphuric Acid (0.004891 Gm.). Deci and centinormal solutions are employed for the determina- tion of minute quantities of acids or alkalies. Because of their great dilution, we are enabled to measure off volumes representing exceedingly small quantities of the actual reagent, which under ordinary circumstances, would be impossible with a burette of the usual graduations. Since the solutions are very dilute, an error of a tenth or fifth of a cubic centimeter would not affect the result, which would be the case, however, were we to employ a normal solution which is 100 times as strong. Standard Solution of Silver Nitrate. The U. S. Pharmacopoeia gives the following directions :— (7) Decinormal Silver Nitrate Volumetric Solution. AgNO3 = 169.55. 16.955 Gm.* in 1 Liter. Dissolve 16.955 Gm.* of pure silver nitrate in enough water to make, at or near 15° C. (59° F.), exactly 1000 Cc. Keep the solution in small, dark amber-colored, glass-stoppered vials, carefully protected from dust. Note.—Titration by decinormal silver nitrate V. S. may be managed in various ways, adapted to the special preparation to be tested. a. In most cases it is directed by the U. S. P. to be used in presence of a small quantity of potassium chromate T. S., which serves to indicate the end of the reaction by the appearance of the red color of silver chromate. b. In some cases (potassium cyanide, hydrocyanic acid) it is added until the first appearance of a permanent precipitate. One Cubic Centimeter of Decinormal Silver Nitrate V. S. is the equivalent of: Gramme. Silver Nitrate, AgNO3 0.016955 Ammonium Bromide, NH4Br 0.009777 Ammonium Chloride, NH4C1 0.005338 Calcium Bromide, CaBr2 0.0099715 Ferrous Bromide, FeBr2 0.010770 Ferrous Iodide, Fel2 0.015447 * “ Frequently rounded off to 16.96 Gm., when a delicate balance and exact weights are not available.” 430 HANDBOOK OF PHARMACY. Gramme. Hydrocyanic Acid, absolute, HCN, with indicator, 0.002698 Hydrocyanic Acid, absolute, HCN, to first formation of pre- cipitate, 0.005396 Hydriodic Acid, HI 0.012753 Hydrobromic Acid, HBr 0.008076 Lithium Bromide, LiBr 0.008677 Potassium Bromide, KBr0.011879 Potassium Chloride, KC1 0.007440 Potassium Cyanide, KCN with indicator, 0.006501 Potassium Cyanide, KCN, to first formation of precipitate, . 0.013002 Potassium Iodide, KI 0.016556 Potassium Sulphocyanate, KSCN 0.009699 Sodium Bromide, NaBr 0.010276 Sodium Chloride, NaCl 0.005837 Sodium Iodide, Nal 0.014953 Strontium Bromide, SrBr2 (anhydrous), 0.012341 Strontium Iodide, Sri, (anhydrous),0.017018 Zinc Bromide, ZnBr2 0.011231 Zinc Chloride, ZnCl2 0.006792 Zinc Iodide, Znl2 0.015908 Exercise.—An unknown quantity of pure sodium chloride was dissolved in water in a beaker, a few drops of potassium chromate were added to impart a yellow color, then the silver solution was slowly run in, under constant stirring, until the last drop caused the solution to turn permanently pale reddish (silver chromate); 30 Cc. of silver solution were required. How much sodium chloride was present? (a) AgNO3 + NaCl = AgCl -f- NaNO3 Silver Nitrate. Sodium Chloride. Silver Chloride. Sodium Nitrate. 169.55 58.37 1000 Cc. (fs V.S.) containing 16.955 Gm. of Silver Nitrate are equivalent to 5.837 Gm. of Sodium Chloride. 1 Cc. “ “ 0.016955 “ of Silver Nitrate is equivalent to 0.005837 Gm. of Sodium Chloride. 30 Cc. Silver Nitrate = 30 X 0.005837 = 0.175-f- Gm. of Sodium Chloride. Potassium Bromide. (&) AgNO3 + KBr = AgBr + KN03 169.55 118.8 1000 Cc. (N V. S ) containing 16.955 Gm. Silver Nitrate are equivalent to 11.88 10 Gm. Potassium Bromide. 1 Cc. “ “ “ 0.01695 Gm. Silver Nitrate is equivalent to 0.0118 Gm. Potassium Bromide. Hence each cubic centimeter of the decinormal silver nitrate V. S. is equivalent to 0.01188 Gm. of Potassium Bromide. The other halogen salts are estimated in the same manner. The halogen acids (HI or HBr) must be first neutralized with an alkali (see Syrupus Acidi Hydriodici, page 278). Ferrous Iodide cannot be estimated directly like the above halogen salts, because the indicator, potassium chromate, reacts with the ferrous salt (see Syrupus Ferri lodidi, page 281); hence we have recourse to another method, known as Volhard’s, which is equally applicable to the estimation of all halogens. VOLUMETRIC ANALYSIS. 431 (7) Volhard’s Method. This is applicable where the chromatic indicator cannot be used. It may also be used in the presence of nitric acid, thus enabling us to estimate chlorides in the presence of phosphoric or other acids which precipitate silver in neutral solution. The method depends upon entirely precipitating the halogen, in the presence of nitric acid, by a known excess of standard solution of silver, then esti- mating the excess of silver left uncombined with the halogen, by a standard solution of potassium (or ammonium) sulphocyanate,* using a drop or so of ferric ammonium sulphate as indicator. As soon as the sulphocyanate has precipitated all of the silver excess, it strikes a blood-red color with the ferric salt, due to the forma- tion of ferric sulphocyanate. The difference between the volume of standard silver solution originally added, and that of the sulphocyanate used, will give the number of cubic centimeters of silver equivalent to the chloride present. Estimation of Hydrocyanic Acid. (a) To First Formation of a Precipitate. The hydrocyanic acid is weighed off, diluted with water, and solution of sodium hydrate added until the liquid is strongly alkaline, as shown by litmus paper or solution. Then decinormal silver nitrate solution is slowly dropped in with constant agitation until a faint permanent cloud of silver cyanide (AgCN) is produced. If during the operation, the litmus becomes red, more of the so- dium hydrate must be added until the indicator shows a blue tint. The reaction is as follows:— 2HCN -p 2NaOH = 2NaCN + 2H2O Hydrocyanic Acid. Sodium Hydrate. Sodium Cyanide. Water. 2 X 26.98 2 X <9 The sodium hydrate is added, to prevent the liberation of free nitric acid which would prevent the silver cyanide from pre- cipitating :— 2NaCN 4- AgNO3 = AgCN.NaCN + NaNOs Sodium Cyanide. Silver Nitrate. Double Cyanide of Silver Sodium Nitrate. 2 X 49 169.55 and Sodium. Two molecules of Hydrocyanic Acid (53.96 parts) are equivalent to one molecule of Silver Nitrate (169.55 parts). Or 5.396 parts of Hydrocyanic Acid are equivalent to 16.955 parts of Silver Nitrate. 0r0.005396 “ “ “ “ “ “ 0.016955 “ “ “ Therefore 1 Cc. of Silver Nitrate V. S. (containing 0.016955 Gm. of the salt) is equivalent to 0.005396 Gm. of Hydrocyanic Acid. * KSCN + AgNO3 = AgSCN + KNO3 Potassium Silver Silver Potassium Sulphocvanate. Nitrate. Sulphocyanate. Nitrate. 96.99 169.55 N Potassium Sulphocyanate, 9.699 Gm. = 16.955 Gm. (1000 Cc. — V. S.) Silver Nitrate. '* “ 0.009699 Gm. = 0.016955 Gm. (1 Cc. V. S.) “ “ Then 1 Cc. of the Sulphocyanate solution (containing 0.009699 Gm. of the salt) is equivalent to 1 Cc. of the Silver Nitrate Solution (containing 0.016955 Gm. of the salt). 432 HANDBOOK OF PHARMACY. (6) Estimation with Indicator. The Pharmacopoeia directs that sufficient magnesia paste be added to the weighed and diluted acid to impart an opaque milk- iness to the liquid. This serves to neutralize the acid as well as to afford a better opportunity to distinguish the red color (silver chromate) which indicates the end point of the reaction, potassium chromate being the indicator. The reaction is the same as in the preceding:—* 2NaCN 4- AgNOs = AgCN.NaCN + NaNO3 Sodium Cyanide. Silver Nitrate. Double Cyanide of Silver Sodium Nitrate, and Sodium. AgCN.NaCN 4- AgNO3 = 2AgCN + NaNO3 2NaCN or 2HCN are then equivalent to 2AgNO3 2 X 49 2 X 26.98 2 X 169.55 49 parts of Sodium Cyanide or 26.98 parts of Hydrocyanic acid are equivalent to 169.55 parts of Silver Nitrate. or 4.9 parts of Sodium Cyanide or 2.698 parts of Hydrocyanic acid are equivalent to 16.955 parts of Silver Nitrate. AT 1000 Cc. of — silver solution containing 16.955 Gm. AgNO3 are equivalent to 4.9 Gm. of sodium cyanide, which is equivalent to 2.698 Gm. of hydrocyanic acid. Therefore 1 Cc. of — silver solution (0.016955 Gm. of the salt) is equivalent to 0.002698 Gm. of hydrocyanic acid. Potassium Cyanide is estimated in the same manner and sub- jected to the same reactions as given above. (8) Decinormal Iodine Volumetric Solution. I — 126.53 12.653 Gm.f in 1 Liter. Dissolve 12.653 Gm. of pure iodine in a solution of 18 Gm. of pure potassium iodide in 300 Cc. of water; then add enough water to make the solution measure, at or near 15° C. (59° C.), exactly 1000 Cc. The potassium iodide plays the part of a solvent for the iodine. One Cubic Centimeter of Decinormal Iodine V. S. is the equivalent of: Gramme. Iodine, I 0.012653 Arsenic Trioxide (arsenous acid), As.2O3 0.004942 Potassium Sulphite, crystallized, K2SO3 + 2H2O 0.009692 Sodium Bisulphite, NaHSO30.005193 Sodium Hyposulphite (Thiosulphite) crystals, Na2S2O3-|- 5H2O 0.024764 Sodium sulphite, crystallized, Na2SO3 4- 7H2O 0.012579 Sulphur Dioxide, SO20.003195 Antimony and Potassium Tartrate, crystals, 2K(SbO)C4H4O6- + H2O 0.01656. *For the sake of uniformity and clearness sodium is retained in the explanatory formula instead of magnesium. fMay be rounded off to 12.65 Gm. VOL UMETRIC ANA LYSIS. 433 (a) Estimation of Arsenous Oxide. The arsenous oxide is weighed off and dissolved in boiling water with the aid of sodium bicarbonate. The solution is al- lowed to cool, some starch paste added, and iodine solution run in until a faint, permanently blue color is obtained. The addition of iodine to arsenous acid in alkaline solution causes its oxidation to arsenic acid, the iodine being thereby converted into hy- driodic acid, with disappearance of color. As soon as all of the arsenous acid is oxidized to arsenic acid, the next drop of iodine (being free) will strike a blue color with the starch. The excess of sodium bicarbonate serves the purpose of com- bining with the liberated hydriodic acid, which, if present in free condition, would interfere with the reaction:— As2O3 4- 41 + 4NaHCO3 — As.2O5 + 4NaI + 4CO2 + 2H2O Arsenous Iodine. Sodium Arsenic Sodium Carbonic Water. Oxide. 4 X 126.5 Bicarbonate. Oxide. Iodide. Acid Gas. 197.68 Since four molecules of iodine (4 X 126.5) are necessary to oxidize one molecule (197.68) of arsenous to arsenic oxide, hence, one atom of iodine is equivalent to one-fourth of a molecule of arsenous oxide:— Iodine. Arsenous Oxide. 126.5 p., 49.42 p. 1000 Cc. ~ V. S. containing12.65 Gm., 4.942 Gm. 1 Cc. “ “ 0.01265 Gin., 0.004942 Gm. Therefore each Cc. of Iodine Solution is equivalent to 0.004942 Gm. Arsenous Oxide. (6) Estimation of Sulphurous Acid, Free and in Sulphites. The acid or sulphite is largely diluted with water, starch paste added, then iodine solution added until a faint permanent blue appears. The sulphurous oxide or sulphite undergoes oxidation to sulphuric acid or to sulphate, and the iodine is thereby con- verted into hydriodic acid according to the equation :— I2 4- H2O 4- SO2.H2O = H2SO4 4- 2HI Iodine. Water. Sulphurous Acid. Sulphuric Hydriodic 2 X 126.5 63.90 (SO2) Acid. Acid. 126.5 parts are equivalent to . . 31.95 parts. 1000 Cc. V. S. containing 12.65 Gm. Iodine are equivalent to 3.195 Gm. of Sul ph urous Oxide. 1 Cc. “ “ 0.01265 Gm. Iodine is equivalent to 0.003195 Gm. of Sulphurous Oxide. (c) Estimation of Hyposulphites {Thiosulphates'). The equation is as follows:— 21 4- 2(Na2S2O3.5H2O) = 2NaI 4- NaAOg 4- 10H2O Iodine. Sodium Hyposulphite. Sodium Sodium Water. 2 X 126.5 2 X 247.64 Iodine. Tetrathionate. 126.5 parts are equivalent to 247.64 parts. 1000 Cc. ~ V. S. containing 12.65 Gm. Iodine are equivalent to 24.764 Gm. of Sodium Hyposulphite. 1 Cc. “ “ 0.01265 Gm. Iodine is equivalent to 0.024764 Gm. of Sodium Hyposulphite. 434 HANDBOOK OF PHARMACY. (9) Decinormal Sodium Hyposulphite Volumetric Solution. Na2S2O3 + 5H2O = 247.64. 24.764 Gm. in 1 Liter. This solution is standardized by means of decinormal iodine V. S. “ Dissolve 30 Gm. of selected crystals of sodium hyposulphite (sodium thiosulphate) in enough water to make, at or near 15° C. (59° F.), 1100 Cc. Of this solution transfer 10 Cc. into a flask, add a few drops of starch T. S., and then gradually add, from a burette, decinormal iodine V. S., in small portions at a time, shaking the flask after each addition, and regulating the flow to drops toward the end of the operation. As soon as the color produced by the influx of the iodine solution no longer dis- appears on shaking, but is not deeper than very pale blue, note the number of Cc. of the iodine solution consumed. Then dilute the sodium hyposulphite solution so that equal volumes of it and of decinormal iodine V. S. will exactly correspond to each other under the conditions mentioned above. Example.—Assuming that 10 Cc. of the stronger sodium hypo- sulphite solution first prepared had required 10.7 Cc. of deci- normal iodine V. S. to produce a faint reaction with starch, the hyposulphite solution must be diluted in the proportion of 10 Cc. to 10.7 Cc., or 1000 Cc. to 1070 Cc. After the solution is thus diluted, a new trial should be made in the manner above described, in which 50 Cc. of the decinormal sodium hyposulphite V. S. should require exactly 50 Cc. of deci- normal iodineV. S. to produce a faint reaction with starch. If necessary, a new adjustment should then be made to render the correspondence perfect. Keep the solution in small, dark amber-colored, glass-stoppered bottles, carefully protected from dust. Note.—When this solution is to be used, fill a burette with it, place the liquid to be tested either for the free iodine it already contains, or for that which it liberates from an excess of potassium iodide added to it, into a flask, and gradually add small portions of the solution from the burette, shaking after each addition, and regulating the flow to drops towards the end of the operation, until the brown color of the iodine has nearly disappeared. Now add a few drops of starch T. S., which will produce a blue color, and then continue to add the hyposulphite solution in drops until the blue tint is exactly discharged.” One Cubic Centimeter of Decinormal Sodium Hyposulphite V. S. is the equivalent of: Gramme. Sodium Hyposulphite (Thiosulphate), Na2S2O3-|-5H2O . . 0.024764 Bromine, Br 0.007976 Chlorine, Cl 0.003537 Iodine, I 0.012653 Iron, Fe, in ferric salts, 0.005588 VOLUMETRIC ANALYSIS. 435 (a) Estimation of Free Iodine. A quantity of Iodine is weighed off, and by aid of potassium iodide dissolved in water. Then the hyposulphite solution is added, under constant stirring, until the solution has paled to a yellowish tint. A little starch paste is now added, and the addi- tion of the hyposulphite continued in drops until the blue color just disappears. Then according to the equation:— 2(Na2S2O3.5H2O) + 21 = 2NaI + Na.2S4O6 + 10H2O Sodium Hyposulphite. Iodine. Sodium Sodium Water. 2 x 247.64 2 X 126.5 Iodide. Tetrathionate. 247.64 parts are equivalent to 126.5 parts. 1000 Cc. X V. S. containing 24.764 Gm. Sodium Hyposulphite are equivalent to 12.65 Gm. Iodine. 1 Cc. “ “ “ 0.024764 Gm. Sodium Hyposulphite is equivalent to 0.01265 Gm. Iodine. (6) Estimation of Free Chlorine or Bromine. This process is adapted to all substances containing free Chlo- rine or Bromine. (See also, Aqua Chlori, page 223.) The sub- stance is weighed off and added to water containing a slight excess of potassium iodide, whereupon either the chlorine or bromine liberates an equivalent quantity of iodine from the potassium iodide, which in turn is estimated by means of the hyposulphite solution as directed above:— 2C1 + 2KI = 2KC1 -f- 21 Chlorine. Potassium Potassium Iodine. 2 X 35.37 Iodide. Chloride. 2 X 126.5 35.37 parts of Cl are equivalent to126.5 parts of I. 3.537 “ “ “ “ “ “12.65 “ “ “ 0 003537 “ “ “ “ “ “ 0.01265 “ “ “ Since 1 Cc. of decinormal Sodium Hyposulphite solution (0.024764 Gm. of the salt) is equivalent to 0.01265 Gm. of iodine, and as this is equivalent to 0.003537 Gm. of Chlorine, hence 1 Cc. of decinormal sodium hyposulphite solution is equivalent to 0.003537 Gm. of Chlorine. On this same principle 1 Cc. of decinormal Sodium Hyposul- phite solution is equivalent to 0.007976 Gm. of bromine, for— 2Br -I- 2KI = 2KBr + 21 Bromine. Potassium Potassium Iodine. 2 X 79.76 Iodide. Bromide. 2 X 126.5 79.76 parts of Br. are equivalent to126.5 parts of Iodine. 0.007976 “ “ “ “ 0.01265 " “ (c) Estimation of Iron in Ferric Salts. A suitable quantity of the iron salt or solution is weighed off and added to water contained in a glass stoppered bottle. To this is added some hydrochloric acid and an excess of potassium iodide (which must be absolutely free from iodate). The mixture is kept for half an hour at a temperature of 40° C., then cooled, and mixed with a few drops of starch T. S. Decinormal solution 436 HANDBOOK OF PHARMACY. of sodium hyposulphite is then run in till the blue color of the solution is discharged. The ferric chloride causes the liberation of an amount of iodine equivalent to the amount of metallic iron present. The ferric is reduced to ferrous chloride. The hydrochloric acid added serves to prevent the solution of the iodine by the excess of potassium iodide present. The reaction is as follows:— Fe2Cl6 + 2KI = 2FeCl2 + 2KC1 + 21 Ferric Potassium Ferrous Potassium Iodine. Chloride. Iodide. Chloride. Chloride. 2 X 126.5 2 X 55-8 (Fe) 55.8 parts of Metallic Iron are equivalent to126.5 parts of Iodine. 0.00558 “ “ “ “ “ “ 0.01265 Since, according to the equation c(page 433), 1 Cc. of decinormal hyposulphite solution (containing 0.02476 Gm. of the salt) is equivalent to 1 Cc. of decinormal iodine solution (0.01265 Gm.), and as this is equivalent to 0.00558 Gm. metallic iron, hence 1 Cc. of the hyposulphite solution is equivalent to 0.00558 Gm. of metallic iron. (10) Decinormal Potassium Dichromate Volumetric Solu- tion. K2Cr2O7 = 293.78. 4.896 Gm.* in 1 Liter. Dissolve 4.896 Gm.* of pure potassium dichromate (see below) in enough water to make, at or near 15° C. (59° F.), exactly 1000 Cc. If the potassium bichromate is pure,f it is directly dissolved as above indicated. If not, it may be standardized by making an estimation upon 0.5 Gm. of pure iron (piano) wire, dissolved in dilute sulphuric acid, as described on page 437 equation a. When used with phenolphtalein as indicator, to neutralize alkalies, the volumetric solution of potassium dichromate is deci- normal when it contains 14.689 Gm. in 1 liter. It is then the exact equivalent of any decinormal acid, corresponding to the amounts of alkalies quoted, for instance, under Decinormal Oxalic Acid V. S. The dichromate is equivalent to two molecules of hydrochloric acid; thus:— K2Cr2O7 + 2HC1 = 2KC1 + 2CrO3 + H2O Hence 1 molecule of the acid is equivalent to | molecule of the bichromate (K2C2O7 = 146.89). The decinormal solution, there- fore, is made to contain but 14.689 Gm. When used as an oxidizing agent to convert ferrous into ferric salts, or to liberate iodine from potassium iodide, the solution just * “ Generally rounded off to 4.9 Gm., when a delicate balance and exact weights are not available.” f The Pharmacopoeia specifies that. Pure Potassium Dichromate for use in volumetric analysis, besides responding to the tests given in the text of the Pharmacopoeia (under Potassii Bichromas), must conform to the following tests. In a solution of 0.5 Gm. of the salt in 10 Cc. of water rendered acid by 0.5 Cc. of nitric acid, no visible change should be produced either by barium chloride T. S. (absence of sulphate), or by silver nitrate T. S. (absence of chloride). In a mixture of 10 Cc. of the aqueous solution (1 in 20) with 1 Cc. of ammonia water, no precipitate should be produced by ammo- nium oxalate T. S. (absence of calcium). VOLUMETRIC ANALYSIS. 437 mentioned (containing 14.689 Gm. in 1 liter) has the effect of a — volumetric solution, and a solution of one-third of this strength, containing 4.896 Gm. in 1 liter, has the value of a decinormal solution. Upon heating 1 molecule of the bichromate with an acid (H2SO4), three atoms of nascent oxygen are liberated. Thus :— K2Cr2O7 + 4H2SO4 = K2SO4 + Cr2(SO4)3 + 4H2O + O3 These three atoms of oxygen possess the power to convert six atoms of iron from the ferrous to the ferric state, according to the equation— 6FeO 4- O3 = 3Fe2O3 Therefore each molecule of the dichromate, yielding three atoms of oxygen, is equivalent to six atoms of hydrogen. Hence, accord- ing to the principle expressed on page 413, we take | of the molecular weight of a decinormal solution of the bichromate (| of 29.378 — 4.896), thereby reducing it to the valency correspond- ing to one atom of replaceable hydrogen. As a decinormal solution, it is the equivalent of an equal volume of decinormal potassium permanganate V. S., or, in the case of iodine liberated from potassium iodide, it is the equiva- lent of an equal volume of decinormal sodium hyposulphite V. S. For titrating iron in ferrous compounds, it is used in the following manner: Introduce the aqueous solution of the ferrous salt into a flask and, if it is not already acid, render it so with sulphuric acid. Now add, gradually, decinormal potassium dichromate V. S. from a burette, until a drop taken out upon a white surface no longer shows a blue color with a drop of freshly prepared potassium ferricyanide T. S. Decinormal potassium dichromate V. S. may also be used, in conjunction with potassium iodide (from which it liberates iodine) and sulphuric acid, for adjustingthe titer of sodium hyposulphite (thiosulphate) V. S. and, by its means, that of the iodine V. S. One Cubic Centimeter of Decinormal Potassium Dichromate V. S. is the equivalent of : Gramme. Potassium Dichromate, K2Cr2O7 0.0048963 Iron, in ferrous compounds, 0.005588 Ferrous Carbonate, FeCO3 0.011573 Ferrous Sulphate, anhydrous, FeSO40.015170 Ferrous Sulphate, crystallized, FeSO4 + 7H2O 0.027742 Ferrous Sulphate, dried, 2FeSO4 + 2H2O 0.017864 Potassium Hydrate, KOH 0.001866 Sodium Hyposulphite (Thiosulphate), Na2S2O3 + 5H2O . . 0.024764 Estimation of Metallic Iron and Ferrous Salts. (a) Metallic Iron.—Any definite amount of iron (about 0.5 Gm.) is weighed off (if it is intended for standardizing, piano wire should be selected), then dissolved by the aid of heat in dilute sul- 438 HANDBOOK OF PHARMACY. phuric acid, in a flask with a close fitting cork, through which passes a short glass tube, which is fitted into a rubber tube closed at the other extremity, and in the side of which an incision is made which will allow steam and hydrogen gas to pass out, but will prevent the air from passing in. When the iron is dissolved, the solution is titrated directly in the flask, or rinsed out into a beaker. The titration is carried out as directed in the preceding paragraph. The failure of the ferricyanide solution to produce a blue color with the resulting mixture indicates that the oxidation of the ferrous to the ferric condition is complete. The first half of the operation embraces the solution of the metallic iron, yielding ferrous sulphate, the operation being per- formed under conditions which obviate any possible formation of ferric salts resulting from contact with air :— 6Fe + 6H2SO4 = 6FeSO4 + 3H2 6 X 55.88 6 X 151.7 The following reaction illustrates the oxidation of the ferrous to ferric salt:— 6FeSO4 + K2Cr2O7 + 7H2SO4 = 3Fe2(SO4)3 + K2SO4 + Ferrous Potassium Sulphuric Ferric Potassium Sulphate. Dichromate. Acid. Sulphate. Sulphate. 910.2 293.78 Cr2(SO4)3 + 7H2O Chromium Sulphate. Water. Hence— K2Cr2O7 = 6FeSO4 = 6Fe 293.78 6 X 151.7 6 X 55.88 48.96 parts = 151.7 parts = 55.88 parts. 1000 Cc. N V. S. containing 4.896 Gm. dichromate =15.17 Gm. ferrous sulphate = 10 5.588 Gm. metallic iron. lCc. “ “ 0.004896 Gm. dichromate = 0.01517 Gm. ferrous sul- phate = 0.005588 metallic iron. (6) C'ystallized Ferrous Sulphate. The weighed amount of salt is dissolved in water containing dilute sulphuric acid and titrated as directed above. K2Cr2O7 4- 6 FeSO4.7H2O + 7H2SO4 = 3Fe2(SO4)3 + K2SO4 + Cr2(SO4)3 + 14H2O 293.78 6 X 277.42 293.78 parts of K»Cr»O7are necessary for the oxidation of 6 X 277.42 parts of ferrous sulphate. 48.96 “ “' “ “ “ “ “ 277.42 “ “ “ “ 1000 Cc. V. S. containing 0.004896 Gm. of K2Cr2O7 are necessary for the oxidation of 0.027742 Gm. of crystallized ferrous sulphate. (c) Ferri Carbonas Saccharatus. K2Cr2O7 + 6FeSO3 + 7H2SO4 = 3Fe.2(SO4)3 + K2SO4 + Cr2(SO4)3 + 7H2O 293.78 6 X 115.73 293.78 parts of K2Cr2O8 are necessary for the oxidation of 6 X 115.73 parts of ferrous carbonate. 48.96 “ ' “ “ “ 115.73 “ “ “ Then 1 Cc. of the dichromate solution (or 0.004896 Gm. of the salt) is equivalent to 0.011573 Gm. of ferrous carbonate. VOLUMETRIC ANALYSIS. 439 (d) Potassium Iodide and Sodium Hyposulphite. K2Cr2O7 + 6KI + 7H2SO4 = 4K2SO4 + Cr2(SO4)3 + 3I2 293.78 6 X 126.6 48.96 parts are capable of liberating126.6 parts 1000 Cc. containing 4.896 Gm. of - Dichromate V. S. are equivalent to 12.66 Gm. of 10 Iodine. 1 Cc. “ 0.004896 “ “ “ “ is equivalent to 0.01266Gm. of Iodine, or 0.02476 Gm. of Sodium Hyposulphite (1 Cc.). (11) Decinormal Potassium Permanganate Volumetric So- lution. 2KMnO4 = 315.34. 3.1534 Gnt* in 1 Liter. For the estimation of Iron, this solution is far more satisfac- tory than the decinormal dichromate solution, since the end point of the reaction is readily distinguished, and does not require the use of reagents, as is the case in the latter. Two molecules of potassium permanganate (2KMnO4) in oxida- tion give off five atoms of oxygen, which oxidizes the ferrous of 10 atoms of metallic iron to ferric condition, thus:— 2KMuO4 + lOFeO = 5Fe2O3 + 2MnO + K2O Potassium Ferrous Ferric Manganous Potassium Permanganate. Oxide. Oxide. Oxide. Oxide. 315.34 molecule KMnO4 yield T molecule of oxygen, or molecule KMnO4 yields molecule of oxygen. But h molecule of oxygen — 1 atom of hydrogen. Hence of the molecular weight of KMnO4 or of the mole- cular weight of 2KMnO4 is equivalent to one atom of hydrogen ; hence the normal solution of potassium permanganate should contain (2KMnO4) — 31.534 Gm. of salt. If the normal solution contains 31.534 Gm., then the decinormal solution must contain of this, or 3.1534 Gm. in the Liter. The next step is to prepare the solution. This cannot be done directly, by weighing out 3.1534 Gm. of the salt, partly because the salt is but rarely absolutely pure, and partly because any oxidizable matters in the water used for solution would consume some of the salt. The adjustment must, therefore, be made indirectly by means of either Oxalic Acid or Iron. In order to do this, a solution of approximate strength is first prepared. The Pharmacopoeia gives the following directions:— “ I. Place 3.5 Gm. of pure, crystallized potassium permanganate in a flask, add 1000 Cc. of boiling water, and boil until the crys- tals are dissolved. Close the flask, and set it aside for two days, so that any suspended matters may deposit. This is the stronger solution. Prepare another, weaker solution, in the same manner, using 6.6 Gm. of the salt and 2200 Cc. of water, and set this also aside for two days. After the lapse of this time, pour off the clear * This quantity is never directly weighed, but adjusted either by Oxalic Acid or by Iron ; in cal- culations it is often abbreviated. 440 HANDBOOK OF PHARMACY. portion of each solution into separate vessels provided with glass stoppers, and then proceed to test each separately.” This solution is standardized by means of oxalic acid, the deci- normal volumetric solution being employed. The reaction pro- ceeds thus:— 2KMnO4 + 5(H2C2O4 + 2H2O) + 3H2SO4 = K2SO4 + 2MnSO4 + 10CO2 Potassium Oxalic Acid. Sulphuric Potassium Manganese Carbonic Permanganate. 628.5 Acid. Sulphate. Sulphate. Acid Gas. 315.3 + 8H2O Water. 1000 Cc. of the decinormal V. S. should contain 3.153 Gm. permanganate = 6.285 Gm. oxalic acid. 1 Cc. of the decinormal V. S. should contain 0.003153 Gm. permanganate = 0.006285 Gm. oxalic acid. Hence the 10 Cc. of the decinormal acid solution containing 0.06285 Gm. of oxalic acid will be equivalent to 0.03153 Gm. of potassium permanganate. Sulphuric acid is employed in all reactions with permanganate, in order to dissolve the separated brown manganic hydrate and to convert it into manganic sul- phate, which does not impart a color to the liquid. The pres- ence of the suspended brown precipitate of manganic hydrate would render it next to impossible to recognize the end of the reaction. “Introduce into a flask 10 Cc. of decinormal oxalic acid V. S., add 1 Cc. of pure, concentrated sulphuric acid, and, before this mixture cools, gradually add from a burette small quantities of the weaker permanganate solution, shaking the flask after each addition and reducing the flow to drops toward the end of the operation. When the last drop of the permanganate solution added is no longer decolorized but imparts a pinkish tint to the liquid, note the number of Cc. consumed. In the same manner ascertain the titer of the stronger solution, and likewise note down the number of Cc. of the latter consumed. Finally mix the two solutions in such proportions that 50 Cc. of the mixture will exactly correspond to an equal volume of decinormal oxalic acid V. S. Note.—To obtain the accurate proportions for mixing the two solutions, deduct 10 from the number of Cc. of the weaker solu- tion required to decompose 10 Cc. of decinormal oxalic acid V. S. With this difference multiply the number of Cc. of the stronger solution required for the same purpose. The product shows the number of Cc. of the stronger solution needed for the mixture. Next deduct the number of Cc. of the stronger solution required to decompose 10 Cc. of decinormal oxalic acid V. S. from 10, and with the difference multiply the number ofCc. of the weaker solu- tion required for the same purpose. The product shows the number of Cc. of the weaker solution needed for the mixture. Or, designating by S the number of Cc. of the stronger solution and by W the number of Cc. of the weaker solution required to VOLUMETRIC ANALYSIS. 441 decompose 10 Cc. of decinormal oxalic acid V. S., the following- formula will give the proportions in which the solutions must be mixed :— Stronger Solution. Weaker Solution. (W—10)S + (10—S)W Example.—Assuming that 9 Cc. of the stronger (S) and 10.5 of the weaker (W) solution had been required, then substituting these values in the above given formula, we obtain:— Stronger Solution. Weaker Solution. (10.5—10)9 + (10—9) 10.5 or, 4.5. -j- or, 10.5 making 15 Cc. of final solution. The bulk of the two solutions is now mixed in the same pro- portion 450 Cc. of the stronger and 1050 Cc. of the weaker, or 900 Cc. of the stronger and 2100 Cc. of the weaker solution. After the mixture is thus prepared, a new trial should be made, when 10 Cc. of the solution should exactly decompose 10 “ Cc. of the decinormal oxalic acid V. S. If necessary, a new adjustment should be made to render the correspondence perfect. This solution should be kept in small, dark amber-colored and glass-stoppered bottles (or in bottles provided -with tubes, especially designed for the purpose). Thus prepared, this solution will hold its titer for months; yet it should be tested occasionally, and, when it is found reduced, the liquid should be brought back to normal strength by the addition of such an amount of the stronger solution as may be determined in the manner above described. II. When potassium permanganate V. S. is to be prepared for immediate use, this may be done in the following manner. Dis- solve 3.5 Gm. of pure, crystallized potassium permanganate in 1000 Cc. of pure water, recently boiled and cooled. Introduce 10 Cc. of decinormal oxalic acid V. S. into a beaker, add 1 Cc. of pure, concentrated sulphuric acid, and proceed as directed above for the weaker permanganate solution. Note the number of Cc. of the solution consumed, and then dilute the remainder with pure water recently boiled and cooled, until 50 Cc. will exactly corres- pond to 50 Cc. of decinormal oxalic acid V. S. Example.—Assuming that 9.1 Cc. of the Permanganate solu- tion first prepared had been required to produce a permanent pink tint, then every 9.1 Cc. of the solution must be diluted to 10 Cc., or the whole of the remaining solution in the same proportion. A new trial should then be made to verify the agreement. Note.—Potassium permanganate V. S. thus prepared is liable to deteriorate more readily and quickly than that prepared by the method first given (under I.). It cannot be safely trusted without verification, each time it is to be used.” 442 HANDBOOK OF PHARMACY. One Cubic Centimeter of Decinormal Potassium Permanganate V. S. is the equivalent of: Gramme. Potassium Permanganate, KMnO4 0.0031534 Barium Dioxide, BaO2 0.008441 Calcium Hypophosphite, Ca(PH2O2)2 0.0021209 Ferric Hypophosphite, Fe2(PH2O2)6 0.0020877 Iron, in ferrous compounds, Fe 0.005588 Ferrous Carbonate, FeCO30.011573 Ferrous Oxide, FeO 0.007195 Ferrous Sulphate, anhydrous, FeSO40.015170 Ferrous Sulphate, crystals, FeSO4+ 7H2O 0 027742 Ferrous Sulphate, dried, 2FeSO4 4-3H2O 0.017864 Hydrogen Dioxide, H2O2 0.001696 Hypophosphorous Acid, HPH2O20.001647 Oxalic Acid, crystallized, H2C2O4 + 2H2O6 0.006285 Oxygen, O 0.000798 Potassium Hypophosphite, KPH2O2 0.002598 Sodium Hypophosphite, NaPH2O2 + H2O 0.002646 (а) Estimation of Hydrogen Dioxide. A weighed quantity of the solution, diluted with water, is ren- dered decidedly acid with sulphuric acid, and decinormal per- manganate solution is run in until the liquid retains a faint pink tint after being stirred. The reaction proceeds thus:— 2KMnO4 4 5H2O2 4- 3H2SO4 = 5O2 + 8H2O 4- K2SO4 4- 2MnSO4 315.2 169.6 N 1000 Cc. of r- V. S. containing 3.152 Gm. of permanganate correspond to 1.696 Gm. of Hydrogen Peroxide. 1 Cc. “ “ 0.003152 Gm. of permanganate correspond to 0-001696 Gm. of Hydrogen Peroxide. Barium Dioxide, is estimated in the same manner, its oxygen being, however, first converted into hydrogen peroxide by reaction with phosphoric acid, thus:— 3BaO2 4- 2H3PO4 = Bas(PO4)2 + 3H2O2 Barium Dioxide. Phosphoric Acid. Barium Phosphate. Hydrogen Peroxide. 3 X 168.8 3 X 33.92 Each 506.4 parts of Barium Dioxide yield theoretically 101.76 parts of absolute hydrogen peroxide. (б) Estimation of Ferrous Sulphate. The reaction proceeds as follows : 2KMnO4 4- 10FeSO4 4- ?H2O 4- 8H2SO4 = 5(Fe2(SO4)3) 4- 315.3 2774.2 (558.8 Fe.) K2SO4 -I- 2MnSO4 4- 15H2O That is, 315.3 parts of 2KMnO4 correspond to 558.8 parts of Fe or to 2774.2 parts of FeSO44-7H2O. 1000 Cc. of the decinormal permanganate (containing 3.153 Gm. of the salt) correspond to 5.588 Gm. of metallic iron, or to 27.742 Gm. of crystallized ferrous sulphate. Hence, 1 Cc. of the decinormal permanganate (containing 0.003153 Gm. of the salt) corresponds to 0.027742 Gm. of crystallized ferrous sulphate. VOLUMETRIC ANALYSIS. 443 (c) Estimation of Metallic Iron. The metallic iron is dissolved in a flask containing dilute sul- phuric acid under the same precautions, to avoid oxidation, as directed under potassium bichromate (page 437, a). The result- ing solution contains the iron as ferrous sulphate.:— 5Fe.2 + 10H2SO4 = 10FeSO4 + 5H2 558.8 1517 The decinormal permanganate solution is now run in, until the solution, after stirring, retains a faint pink color. 2KMnOt + lOFeSO, + 8H2SO4 = 5(Fe2(SO4)s) + K2SO4 + 315.3 1517 (558.8 Fe) 2MnSO4 + 8H2O 1 Cc. of the decinormal permanganate (containing 0.003153 Gm. of the salt) corresponds to 0.01517 Gm. of anhydrous ferrous sulphate or to 0.005588 Gm. of metallic iron. (d) Estimation of Ferrous Carbonate. A weighed amount of ferrous carbonate is dissolved in dilute sulphuric acid and titrated as directed in the U. S. P. The reaction is as follows:— 10FeCO3 -f- 10H2SO4 = 10FeSO4 + 10CO2 + 10H2O 1157.3 (558.8 Fe). 1517 2KMnO4 + lOFeSO, + 8H2SO4 = 5(Fe2(SO4)3) + 2MnSO4 + 315.3 1517 (558.8 Fe). K2SO4 + 8H2O. That is, 315.3 parts of permanganate correspond to 558.8 parts of metallic iron, which in turn corresponds to 1157.3 Gm of fer- rous carbonate. 1 Cc. of decinormal potassium permanganate solu- tion (containing 0.003153 Gm. of the salt) corresponds to 0.005589 Gm. of metallic iron, or to 0.011573 Gm. of ferrous carbonate. (e) Estimation of Hijpophosphorous Acid, Free and in Hypophos- phites. The reaction occurring in these titrations is as follows:— 2K2Mn2O8 4- 5HSPO2 4- 6H2SO4 = 2K2SO4 4- 4MnSO4 + 2 X 315.3 329.4 6H2O 4- 5H3PO4. 315.3 parts of Permanganate correspond to 164.7 parts of Hypophosphorous acid. 1 Cc. of permanganate solution (containing 0.003153 Gm. of potassium permanganate) corresponds to 0.001647 Gm. of hypo- phosphorous acid or to a corresponding amount of any hypo- phosphite. (12) Decinormal Bromine Volumetric Solution. [Koppeschaak’s Solution.] Br = 79.76 7.976 Gm. in 1 Liter. (NaBrO3 = 150.64.— NaBr = 102.76.) (KBtO3 = 166.67.—KBr = 118.79.) “ Dissolve 3 Gm. of sodium bromate and 50 Gm. of sodium 444 HANDBOOK OF PHARMACY. bromide (or 3.2 Gm. of potassium bromate and 50 Gm. of potas- sium bromide) in enough water to make, at or near 15° C. (59° F.), 900 Cc. Of this solution transfer 20 Cc., by means of a pipette, into a bottle having a capacity of about 250 Cc., provided with a glass stopper; add 75 Cc. of water, next 5 Cc. of pure hydrochloric acid, and immediately insert the stopper. Shake the bottle a few times, then remove the stopper just sufficiently to quickly introduce 5 Cc. of potassium iodide T. S., taking care that no bromine vapor escape, and immediately stopper the bottle. Agitate the bottle thoroughly, remove the stopper and rinse it and the neck of the bottle with a little water so that the washings flow into the bottle, and then add from a burette deci- normal sodium hyposulphite V. S. until the iodine tint is exactly discharged, using toward the end a few drops of starch T. S. as indicator. Note the number of Cc. of the sodium hyposulphite V. S. thus consumed, and then dilute the bromine solution so that equal volumes of it and of decinormal sodium hyposulphite V. S. will exactly correspond to each other under the conditions men- tioned above. Example.—Assuming that the 20 Cc. of the bromine solution have required 25.2 Cc. of the hyposulphite to completely discharge the iodine tint, the bromine solution must be diluted in the pro- portion of 20 to 25.2. Thus, if 850 Cc. of it are remaining, they must be diluted with water to measure 1071 Cc. After the solution is thus diluted, a new trial should be made in the manner above described, in which 25 Cc. of the decinormal sodium hyposulphite V. S. should exactly discharge the tint of the iodine liberated by the bromine set free from the 25 Cc. of bromine solution. Keep the solution in dark amber-colored,glass-stoppered bottles.” One Cubic Centimeter of Decinormal Bromine Solution V. S. is the equivalent of: Gramme. Bromine, Br 0.007976 Carbolic Acid, C6H5OH 0.001563 On mixing potassium or sodium bromate with their respective bromides in presence of hydrochloric or sulphuric acid and water, bromine is set free according to the following reaction. KBrO, + 5KBr + 6HC1 = 6KC1 + 3H2O + 3Br2 In order to ascertain the normal amount of bromine present, for the purpose of standardization, potassium iodide is introduced, whereby a quantity of iodine exactly equivalent to the free bro- mine present is liberated. Upon estimating the amount of the liberated iodine with sodium hyposulphite, the result represents the equivalent amount of bromine:— Br2 = I2 = 2(Na2S2O3,5H2O) 2 X 79.76 2 X 126-6 2 X 247.64 79.76 parts = 126.6 parts = 247.64 parts. VOLUMETRIC ANALYSIS. 445 That is, 1 Cc. of decinormal hyposulphite solution (containing 0.024764 Gm. of sodium hyposulphite) corresponds to 0.01266 Gm. of Iodine, which in turn represents 0.007976 of Bromine. This solution is employed in the valuation of carbolic acid, depending, for its action, upon the formation of tribrom-phenol, in which an excess of the bromine solution is added to a weighed amount of carbolic acid dissolved in water; the excess of bromine which has not combined with the phenol, is estimated as explained above; that is, the equivalent amount of iodine liberated from potassium iodide added is determined by sodium hyposulphite, the difference being the amount of combined bromine. The reaction proceeds thus:— 6Br + C6H5OH = C6H2Br3OH + 3HBr Bromine. Phenol. Tribrom-phenol. Hydrobromic Acid. 79.76 parts of bromine correspond to 15.63 parts of phenol. Hence 1 Cc. of the bromine solution (containing 0.007976 Gm. of bromine) corresponds to 0.001563 Gm. of phenol. APPENDIX. TABLE OF ATOMIC WEIGHTS. According to L. Meyer and K. Seubert. Name. Symbol. Atomic Weight. Name. Symbol. Atomic. Weight. Aluminum, .... Al 27.04 Molybdenum. . . Mo 95.9 Antimony, ... Sb 119.6 Nickel, Ni 58.6 Arsenic, As 74.9 Nitrogen, .... N 14.01 Barium, Ba 136.9 Osmium, Os 190.3 Beryllium,* .... Be 9.03 Oxygen, O 15.96 Bismuth, Bi 208.9 Palladium, .... Pd 106.35 Boron, B 10.9 Phosphorus, . . . P 30.96 Bromine, Br 79.76 Platinum, .... Pt 194 3 Cadmium, .... Cd 111.5 Potassium, .... K 39.03 Caesium, Cs 132.7 Rhodium, Rh 102.9 Calcium, Ca 39.91 Rubidium, .... Rb 85.2 Carbon, C 11.97 Ruthenium, .... Ru 101.4 Cerium, Ce 139.9 Samarium, .... Srn 149.62 Chlorine, Cl 35.37 | Scandium, .... Sc 43.97 Chromium, .... Cr 52.0 Selenium, .... Se 78.87 Cobalt, ..... Co 58.6 Silicon, Si 28.3 Columbium ,f . . . Cb 93.7 Silver, Ag 107.66 Copper, Cu 63.18 Sodium, . ... Na 23.0 Didymium. J • • • Di 142.0 Strontium, .... Sr 87.3 Erbium, Er 166.0 Sulphur, S 31.98 Fluorine, F 19.0 Tantalum, .... Ta 182.0 Gallium Ga 69.9 Tellurium, .... Te 125.0 Germanium, . . . Ge 72.3 Terbium, Th 159.1 Gold, Au 196.7 Thallium, .... T1 203.7 Hydrogen, H 1.0 Thorium, .... Th 231.9 Indium, In 113.6 Tin, Sn 118.8 Iodine, I 126.53 Titanium, .... Ti 48.0 Iridium, Ir 192.5 Tungsten, .... W 183.6 Iron, Fe 55.88 | Uranium, U 238.8 Lanthanum, . . . La 138.2 Vanadium, .... V 51.1 Lead Pb 206.4 Ytterbium, .... Yb 172 6 Lithium, Li 7.01 1 Yttrium, Yt 88.9 Magnesium, .... Mg 24 3 Zinc, Zn 65.1 Manganese, .... Mu 54.8 Zirconium,. .... Zr 90.4 Mercury, Hg 199.8 * Also called Glucinum, G1 = 9.03. + Also called Niobium, Nb = 93.7. t Composed of Neo- and Praseo-Didymium. 447 448 HANDBOOK OF PHARMACY. TABLE OF SOLUBILITIES.* IN WATER, ALCOHOL, ETHER, CHLOROFORM AND GLYCERIN, OF MEDICINAL SUB- STANCES OFFICIAL IN THE U. S. PHARMACOPOEIA, INCLUDING MANY OTHERS OF COMMON OR FREQUENT USE. Abbreviations— s., soluble; v. s., very soluble; sp., sparingly; a., all proportions; si., slightly; ins., insoluble; n. ins., nearly insoluble; dec., decomposed. Medicinal Substances. One part is soluble in [at 59° F (15° C.) U. 8. P. Standard Temperature.] Parts of Water. Alcohol. Ether. Chloroform. Glycerin. Acacia, 2 ins. Acetanilid, 194 5 18 V. s. Acid, Arsenic 2 5 Arsenous, 80 141 5 Benzoic, 500 2 3 7 10 Boric 25 15 10 Carbolic, Anhyd, 15 a. a. a. a. Chromic, ... V. s. dec. dec. ins. dec. Citric 0.63 1.61 18 50 2 Formic, V. 8. V. s. 3 8. Gallic, 100 5 40 12 Lactic, a. a. a. ins. Meconic sp. v. s. Oleic, ins. a. a. a. Oxalic, cryst 8.17 6.8 n. ins. ins. 7.5 Phosphoric, Glacial, V. s. V. 8. ins. Picric, 86 s. s. s. Pyrogallic, (see Pyrogallol), . . . . Salicylic, 450 2.4 2 80 60 Stearic, ins. 45 9 s. Succinic, 19 8 79 n. ins. Tannic, 1 0.6 n. ins. n. ins. 9 Tartaric, 0.8 2.5 250 n. ins. a. Valerianic, 30 a. 2 3 s. Aconitine, • 150 5 2 3 Alcohol, a. a. a. a. Amylic, sp. a. a. Alum, 9 ins. ins. ins. 2.5 Exsiccated, 20 ins. ins. ins. V. 8. Aluminum Hydrate, ins. ins. ins. ins. ins. Sulphate, 1.2 ins. ins. ins. ins. Ammonium Benzoate, 5 28 ins. ins. ins. Bicarbonate, 8 ins. Borate, 12 Bromide 1.5 30 600 Carbonate, 4 dec. ins. Chloride, 3 sp. sol. ins. 5 Iodide, 1 9 ins. Nitrate, 0.5 20 Oxalate, 3 Phosphate, 4 ins. Sulphate, 1.3 sp. Valerianate V. s. V. s. Amyl Acetate, ins. a. a. Nitrite, ins. a. a. a. Anilin, si. a. a. a. Antifebrin, (see Acetanilid), . . . Antimony Arseniate ins. ins. Oxide, n. ins ins. ins. ins. Sulphide, ins. ins. and Potassium Tartrate, . . 17 ins. ins. 20 20 Antipyrin, 1 1 50 Apocodeine, ins. s. s. s. Apomorphine Hydrochlorate, . . . 6.8 25 si. sl. Aristol, ins. sp. s. s. Arsenic Bromide, dec. Iodide, 3.5 10 sol. Atropine, 130 3 16 4 50 Hydrochlorate, V. s. V. s. sl. Sulphate, 0.4 6.2 2270 694 3 Balsam Peru, 5 * “ Era” Formulary. TABLE OF SOLUBILITIES. 449 TABLE OF SOLUBILITIES.—Continued. Medicinal Substances. One part is soluble in [at 59° F. (15° C.) U. S. P. Standard Temperature.] Parts of Water. Alcohol. Ether. Chloroform. Glycerin. Balsam Tolu, n. ins. s. s. s. Barium Acetate, 2 100 Bromide, V. s. s. Carbonate, ins. n. ins. Chloride, ins. 10 Nitrate, 8-12 ins. Benzanilide, n. ins. 58 Benzene, ins. s. s. Benzin, ins. 6 s. s. Bebeerine, 6000 sol. 13 s. Hvdrochlorate, s. s. Sulphate, s. V. s. Berberine, 500 250 ins. Hvdrochlorate, 600 sp. ins. Bismuth Chloride ins. ins. Citrate, ins. ins. Oxide, ins. ins. Oxyiodide, ins. ins. Salicylate, ins. ins. ins. Subcarbonate, ins. ins. ins. Subgallate, ins. ins. ins. Subnitrate, ins. ins. Tannate, ins. ins. and Ammonium Citrate, . . v. s. sp. Bromal Hydrate, s. s. s. s. s. Bromine, 30 s. (dec.) s. (dec.) s. Bromoform, v. sp. s. s. Brucine 750 2 ins. 50 Sulphate, V. s. V. s. Butyl Chloral Hydrate, 50 1 s. n. ins. 1 Cadmium Acetate, V. s. Chloride 0.7 s. Iodide, 2 sol. Sulphate, V. s. V. s. Caffeine 80 33 555 y Citrate, 30 s. Phosphate, V. s. Calcium Acetate, s. s. Benzoate, 29 Bromide, 0.7 1 Carbonate, ins. ins. ins. ins. Chloride 8 ins. Hypophosphite, 6.8 ins. Hyposulphite, 1 Iodide, s. Lactate, 9-12 s. ins. Phosphate, .... ins. ins. ins. Sulphate, 382 ins. Sulphite, 800 . . . 20 Camphor, sp. v. s. v. s. v. s. Monobromated n. ins. 6 v. s. v. s. sl. Cannabine Tannate, si. sl. sl. Carbon Disulphide, 535 V. s. V. s. V. s. Cerium Acetate, V, s. s. Bromide, si. s. Nitrate, s. s. Oxalate, ins. ins. ins. Chinoidine, n. ins. sp. s. s. Chloral, v. s. V. s. V. s. V. s. s. Chloroform, 200 a. a. Chrvsarobin, n. ins. sp. s. Cinchonine, 3760 116 526 163 200 Hydrochlorate, . . . 22 1 550 Sulphate, 66 10 ins. 78 16 Cinchonidine, 2500 20 80 10 Hvdrochlorate, 27 .8. n. ins. n. ins. Sulphate 70 66 ins. 1316 Codeine, 80 3 30 2 Hydrochlorate 20 Sulphate, 35 Phosphate, 4 sp. Cocaine, 700 v. s. V. s. Hydrochlorate, 0.48 3.5 2800 17 450 HANDBOOK OF PHARMACY. TABLE OF SOLUBILITIES.—Continued. Medicinal Substances. One part is soluble in [at 59° F. (15° C.) U. S. P. Standard Temperature.] Parts of Water. Alcohol. Ether. Chloroform. Glycerin. Coniine, 100 V. s. 6 1 Hydrobromate, 2 2 8. 8. Copper Acetate 15 16 ins. 10 Ammoniated, ins. Chloride, V. s. V. 8. Lactate, 2-6 8. Nitrate, 8. s. Sulphate, 2.6 n. ins. ins. 3% Creosote, 150 s. a. a. Delphinine, n. ins. 8 s. 8. Digitalin, 1000 s. ins. Digitin 8. Diuretin, sl. sp. Duboisine, 500 V. s. 8. S. Sulphate, 8. 8. Elaterin, 4250 337 543 2.4 Emetine, 2000 8. sp. V. s. Ergotinine, ins. V. 8. V. s. V. s. Ether Acetic, 8 a. a. Butyric, sl. a. Formic, sp. a. a. Sulphuric, 12 a. a. Ethyl Bromide, sp. a. a. Iodide, n. ins. V. 8. V. 8. Eucalyptol, a. Eugenol, sp. v. s. V. s. Euphorin, sl. Europhen, ins. s. Gelseminine, n. ins. s. 25 V. s. Tartrate, v. s. V. 8. Glycerin, a. a. ins. ins. Glvcyrrhizin, Ammoniated, .... s. s. Gold Bromide (mono), ins. (tri), s. Chloride (tri), s. s. s. Iodide, ins. ins. and Sodium Chloride, .... 2 sp. Guaiacol, 200 a. a. Benzoate, ins. s. v. s. V. s. Gutta Percha, ins. ins. 8. Hydrastinine, n. ins. V. 8. V. s. V. s. Hydrochlorate, 0.3 3 n. ins. n. ins. Hydroquinone, 20 V. 8. V. 8. . . . Hyoscine, sl. V. S. V. s. Hydrobromate, 1.9 13 sl. sl. Hydrochlorate, .... s. ins. ins. Hyoscyamine, 500 v. s. s. 8. Hydrobromate, 0.3 2 3000 250 Sulphate 0.5 .5 sl. sl. Hypnone, n. ins. V. 8. V. 8. s. Ichthyol, 8. sp. sp. s. s. Iodine, 5000 10 3 s. 50 Iodoform., n. ins. 52 5.2 V. 8. Iodol, 5000 3 1 Iron Acetate, 4 8. Albuminate, 8. ins. Arsen iate, ins. ins. Bromide, s. s. Carbonate Saccharated, .... sp. ins. Chloride (Ferric), V. s. v. s. sl. Citrate, s. ins. ins. Hypophosphite, n. ins. Iodide, s. s. Iodide, Saccharated, 7 n. ins. Lactate, 40 ins. ins. 7 Nitrate, 8. s. Oxalate, n. ins. ins. Phosphate (Soluble), V. 8. ins. Pyrophosphate, V. 8. ins. Santonate, n. ins. V. s. sp. s. Sulphate, 1.8 ins. ins. 4 Valerianate, ins. V. s. and Ammonium Chloride, . . ins. TABLE OF SOLUBILITIES. 451 TABLE OF SOLUBILITIES.—Continued. Medicinal Substances. One part is soluble in [at 59° F. (15° C.) U. S. P. Standard Temperature.] Parts of Water. Alcohol. Ether. Chloroform. Glycerin. Iron and Ammonium Citrate, . . . s. ins. Ammonium Sulphate, . . 3 ins. Ammonium Tartrate, . . V. s. ins. 13 Potassium Tartrate, . . . V. s. ins. Quinine Citrate, 2-3 sp. Strychnine Citrate, . . . s. sp. Katrine, 6 20 ins. Lead Acetate, 2.3 21 ins. 3 5 Carbonate, ins. ins. Chloride, 140 200 Chromate, ins. Iodide, 2000 sp. n. ins. Nitrate, 2 n. ins. Oxide, n. ins. ins. Sulphate, n. ins. ins. Lime, 750 ins. 65 Chlorinated, sp. sp. Sulphuretted sl. ins. 20 Lithium Benzoate, 4 12 Bromide, 0.6 V. s. s. Carbonate, 80 ins. ins. Chloride, 1.7 V. 8. Citrate, 2. n. ins. ins. s. Iodide, 0.6 Nitrate, 2 Salicylate, v. s. v. s. Magnesia, n. ins. ins. Magnesium Acetate, s. 8. Benzoate, V. 8. Bromide, V. 8. 8. Carbonate, n. ins. ins. Chloride, 0.6 Lactate, 30 ins. Phosphate, 350 ins. Sulphate, 1.5 ins. ins. Sulphite, 40 ins. ins. Tartrate 122 Manganese Benzoate, 20 sp. Carbonate, ins. ins. Chloride 2% s. ins. Dioxide, ins. ins. ins. Hypophosphite, V. 8. Iodide, s. Lactate 12 8. Phosphate, ins. ins. Sulphate, 0 8 ins. ins. Mastich, ins. sp. s. s. Menthol, sl. V. s. V. 8. V. s. Mercury Bisulphate, 333 ins. ins. Chloride, Ammoniated, . . . ins. ins. Corrosive, 16 3 4 4 Mild, ins. ins ins. Cvanide, 12.8 15 sp. 4 Iodide, Green, n. ins. ins. ins. Red, n. ins. 130 ins. 8. 3’W Oxide, Black, ins. ins. Red, ins. ins. Salicylate, ins. ins. Sulphate, Basic, 2000 ins. Sulphide, Black, . . . ins. Red, ins. ins. Morphine, 4350 300 4000 160 210 Acetate, 2.5 47.6 1700 2100 5 Ilydrobromate, . 25 20 Hydrochlorate, 24 62 sl. sl. 8. Lactate, 8 93 Meconate, 25 V. s. Sulphate 21 702 n. ins. 5 Tartrate, 10 V. s. Naphthalin ins. 15 v. s. V. 8. Naphthol (Alpha), s. V. s. V. 8. (Beta) 1000 0.75 V. 8. V. S. Narceine, 1200 800 ins. 452 HANDBOOK OF PHARMACY. Medicinal Substances. One part is soluble in [at 59° F. (15° C.) U. S. P. Standard Temperature.] Parts of Water. Alcohol. Ether. Chloroform. Glycerin. Narceine, Hydrochlorate, s. V. 8. Narco tine, n. ins. 80 35 3 Nickel Acetate, 6 ins. Bromide, s. 8. 8. Nitrate, 2 8. Phosphate, ins. Sulphate, 4 ins. ins. Nicotine, V. s. v. s. s. 8. Hydrochlorate, V. s. v. s. ins. Nitroglycerin, n. ins. V. s. 8. Orexin, 8. Pancreatin, s. ins. Papaverine, . . ins. sp. 8. 8. Paraffin, ins. ins. 8. S. Paraldehyde, 8.5 a. a. Pelletierihe, V. s. v. s. V. 8. V. 8. Tannate, 700 80 Pepsin, 100 ins. ins. ins. Petrolatum, ins. ins. 8. s. Phenacetin, sp. 16 8. Phenocoll Hydrochlorate, 16 Phenyl Hydrazine, sp. V. 8. V. s. Phosphorus, ins. 8. 80 V. s. 500 Physostigmine, sp. V. S. V. s. 8. Salicvlate, 130 12 Sulphate, s. Picrotoxin, 240 9 si. sl. Pilocarpine, s. V. 8. 8. 8. Hydrochlorate, V. 8. V. S. n. ins. n. ins. Hydrobromate, s. 8. s. Nitrate, 9 40 8. Sulphate, 8. 8. 8. 8. Piperazine, V. 8. Piperin, n. ins. 30 si. 8. Podophyllin, n. ins. 8. sp. Potassa, Sulphurated, 2 sp. Potassium Acetate, 0.36 1.9 ins. Arseniate, 5.3 25 2 Arsenite, V. 8. sp. Benzoate, V. S. Bicarbonate, 3.2 n. ins. ins. Bichromate, 10 ins. ins. Bisulphate, 2 ins. Bisulphite, V. s. Bi tart rate, 201 sp. ins. Bromide, 1.6 200 ins. 4 Carbonate, 1.1 ins. ins. Chlorate, 16.7 sp. ins. 30 Chloride, 3 8. ins. 30 Citrate, 0.6 sp. Cyanide, 2 sp. 3.5 Ferricyanide, 4 sp. Ferrocyanide, 4 ins. Hydrate, 0.5 2 si. Hypophosphite 0.6 7.3 Iodide, 0.75 18 ins. 2.5 Nitrate, 3.8 sp. ins. Nitrite, V. s. Oxalate, 8. Permanganate 16 dec. ins. Phosphate, 8. Salicvlate, 8. 8. ins. Sulphate, 9.5 ins. ins. Tartrate, 1 ins. ins. and Sodium Tartrate, .... 1.4 n. ins. ins. Pyoktanin, 75 12 ins. 8. 50 Pyridine, a. V. s. v. s. Nitrate, V. s. sp. Sulphate, v. s. V. s. Pyrodine Hydrochlorate, sp. V. s. ins. Pyrogallol, 1.7 1 1.2 Quinidine, 2000 20 30 Hydrochlorate 27 V. 8. ins. TABLE OF SOLUBILITIES. .—Continued. TABLE OF SOLUBILITIES. 453 TABLE OF SOLUBILITIES. .—Continued. Medicinal Substances. One part is soluble in [at 59c F. (15° C.) U. S. P. Standard Temperature.] Parts of Water. Alcohol. Ether. Chloroform. Glycerin. Quinidine Sulphate, 100 8 n. ins. 14 Quinine, . . 1670 6 23 5 200 Acetate, 600 7 Arseniate, sp. Arsenite, sp. 15 *25 8 Benzoate, - . 350 Bisulphate, 10 32 ins. Hydrobromate 54 0.6 6 12 s. Hydrochlorate, 34 3 ins. 9 Hypophosphite, 45 10 Lactate, 3 s. Phosphate, . . . 700 si. Salicylate, 225 20 120 V. s. Sulphate, 740 65 sl. 680 40 Tannate, n. ins. sl. 135 Valerianate, 100 5 s. Quinoline Nitrate, V. s. V. 8. ins. Salicylate, 100 Tartrate, s. Resin, ins. S. s. s. Resorcin, 0.6 0.5 V. s. sl. V. s. Retinol, ins. ins. sol. Saccharin, 230 30 0.3 s. Salicin, 28 30 n. ins. n. ins. Salol, n. ins. 10 0.3 V. s. Sanguinarine, ins. V. s. V. 8. s. Nitrate n. ins. Sulphate, s. s. Santonin, 5000 40 140 4 Scoparine, n. ins. s. Silver Acetate, 100 sp. Bromide, ins. Chloride, ins. Cyanide, ins. ins. Iodide, ins. ins. Nitrate, 0.6 26 Oxide, _ . n. ins. ins. Sulphate, 200 Sodium Acetate, 1.4 30 ins. Arsenate, 4 sp. 2 Arsenite, s. sp. . . . Benzoate, 1.8 45 ins. Bicarbonate, 11.3 ins. ins. 13 Bisulphite, 4 72 Borate, 16 ins. ins. 2 Bromide, 1.2 13 ins. Carbonate, 1.6 ins. ins. 1.02 Chlorate, 1.1 100 5 Chloride, 2.8 n. ins. ins. ins. 5 Citrate, V. s. Formate, s. s. Hydrate, 1.7 v. s. Hypophosphite, 1 30 ins. Hyposulphite, 0 65 ins. Iodide, 0.6 3 ins. Lactate, V. s. V. s. ins. Nitrate, 1.3 100 ins. Nitrite, 1.5 sl. Phosphate, 5.8 ins. ins. Pyrophosphate 12 ins. Salicylate, 0.9 6 ins. s. Santoninate, 3 12 ins. Sulphate, .... 2.8 ins. ins. s. Sulphide, V. s. sl. Sulphite, 4 sp. Sulphocarbolate, 4.8 132 Tartrate, 5 ins. Valerianate, V. s. s. Solanine, ins. 400 sl. Sozal, v. s. V. s. s. Sparteine, sp. V. s. V. s. v. s. Sulphate, V. s. V. s. Spermaceti, ins. n. ins. s. s. 454 HANDBOOK OF PHARMACY. Medicinal Substances. One part is soluble in [at 59° F. (15° C.) U. S. P. Standard Temperature.] Parts of Glycerin. Water. Alcohol. Ether. Chloroform. Strontium Bromide, 1.05 s. Carbonate, sl. Chloride, 2 20 Iodide, 0.6 8. sl. Lactate, 4 S. Nitrate, 5 ins. Sulphate, sl. ins. Strophanthin, s. 8. ins. Strychnine, 6700 110 ins. 7 400 Acetate, 75 15 Hydrobromate, 32 sp. Hydrochlorate, 50 Nitrate, 75 100 ins. 30 Sulphate, 50 109 ins. 5 Sugar, Cane, 0.5 175 ins. ins. s. Milk, 6 ins. ins. ins. Sulphonal, 500 65 125 Sulphur Iodide, ins. sp. sp. 60 Precipitated, ins. ins. 8. s. Sublimed, ins. ins. S. 8. Washed, ins. ins. s. S. Terebene, sl. s. Terpin Hydrate, 250 10 10 200 Terpinol ins. 8. 8. Tetronal, sl. V. S. S. Thalline Sulphate, 7 100 sl. sl. Tartrate, 10 sp. n. ins. Trimethylamine, s. s. Hydrochlorate, s. s. Trional, 320 V. s. v. s. Thymol, 1200 1 0.8 6.7 120 Uranium Acetate, 10 sl. Chloride s. Nitrate, V. s. V. 8. 4 Urea, 1 ins. ins. 2 Urethane s. 8. 8. Urexine, sp. s. Vanilla, sp. 8. 8. s. Veratrine, sl. 3 6 2 Hydrochlorate, V. s. V. 8. Zinc Acetate, 2.7 36 ins. Bromide, V. s. V. 8. Carbonate, Precipitated, . . ins. ins. Chloride, 0.3 V. 8. 8. 2 Cyanide, ins. ins. Iodide, v. s. v s. v. s. 2.5 Lactate, 60 ins. Nitrate V. s. 8. Oxide, ins. ins. Permanganate, v. s. V. 8. explodes. Phosphate, ins. ins. Phosphide, ins. ins. Salicylate, 25 3.5 36 Sulphate, 0.6 ins. ins. 3 Tannate, ins. ins. Valerianate, 100 40 n. ins. TABLE OF SOLUBILITIES.—Continued. LIST OF THE PRINCIPAL PHARMACOP(EIAL CHEMICALS AND REAGENTS.* Acetanilid,C6H5NH.C2H3O134.73 Acid, Acetic,HC2H3O259.86 “ Arsenous,As.2O3197.68 “ Aurochloric,HAuC14 + 2H2O 375.10 “ Benzoic,HC7H5O2121.71 “ Boric, H3BO361.78 “ Carbolic, C6H5OH93.78 “ Chloroplatinic,H2PtCl6 + 6H2O516.28 “ Chromic,CrO399.88 “ Citric, H3C6H5O7 + H2O 209.50 “ “ dry,H3C6H5O7191.54 “ Gallic, HC7H5O5 + H2O187.55 “ “ dry,HC7H5O5169.59 “ Hydriodic, HI127.53 “ Hydrobromic,HBr80.76 “ Hydrochloric,HC136.37 “ Hydrocyanic,HCN26.98 “ Hydrosulphuric (See Hydrogen Sulphide). “ Hypophosphorous,HPH2O265.88 “ Lactic,HC3H5O389.79 “ Nitric, HNOS62.89 “ OleicHC18H33O2281.38 “ Oxalic,H2C2O4 + 2H2O 125.70 “ “ dry, . . H2C2O489.78 “ Phosphoric,H3PO497.80 “ Picric, C6H2(NO2)3OH 228.57 “ Pyroboric,H2B4O7 157.32 “ Pyrogallic (See Pyrogallol). “ Salicylic,HC7H5O3137.67 “ Stearic,HC18H35O2 283.38 “ Sulphuric,H2SO497.82 “ Sulphurous,H2SO381.86 “ Tannic,HCj4H9O9321.22 “ Tartaric, H2C4H4O6 149.64 “ Tetraboric (See Pyroboric). Alcohol, ethylic,C2H5OH45.90 “ methylic,CH3OH31.93 Aldehyde, ethylic,C2H4O43.90 Alum (See Aluminum and Potassium Sulphate). Aluminum Hydrate, A12(OH)6155.84 “ and Potassium Sulphate, . . A12K2(SO4)4 + 24H2O 946.46 “ “ “ dry, . A12K2(SO4)4 515.42 “ Sulphate,A12(SO4)3 + 16H2O 628.90 “ “ dry, A12(SO4)3341.54 Ammonia, NH317.01 Ammonium Acetate,NH4C2H3O276.87 *U. S. Pharmacopoeia, 1890. 455 456 HANDBOOK OF PHARMACY. Ammonium Arsenite (Metarsenite), . . . NH4AsO2124.83 “ Benzoate,NH4C7H5O2138.72 “ Bromide,NH4Br97.77 “ Carbonate (normal), .... (NH4)2CO395.87 “ “ (U.S.P.), .... NH4HCO3.NH4NH2CO2 .... 156.77 “ Chloride,NH4C153.38 “ Citrate,(NH4)3C6H5O7 242.57 “ Iodide,NH4I 144.54 “ LactateNH4C3H5O3106.80 “ Molybdate,(NH4)2MoO4195.76 “ Nitrate,NH4NO379.90 “ Oxalate, (NH4)2C2O4 + H2O141.76 “ “ dry, (NH4)2C2O4123.80 “ Phosphate, (NH4)2HPO4131.82 “ Salicylate,NH4C7H5O3154.68 “ Sulphate,(NH4)2SO4131.84 “ Sulphhydrate,NH4HS50.99 “ Sulphide,(NH4)2S68.00 “ Tartrate, (NH4)2C4H4O6183.66 “ Valerianate,NH4C5H9O2118.78 Amyl Nitrite,C5HnNO2116.78 Antimony Oxide (Trioxide),Sb2O3 287.08 “ and Potassium Tartrate, . . . 2K(SbO)C4H4O6 + H2O .... 662.42 “ “ “ “ dry, . K(SbO)C4H4O6 322.23 “ SulphideSb2S3 335.14 Apomorphine Hydrochlorate,C17H17NO2HC1 302.79 Arsenic Iodide,Asl3 454.49 “ Trioxide (See Acid, Arsenous). Atropine,C17H23NO3 288.38 “ Sulphate,(C17H23NO3)2H2SO4 674.58 Barium Carbonate,BaCO3196.75 “ Chloride,BaCl2 + 2H2O 243.56 “ “ dry,BaCl2 207.64 “ Dioxide,BaO2168.82 “ Hydrate,Ba(OH)2170.82 “ Nitrate, Ba(NO3)2 260.68 Benzol (Benzene),C6H677.82 Bismuth Citrate,BiC6H5O7 397.44 “ Subcarbonate (approximately), . (BiO)2CO3 509.57 “ Subnitrate (approximately), . . BiONO3(OH)2 304.71 Boron Trioxide,B2O3 69 68 Brucine,C23H26N2O4 + 4H2O 465.01 “ dry,C23H2BN2O4 393.17 Caffeine,C8H10N4O2 + H2O211.68 “ dry,C8H10N4O2193.72 Calcium Bromide,CaBr2199.43 “ Carbonate,CaCO399.76 “ Chloride,CaCl2 + 6H2O218.41 “ “ dry,CaCl2110.65 “ Hydrate,Ca(OH)273.83 “ Hypophosphite,Ca(PH2O2)2169.67 “ OxideCaO55.87 “ Phosphate,Ca3(PO4)2 309.33 “ Sulphate (Gypsum),CaSO4 + 2H2O171.65 “ “ dry,CaSO4135.73 “ Sulphide (Monosulphide), . . . CaS 71.69 Camphor,C10HlfiO151.66 ‘ ‘ Monobromated, C10H15BrO . 230.42 Carbon Disulphide, CS275.93 Cerium Oxalate,Ce2(C2O4)3 + 9H2O 704.78 “ “ dry, Ce2(C2O4)3 543.14 Chloral Hydrate,C2HC13O + H2O164.97 “ anhydrous, C2HC13O147.01 PRINCIPAL PHARMACOPCEIAL CHEMICALS AND REAGENTS. 457 Chloroform,CHC13119.08 Cinchonidine Sulphate,(C19H22N2O)2H.,SO4 -p 3H2O . . 738.50 “ “ dry,(C19H22N2O)2H2SO4 684.62 Cinchonine,C]9H22N2O 293.41 “ Sulphate,(C19H22N2O)2H2SO4 + 2H2O . . 720.54 “ “ dry,(C19H22N.2O)2H2SO4 684.62 Cobaltous Nitrate,Co(NO3)2 + 6H2O 290.14 Cocaine Hydrochlorate,C17H21NO4HC1 338.71 Codeine,C18H2]NO3 -f- H2O316.31 Codeine, dry,C18H21NO3 298.35 Cupric Ammonium Sulphate,Cu(NH3)4SO4 + H2O 245.00 “ Sulphate, CuSO4 -f- 5H2O 248.80 “ “ dry,CuSO4159.00 “ TartrateCuC4H4O6 + 3H2O 264.70 Diphenylamine,(C6H5)2NH168.65 Elaterin,C20H28O5 347.20 Ether, (See Ethyl Oxide). Ethyl Acetate,C2H5C2H3O287.80 “ Nitrite,C2H5NO274.87 “ Oxide (JEther, U.S.P.)(C2H5)2O73.84 Eucalyptol,Cl0H18O153.66 Ferric Acetate, Fe2(C2H3O2)6 464.92 “ Ammonium Sulphate,Fe2(NH4)2(SO4)4 + 24H2O . . . 962.10 “ “ “ dry, .... Fe2(NH4)2(SO4)4531.06 “ Chloride,Fe2Cl6 + 12H2O 539.50 “ “ dry,Fe2Cl6 323.98 “ Hydrate,Fe2(OH)B213.52 “ Hypophosphite,Fe2(PH2O2)B501.04 “ Nitrate, Fe2(NO3)B 483.10 “ Oxide,Fe2O3159.64 “ Phosphate (normal, not U.S.P.), . . Fe2(PO4)2301.36 “ Pyrophosphate (normal, not U.S.P), Fe4(P2O7)3 744.44 “ Subsulphate (variable) “ Sulphate,Fe2(SO4)3 . ' 399.20 “ Valerianate (variable) Ferrous Bromide,FeBr2215.40 “ CarbonateFeCO3115.73 “ Iodide,’..... Fel2 . . 308.94 “ Lactate,Fe(C3H5O3)2 + 3H2O 287.34 “ Sulphate,FeSO4 + 7H2O 277.42 “ “ dry,FeSO4151.70 “ Sulphide,FeS87.86 Glucose (See Sugar, Grape). Glycerin,C3H5(OH)391.79 Glyceryl Trinitrate, . . ‘C3H2(NO3)3 226.58 Gold Chloride,AuC13 302.81 Hydrastinine Hydrochlorate,CnHuNO2HCl’224.97 Hydrogen Dioxide,’H2O233.92 “ Sulphide,H2S33.98 Hyoscine Hydrobromate,C17H21NO4HBr + 3H2O .... 436.98 “ “ dry,C17H21NO4HBr 383.10 Hyoscyamine Hydrobromate,C17H23NO3HBr 369.14 “ Sulphate, (C17H23NO3)2H2SO4 674.58 Iodoform,CHI3 392.56 Lead Acetate,Pb(C2H3O2l2 + 3H2O 378.00 “ “ dry,Pb(C2H3O2)2 324.12 “ Carbonate,(PbCO3)2Pb(OH)2 772.82 “ Iodide, Pbl2 459.46 “ Nitrate,Pb(NO3)2 330.18 “ OxidePbO 222.36 “ Subacetate (approximately), .... Pb2O(C2H3O2)2 546.48 458 HANDBOOK OF PHARMACY. Lime (See Calcium Oxide). Lithium Benzoate,LiC7H5O2127.72 “ Bromide,LiBr86.77 “ Carbonate,Li2CO373.87 “ Citrate, Li3C6H5O7 209.57 “ Salicylate,LiC7H5O3143.68 Magnesia (See Magnesium Oxide). Magnesium Carbonate (approximately), . (MgCO3)4Mg(OH)2 + 5H2O . . 484 62 “ Oxide,MgO40.26 “ Sulphate, MgSO4 + 7H2O 245.84 “ dry,MgSO4120.12 Manganese Dioxide,MnO2 86 72 Manganous Sulphate, MnSO4 -f- 4H2O 222.46 “ “ dry,MnSO4150.62 MentholC10H19OH155.66 Mercuric Ammonium Chloride,NH2HgCl 251.18 “ Chloride,HgCl2 270.54 “ Cyanide,Hg(CN)2251.76 “ Iodide,Hgl2 452.86 “ Nitrate,Hg(NO3)2 323.58 “ OxideHgO215.76 “ Potassium Iodide,Hgl2 + 2KI 783.98 “ Subsulphate,Hg(HgO)2SO4 727.14 Mercurous Chloride,Hg2Cl2 470.34 “ Iodide,Hg2I2 652.66 “ Nitrate, Hg2(NO3)2 + 2H2O 559.30 Methyl Salicylate,CH3C7H5O3151.64 Morphine, C17H19NO3 + H2O 302.34 “ dry,CI7H19NO3 284.38 “ Acetate,C17H19NO3C2H4O2 4- 3H2O . . . 398.12 “ Hydrochlorate,C17H19NO3HC1 -J- 3H2O .... 374.63 “ “ dry,C]7H19NO3HC1 320.74 “ Sulphate,(C,7H]9NO3)2H2SO4 + 5H2O . . .756.38 “ “ dry,(C17H19NO3)2H2SO4 666.58 Naphtalin,C10H8127.70 Naphtol,C10H7(OH)143.66 Nitrogen Dioxide,NO29.97 Nitroglycerin (See Glyceryl Trinitrate). Paraldehyde,C6H12O3131.70 Phenol (See Acid, Carbolic). Physostigmine Salicylate,C]5H2IN3O2C7H6O3412.08 “ Sulphate,(C15H2]N3O2)2H2SO4 934.28 Picrotoxin,C30H34O13 600.58 Pilocarpine Hydrochlorate,CnH16N2O2HCl 243.98 Piperine,C17H19NO3 284.34 Platinic Chloride,PtCl4 335.78 Potassa (See Potassium Hydrate). Potassium Acetate, KC2H3O297.89 “ Arsenite (Metarsenite), .... KAsO2145.85 “ Benzoate,KC7H5O2 + 3H2O213.62 “ “ dry,KC7H5O2159.74 Bicarbonate,KHCO399.88 “ Bichromate (See Dichromate). “ Bitartrate, KHC4H4O6187.67 “ Bromate,KBrO3166.67 “ Bromide,KBr118.79 “ Carbonate, K2CO3137.91 PRINCIPAL PHARMA COPCEIAL CHEMICALS AND REAGENTS. 459 Potassium Chlorate,KC1O3122.28 “ Chloride,KC174.40 “ Chromate,K2CrO4193.90 “ Citrate,K3C6H5O7 + H2O 323.59 “ “ dry,K3C6H5O7 305.63 “ Cyanide,KCN 65.01 “ Dichromate, K2Cr2O7 293.78 “ Ferricyanide,K6Fe(CN)12 657.70 “ Ferrocyanide,K4Fe(CN)6 4* 3H2O421.76 “ “ dry,K4Fe(CN)6 367.88 “ Hydrate,KOH55.99 “ Hypophosphite,KPH2O2103.91 “ Iodide,KI 165.56 “ Lactate,KC3H5O3 127.82 “ Nitrate,KN03 100.92 “ Permanganate, KMnO4157.67 “ Phosphate,K2HPO4173.86 “ Salicylate, KC7H5O3175.70 “ and Sodium Tartrate, . . . . KNaC4H4O6 + 4H2O281.51 “ “ “ “ dry, . . . KNaC4H4O6 209.67 “ Sulphate,K2SO4173.88 “ Sulphite,K2SO3 + 2H2O193.84 “ “ dry,K2SO3157.92 “ Sulphocyanate, KSCN96.99 “ Tartrate,2K2C4H4O6 + H2O 469.36 “ “ dry,K2C4H4O6225.70 Propenyl Trinitrate (See Glyceryl Trinitrate). Pyrogallol,C8H3(OH\,125.70 Quinidine Sulphate,(C20H24N2O2)2H2SO4 + 2H2O . . 780.42 “ “ dry,(C20H24N2O2)2H2SO4 744.50 Quinine,C20H24N2O2 + 3H2O 377.22 “ dry,C20H24N2O2 323.34 “ Bisulphate,C20H24N2O2H2SO4 + 7H2O . . . 546.88 “ “ dry,C20H24N2O2H2SO4412.16 “ Hydrohromate,C20H24N2O2HBr + H.,0 .... 422.06 “ “ dry, C20H24N2O2HBr 404.10 “ Hydrochlorate, C20H24N2O2HCl + 2H2O .... 395.63 “ “ dry, C20H24N2O2HCl 359.71 “ Sulphate,(C20H24N2O2)2H2SO4 + 7H2O . . 870.22 “ “ dry, (C20H24N2O2)2HsSO4 744.50 “ Valerianate,C20H24N2O2C5H)0O2 + H2O . . . 443.07 Resorcin,C8H4(OH)2109.74 Salicin,C13HI8O7 285.33 Salol,C8H5C7H5O3213.49 Santonin,C15H]8O3 245.43 Silver Cyanide, . AgCN133.64 “ Iodide,Agl 234.19 “ Nitrate,AgNO3169.55 “ Oxide,Ag2O 231.28 “ Sulphate,Ag2SO4311.14 Soda (See Sodium Hydrate). Sodium Acetate,NaC2H3O2 + 3H2O135.74 “ “ dry,NaC2H3O281.86 41 Arsenate,Na2HAsO4 + 7H2O311.46 “ dryNa2HAsO4185.74 “ Arsenite (Metarsenite),NaAsO2129.82 “ Benzoate,NaC7H5O2143.71 “ Bicarbonate, NaHCO383.85 “ Bisulphite,NaHSO3103.86 “ Bitartrate,NaHC4H4O8 + H2O189.60 “ Borate,Na2B4O7 + 10H2O 380.92 460 HANDBOOK OF PHARMACY. Sodium Borate, dry,Na2B4O7201.32 “ Bromate,NaBrO3 150.64 “ Bromide,NaBr102.76 “ Carbonate, + 10H2O 285.45 “ “ dry,Na2CO3105.85 “ Chlorate,NaC103106.25 “ Chloride,NaCl58.37 “ Citrate,2NagC6H5O7 + 11H2O712.64 “ “ dry,Na.iC(1H5O7 257.54 “ Cobaltic Nitrite,Co2(NO2)66NaNO2 4~ H2O . . . 824.32 “ Hydrate,NaOH39.96 “ Hypophosphite,NaPH2O2105.84 “ Hyposulphite,Na2S2O3 4~ 5H2O 247.64 “ “ dry,Na2S2O3157.84 “ Iodide,Nal149.53 “ Lactate, NaC3H5O3111.79 “ Nitrate,NaNO384.89 “ Nitrite,NaNO268.93 “ Nitroprusside,Na2Fe(NO)(CN)5 + 2H2O . . . 297.67 “ Phosphate,Na2HPO4 4- 12H2O 357.32 “ “ dry,Na2HPO4141.80 “ Pyrophosphate,Na4P2O7 + 10H2O 445.24 “ “ dry,Na4P2O7 265.64 “ Salicylate, NaC7H5O3159.67 “ Sulphate,Na2SO4 + 10H2O321.42 “ “ dry,Na2SO4141.82 “ Sulphite,Na2SO3 4- 7H2O251.58 “ “ dry,Na.2SO3125.86 “ Sulphocarbolate,NaSO3C6H4(OH) + 2H2O . . . 231.56 “ Tartrate,Na2C4H4O6 4~ 2H2O 229.56 “ Thiosulphate (See Hyposulphite). Sparteine Sulphate,Ci5H26N2H.2SO4 + 4H2O .... 403.23 “ “ dry,C15H26N2H2SO4331.39 Stannous Chloride,SnCl2 4" 2H2O 225.46 Strontium Bromide,SrBr2 4~ 6H2O 354.58 “ “ dry,SrBr2 246.82 “ Iodide,Srl2 4- 6H.2O 448.12 “ “ dry,Srl2 340.36 Lactate, Sr(C3H5O3)2 + 3H2O318.76 “ “ drySr(C3H5O3)2 264.88 Strychnine,C21H22N20.2 333.31 Sulphate,(C21H22N2O2)2H2SO4 4* 5H2O . . 854.24 “ “ dry, (C21H22N2O2)2H2SO4 764.44 Sugar, Cane, C12H22OU341.20 “ Grape,C6H12O6179.58 “ Milk, C12H22On + H2O 359.16 Sulphur Dioxide,SO263.90 Terebene,C10H16135.70 Terpin Hydrate,C10H18(OH)2 + H2O189.58 Thiosinamiue,CS.N2H3(C3H5)115.88 Thymol,C10H14O149.66 Water,H2O17.96 Zinc Acetate,Zn(C2H8O2)2 + 2H2O218.74 “ “ dry,Zn(C2H3O2)2182.82 “ Bromide, ZnBr2 224.62 “ Carbonate (normal, not U.S.P.), . . . ZnCO3124.95 “ Chloride,ZnCI2135.84 “ Iodide, Znl2318.16 “ Oxide,ZnO81.06 “ Phosphide,Zn3P2 257.22 “ Sulphate,ZnSO4 4- 7H2O 286.64 “ “ dry, ZnSO4160.92 “ Valerianate,Zn(C5H9O.2)2 4- 2H2O 302.56 TABLE OF THERMOMETRIC EQUIVALENTS.* According to the Centigrade and Fahrenheit Scales. Given Sought Centigrade: Fahrenheit: Given Fahrenhf n° F. Sought it: Centigrade: _ 5 (n°—32) 9 n° C. 2 c.° F.° c.° F.° 1 C.° F.° c.° F.° — — — — — — —40 —40 —39.4444 —39 —24.4444 —12 —9.4444 15 0.5556 33 —39 —38.2 —24 —11.2 9 15.8 1 33.8 —38.8889 —38 —23.8889 —11 —8.8889 16 1.1111 34 —38.3333 —37 —23.3333 —10 ! —8.3333 17 1.6667 35 —38 —36.4 —23 —9.4 —8 17.6 2 35.6 —37.7778 —36 —22.7778 —9 —7.7778 18 2.2222 36 —37.2222 —35 —22.2222 —8 —7.2222 19 2.7778 37 -37 —34.6 —22 —7.6 7 19.4 3 37.4 —36.6667 —34 —21.6667 —7 —6.6667 20 3.3333 38 —36.1111 —33 —21.1111 —6 —6.1111 21 3.8889 39 —36 —32.8 — 21 —5.8 —6 21.2 4 39.2 —35.5556 —32 —20.5556 —5 —5.5556 22 4.4444 40 —35 —31 —20 —4 —5 23 5 41 — — — — —34.4444 —30 —19.4444 —3 —4.4444 24 5.5556 42 —34 —29.2 —19 —2.2 —4 24.8 i 6 42.8 —33.8889 —29 —18.8889 —2 1 —3.8889 25 6.1111 43 —33.3333 —28 —18.3333 1 —3.3333 26 6.6667 44 —33 —27.4 —18 —0.4 —3 26.6 7 44.6 —32.7778 —27 —17.7778 0 —2.7778 27 7.2222 45 —32.2222 —26 —17.2222 1 —2.2222 28 7.7778 46 —32 —25.6 —17 1.4 —2 28.4 I 8 46.4 —31.6667 —25 —16.6667 2 —1.6667 29 8.3333 47 —31.1111 —24 —16.1111 3 —1.1111 30 8.8889 48 —31 —23.8 —16 3.2 —1 30.2 9 48.2 —30.5556 —23 —15.5556 4 —0.5556 31 9.4444 49 —30 —22 —15 5 —0 32 10 50 — — — — — — —29.4444 —21 —14.4444 6 10.5556 51 —29 —20.2 —14 6.8 11 51.8 —28.8889 —20 —13.8889 7 11.1111 52 —28.3333 —19 —13.3333 8 11.6667 53 —28 —18.4 —13 8.6 12 53.6 —27.7778 —18 —12.7778 9 12.2222 54 —27.2222 —17 —12.2222 10 12.7778 55 —27 —16.6 —12 10.4 13 55.4 —26.6667 —16 —11.6667 11 13.3333 56 —26.1111 —15 —11.1111 12 . 13.8889 57 —26 —14.8 —11 12.2 14 57.2 —25.5556 — 14 —10.5556 13 14.4444 58 —25 —13 —10 14 15 59 * Taken from U. S. Pharmacopoeia, 1890. 461 462 HANDBOOK OF PHARMACY. TABLE OF THERMOMETRIC EQUIVALENTS.—Continued. c.° F.° C.° F.° C.° F.° C.° F.° 15.5556 60 35.5556 96 55.5556 132 75.5556 168 16 60.8 36 96.8 56 132.8 76 168.8 16.1111 61 36.1111 97 56.1111 133 76.1111 169 16.6667 62 36.6667 98 56.6667 134 76.6667 170 17 62.6 37 98.6 57 134.6 77 170.6 17.2222 63 37.2222 99 57.2222 135 77.2222 171 17.7778 64 37.7778 100 57.7778 136 77.7778 172 18 64.4 38 100.4 58 136.4 75 172.4 18.3333 65 38.3333 101 58.3333 137 78.3333 173 18.8889 66 I 38.8889 102 58.8889 138 78.8889 174 19 66.2 39 102.2 59 138.2 79 174.2 19.4444 67 39.4444 103 59.4444 139 79.4444 175 20 68 40 104 60 140 80 176 20.5556 69 40.5556 105 60.5556 141 80.5556 177 21 69.8 41 105.8 61 141.8 81 177.8 21.1111 70 41.1111 106 61.1111 142 81.1111 178 21.6667 71 41.6667 107 61.6667 143 81.6667 179 22 71.6 42 107.6 62 143.6 82 179.6 22.2222 72 42.2222 108 62.2222 144 82.2222 180 22.7778 73 42.7778 109 62.7778 145 82.7778 181 23 73.4 43 109.4 63 145.4 83 181.4 23.3333 74 43.3333 110 63.3333 146 83.3333 182 23.8889 75 1 43.8889 111 63.8889 147 83.8889 183 24 75.2 44 111.2 64 147.2 84 183.2 24.4444 76 44.4444 112 64.4444 148 84.4444 184 25 77 45 113 65 149 85 185 25.5556 78 45.5556 114 65.5556 150 85.5556 186 26 78.8 45 114.8 66 150.8 86 186.8 26.1111 79 46.1111 115 66.1111 151 86.1111 187 26.6667 80 46.6667 116 66.6667 152 86.6667 188 27 80.6 47 116.6 67 152.6 87 188.6 27.2222 81 47.2222 117 67.2222 153 87.2222 189 27.7778 82 47.7778 118 67.7778 154 87.7778 190 28 82.4 48 118.4 68 154.4 88 190.4 28.3333 83 48.3333 119 68.3333 155 88.3333 191 28.8889 84 48.8889 120 68.8889 156 88.8889 192 29 84.2 49 120.2 69 156.2 89 192.2 29.4444 85 49.4444 121 69.4444 157 89.4444 193 30 86 50 122 70 158 90 194 30.5556 87 50.5556 123 70.5556 159 90.5556 195 31 87.8 51 123.8 71 159.8 91 195.8 31.1111 88 51.1111 124 71.1111 160 91.1111 196 31.6667 89 51.6667 125 71.6667 161 91.6667 197 32 89.6 | 52 125.6 72 161.6 92 197.6 32.2222 90 1 52.2222 126 72.2222 162 92.2222 198 32.7778 91 52.7778 127 72.7778 163 92.7778 199 33 91.4 53 127.4 73 163.4 93 199.4 33.3333 92 53.3333 128 73.3333 164 93.3333 200 33.8889 93 53.8889 129 73.8889 165 93.8889 201 34 93.2 54 129.2 74 165.2 94 201.2 34.4444 94 I 54.4444 130 74.4444 166 94.4444 202 35 95 55 131 75 167 95 203 TABLE OF THERMOMETRIC EQUIVALENTS. 463 TABLE OF THERMOMETRIC EQUIVALENTS.—Continued. c.° F.° C.° F.° C.° F.° C.° F.° 95.5556 204 115.5556 240 135.5556 276 155.5556 312 96 204.8 116 240.8 136 276.8 156 312.8 96.1111 205 ! 116.1111 241 136.1111 277 156.1111 313 96.6667 206 116.6667 242 136.6667 278 156.6667 314 97 206.6 117 242.6 137 278.6 157 314.6 97.2222 207 1 117.2222 243 137.2222 279 157.2222 315 97.7778 208 117.7778 244 137.7778 280 157.7778 316 98 208.4 118 244.4 138 280.4 158 316.4 98.3333 209 118.3333 245 138.3333 281 158.3333 317 98.8889 210 118.8889 246 138.8889 282 158.8889 318 99 210.2 119 246.2 139 282.2 159 318.2 99.4444 211 119.4444 247 139.4444 283 159.4444 319 100 212 120 248 140 284 160 320 — — — — — 100.5556 213 120.5556 249 140.5556 285 160.5556 321 101 213.8 121 249.8 141 285.8 161 321.8 101.1111 214 121.1111 250 141.1111 286 161.1111 322 101.6667 215 121.6667 251 141.6667 287 161.6667 323 102 215.6 122 251.6 142 287.6 162 323.6 102.2222 216 122.2222 252 142.2222 288 162.2222 324 102.7778 217 122.7778 253 142.7778 289 162.7778 325 103 217.4 123 253.4 143 289.4 163 325.4 103.3333 218 123.3333 254 143.3333 290 163.3333 326 103.8889 219 123.8889 255 143.8889 291 163.8889 327 104 219.2 124 255.2 144 291.2 164 327.2 104.4444 220 124.4444 256 144.4444 292 164.4444 328 105 221 125 257 145 293 165 329 — — — — — 105.5556 222 125.5556 258 145.5556 294 165.5556 330 106 222.8 126 258.8 146 294.8 166 330.8 106.1111 223 126.1111 259 146.1111 295 166.1111 331 106.6667 224 126.6667 260 146.6667 296 166.6667 332 107 224.6 127 260.6 147 296.6 167 332.6 107.2222 225 127.2222 261 147.2222 297 167.2222 333 107.7778 226 127.7778 262 147.7778 298 167.7778 334 108 226.4 128 262.4 148 298.4 168 334.4 108.3333 227 128.3333 263 148.3333 299 168.3333 335 108.8889 228 128.8889 264 148.8889 300 168.8889 336 109 228.2 129 264.2 149 300.2 169 336.2 109.4444 229 129.4444 265 149.4444 301 169.4444 337 110 230 130 266 150 302 170 338 — 1 — — — — — — 110.5556 231 130.5556 267 150.5556 303 170.5556 339 111 231.8 131 267.8 151 303.8 171 339.8 111.1111 232 131.1111 268 151.1111 304 171.1111 340 111.6667 233 131.6667 269 151.6667 305 171.6667 341 112 233.6 ' 132 269.6 152 305.6 172 341.6 112.2222 234 132.2222 270 152.2222 306 172.2222 342 112.7778 235 132.7778 271 152.7778 307 172.7778 343 113 235.4 133 271.4 153 307.4 173 343.4 113.3333 236 133.3333 272 153.3333 308 173.3333 344 113.8889 237 133.8889 273 153.8889 309 173.8889 345 114 237.2 134 273.2 154 309.2 174 345.2 114.4444 238 134.4444 274 154.4444 310 174.4444 346 115 239 135 275 155 311 175 347 464 HANDBOOK OF PHARMACY. TABLE OF THERMOMETRIC EQUIVALENTS.—Continued. c.° F.° C.° F.° C.° F.° C.° F.° 175.5556 348 195.5556 384 ' 215.5556 420 235.5556 456 176 348.8 196 384.8 216 420.8 236 456.8 176.1111 349 196.1111 385 216.1111 421 236.1111 457 176.6667 350 196.6667 386 216.6667 422 236.6667 458 177 350.6 197 386.6 217 422.6 237 458.6 177.2222 351 197.2222 387 , 217.2222 423 237.2222 459 177.7778 352 197.7778 388 217.7778 424 237.7778 460 178 352.4 198 388.4 218 424.4 238 460.4 178.3333 353 198.3333 389 218.3333 425 238.3333 461 178.8889 354 198.8889 390 218.8889 426 238.8889 462 179 354.2 199 390.2 219 426.2 239 462.2 179.4444 355 199.4444 391 219.4444 427 239.4444 463 180 356 200 392 220 428 240 464 — 1 — — — 180.5556 357 200.5556 393 220.5556 429 240.5556 465 181 357.8 201 393.8 221 429.8 241 465.8 181.1111 358 201.1111 394 221.1111 430 241.1111 466 181.6667 359 201.6667 395 221.6667 431 241.6667 467 182 359.6 202 395.6 222 431.6 242 467.6 182.2222 360 202.2222 396 222.2222 432 242.2222 468 182.7778 361 202.7778 397 222.7778 433 242.7778 469 183 361.4 203 397.4 1 223 433.4 243 469.4 183.3333 362 203.3333 398 223.3333 434 243.3333 470 183.8889 363 203.8889 399 223.8889 435 243.8889 471 184 363.2 204 399.2 | 224 435.2 244 471.2 184.4444 364 204.4444 400 224.4444 436 244.4444 472 185 365 205 401 225 437 245 473 — — : — — — 185.5556 366 205.5556 402 225.5556 438 245.5556 474 186 366.8 206 402.8 226 438.8 246 474.8 186.1111 367 206.1111 403 226.1111 439 246.1111 475 186.6667 368 206.6667 404 226.6667 440 246.6667 476 187 368.6 207 404.6 227 440.6 247 476.6 187.2222 369 207.2222 405 227.2222 441 247.2222 477 187.7778 370 207.7778 406 227.7778 442 247.7778 478 188 370.4 208 406.4 228 442.4 248 478.4 188.3333 371 208.3333 407 228.3333 443 248.3333 479 188.8889 372 208.8889 408 228.8889 444 248.8889 480 189 372.2 209 408.2 229 444.2 249 480.2 189.4444 373 209.4444 409 229.4444 445 249.4444 481 190 374 210 410 230 446 250 482 — — — 1 — — 190.5556 375 210.5556 411 230.5556 447 250.5556 483 191 375.8 211 411.8 231 447.8 251 483.8 191.1111 376 211.1111 412 231.1111 448 251.1111 484 191.6667 377 211.6667 413 231.6667 449 251.6667 485 192 377.6 212 413.6 232 449.6 252 485.6 192.2222 378 212.2222 414 | 232.2222 450 252.2222 486 192.7778 379 212.7778 415 , 232.7778 451 252.7778 487 193 379.4 213 415.4 233 451.4 253 487.4 193.3333 380 213.3333 416 233.3333 452 253.3333 488 193.8889 381 213.8889 417 233.8889 453 253.8889 489 194 381.2 214 417.2 j 234 453.2 254 489.2 194.4444 382 214.4444 418 234.4444 454 254.4444 490 195 383 215 419 235 455 255 491 465 TABLE OF THERMOMETRIC EQUIVALENTS. TABLE OF THERMOMETRIC EQUIVALENTS.—Continued. c.° F.° C.° F.° C.° F.° C.° F.° 255.5556 492 275.5556 528 295.5556 564 315.5556 600 256 492.8 276 528.8 296 564.8 316 600.8 256.1111 493 276.1111 529 296.1111 565 316.1111 601 256.6667 494 276.6667 530 296.6667 566 316.6667 602 257 494.6 277 530.6 297 566.6 317 602.6 257.2222 495 277.2222 531 297.2222 567 317.2222 603 257.7778 496 277.7778 532 297.7778 568 317.7778 604 258 496.4 278 532.4 298 568.4 318 604.4 258.3333 497 278.3333 533 298.3333 569 318.3333 605 258.8889 498 278.8889 534 298.8889 570 ’ 318.8889 606 259 498.2 279 534.2 299 570.2 319 606.2 259.4444 499 279.4444 535 i 299.4444 571 319.4444 607 260 500 280 536 300 572 320 608 260.5556 501 280.5556 537 300.5556 573 320.5556 609 261 501.8 281 537.8 301 573.8 321 609.8 261.1111 502 281.1111 538 301.1111 574 l 321.1111 610 261.6667 503 i 281.6667 539 1 301.6667 575 321.6667 611 262 503.6 282 539.6 302 575.6 322 611.6 262.2222 504 | 282.2222 540 302.2222 576 322.2222 612 262.7778 505 282.7778 541 302.7778 577 322.7778 613 263 505.4 283 541.4 303 577.4 323 613.4 263.3333 506 283.3333 542 303.3333 578 323.3333 614 263.8889 507 283.8889 543 303.8889 579 323.8889 615 264 507.2 284 543.2 304 579.2 324 615.2 264.4444 508 284.4444 544 304.4444 580 I 324.4444 616 265 509 285 545 305 581 325 617 265.5556 510 285.5556 546 305.5556 582 325.5556 618 266 510.8 286 546.8 306 582.8 326 618.8 266.1111 511 286.1111 547 306.1111 583 326.1111 619 266.6667 512 286.6667 548 306.6667 584 326.6667 620 267 512.6 287 548.6 307 584.6 327 620.6 267.2222 513 287.2222 549 307.2222 585 327.2222 621 267.7778 514 287.7778 550 307.7778 586 327.7778 622 263 514.4 288 550.4 308 586.4 328 622.4 268.3333 515 288.3333 551 308.3333 587 | 328.3333 623 268.8889 516 288.8889 552 308.8889 588 328.8889 624 269 516.2 289 552.2 309 588.2 329 624.2 269.4444 517 289.4444 553 309.4444 589 329.4444 625 270 518 290 554 310 590 330 626 270.5556 519 290.5556 555 310.5556 591 330.5556 627 271 519.8 291 555.8 311 591.8 331 627.8 271.1111 520 291.1111 556 311.1111 592 331.1111 628 271.6667 521 291.6667 557 311.6667 593 331.6667 629 272 521.6 292 557.6 312 593.6 332 629.6 272.2222 522 292.2222 558 312.2222 594 332.2222 630 272.7778 523 292.7778 559 312.7778 595 332.7778 631 273 523.4 293 559.4 313 595.4 333 631.4 273.3333 524 293.3333 560 1 313.3333 596 333.3333 632 273.8889 525 293.8889 561 313.8889 597 333.8889 633 274 525.2 294 561.2 314 597.2 334 633.2 274.4444 526 294.4444 562 314.4444 598 334.4444 634 275 527 295 563 315 599 335 635 EQUIVALENTS OF WEIGHTS AND MEASURES,* Customary and Metric. Note.—The values given for the relation of weight to measure are for Water at the temperature of 4° C. (39.2° F.) in vacuo. For ordinary, practical purposes, these values may be used, without cor- rection. Weights, Customary. Metric Weight and Measure. Gm.] [Cc. Measures, Customary. Grains. oz. Troy- grains. lbs Avoirdupois Fluid ounces, minims. Fluid- ounces and fractions. . oz. grains. 15432.4 32 72.4 2 3 119.9 1000 33 390.6 33.814 15360 32 2 3 47.5 995.312 33 314.5 33.655 15U60.9 31 180.9 2 2 185.9 975.932 33 33 15046.6 31 166.6 2 2 171.6 975 32 464.9 32.968 14880 31 2 2 5 964.208 32 289.7 32.604 14660.7 30 260.7 2 1 223.2 950 32 59.1 32.123 14604.5 30 204.5 2 1 167 946.358 32 32 14400 30 2 ... 400 933.105 31 264.9 31.552 14274.9 29 354.9 2 274.9 925 31 133.3 31.278 14148.2 29 228.2 « 148.2 916.785 31 31 14000 29 80 2 907.185 30 324.2 30.676 13920 29 1 15 357.5 902.000 30 240 30.500 13889.1 28 449.1 1 15 326.6 900 30 207.6 30.432 13691.8 28 251.8 1 15 129.3 887.211 30 30 13562.5 28 122.5 1 15 878.635 29 344.1 29.717 13503.3 28 63.3 1 14 378.3 875 29 281.8 29.587 13440 28 1 14 315 870.898 29 215.2 29.448 13235.4 27 275.4 1 14 110.4 857.637 29 29 13125 27 165 1 14 850.486 28 363.9 28.759 13117.5 27 157.5 1 13 430 850 28 356 28.742 12960 27 1 13 272.5 839.794 28 190.4 28.397 12779 26 299 1 13 91.5 828.064 28 28 12731.7 26 251.7 1 13 44.2 825 27 430.3 27.896 12687.5 26 207.5 1 13 822.136 27 383.8 27.800 12480 26 1 12 230 808.691 27 165.6 27.345 12345.9 25 345.9 1 12 95.9 800 27 24.5 27.051 12322.6 25 322.6 1 12 72.6 798.490 27 27 12250 25 250 1 12 793.787 26 403.7 26.841 12000 25 1 11 187.5 777.587 26 140.7 26.293 11960.1 24 440.1 1 11 147.6 775 26 98.7 26.206 11866.2 24 346.2 1 11 53.7 768.916 26 26 11812.5 24 292.5 1 11 765.437 25 423.6 25.883 11574.3 24 54.3 1 10 199.3 750 25 173 25.360 11520 24 1 10 145 746.484 25 115.9 25.241 11409.8 23 369.8 1 10 34.8 739.343 25 25 11375 23 335 1 10 737.087 24 443.4 24.924 11188.5 23 148.5 1 9 251 725 24 247.2 24.515 11040 23 1 9 102.5 715.380 24 91.1 24.190 10953.4 22 393.4 1 9 15.9 709.769 24 24 10937.5 22 377.5 1 9 708.738 23 463.3 23.966 * Taken from U. S. Pharmacopoeia, 1890. 466 EQUIVALENTS OF WEIGHTS AND MEASURES. 467 Weights, Customary. Metric Weight and Measure. Gm.] [Co. Measures, Customary. Grains. oz. Troy grains. Avoirdupois Fluid ounces, minims. Fluid- ounces and fractions. lbs. oz. grains. 10802.6 22 242.6 1 8 302.6 700 23 321.4 23.670 10560 22 1 8 60 684.277 23 66.2 23.138 10500 21 420 1 8 680.388 23 3.1 23.007 10497.0 21 417 1 7 434.5 680.195 23 23 10416.8 21 336.8 1 7 354.3 675 22 395.7 22.824 10080 21 1 7 17.5 653.173 22 41.4 22.086 10062.5 20 462.5 1 7 652.039 22 23.0 22.048 10040.6 20 440.6 1 6 415.6 650.621 22 22 10031.0 20 431 1 6 406 650 21 469.9 21.979 9645.2 20 45.2 1 6 20.2 625 21 64.1 21.134 9625 20 25 1 6 623.689 21 42.9 21.09 9600 20 1 5 412.5 622.070 21 16.6 21.035 9584.2 19 464.2 1 5 396.7 621.048 21 21 9259.4 19 139.4 1 5 71.9 600 20 138.4 20.288 9187.5 19 67.5 1 5 595.340 20 62.7 20.131 9127.8 19 7.8 1 4 377.8 591.474 20 20 9120 19 1 4 370 590.966 19 471.8 19.983 8873.6 18 233.6 1 4 123.6 575 19 212.6 19.443 8750 18 110 1 4 566.990 19 82.6 19.172 8671.4 18 31.4 1 3 358.9 561.900 19 19 8640 18 1 3 327.5 559.863 18 447 18.931 8487.8 17 327.8 1 3 175.3 550 18 286.8 18.598 8312.5 17 152.5 1 3 538.641 18 102.5 18.214 8215.1 17 55.1 1 2 340.1 532.327 18 18 8160 17 1 2 285 528.759 17 422.1 17.880 8102 16 422 1 2 227 525 17 361.1 17.752 7875 16 195 1 2 510.291 17 122.4 17.255 7758.7 16 78.7 1 1 321.2 502.753 17 17 7716.2 16 36.2 1 1 278.7 500 16 435.3 16.907 7680 16 1 1 242.5 497.656 16 397.2 16.828 7437.5 15 237.5 1 1 481.942 16 142.2 16.297 7330.4 15 130.4 1 330.4 475 16 29.6 16.062 7302.3 15 102.3 1 302.3 473.179 16 16 7200 15 1 200 466.552 15 372.4 15.776 7000 14 280 1 453.592 15 162.1 15.338 6944.6 14 224.6 15 382.1 I 450 15 103.8 15.216 6845.9 14 125.9 15 283.4 443.606 15 15 6720 14 15 157.5 435.449 14 347.6 14.724 6562.5 13 322.5 15 425.243 14 182 14.379 6558.8 13 318.8 14 433.8 425 14 178.0 14.371 6389.5 13 149.5 14 264.5 414.032 14 14 6240 13 14 115 404.345 13 322.8 13.672 EQUIVALENTS OF WEIGHTS AND MEASURES.—Continued. 468 HANDBOOK OF PHARMACY. EQUIVALENTS OF WEIGHTS AND MEASURES-—Continued. Weights, Customary. Metric Weight and Measure. Gm.] [Cc. Measures, Customary. Grains. oz. Troy grains. Avoirdupois Fluid ounces, minims. Fluid- ounces and fractions. lbs. oz. grains. 6172.9 12 412.9 14 47.9 400 13 252.3 13.526 6125 12 365 14 396.893 13 201.8 13.421 5933.1 12 173.1 13 245.6 384.458 13 13 5787.1 12 27.1 13 99.6 375 12 326.5 12.680 5760 12 13 72.5 373.242 12 298 12.621 5687.5 11 407.5 13 368.544 12 221.7 12.462 5476.7 11 196.7 12 226.7 354.884 12 12 5401.3 11 121.3 12 151.3 350 11 400.7 11.835 5280 11 12 30 342.138 11 273.1 11.570 5250 10 450 12 340.194 11 241.6 11.503 5020.3 10 220.3 11 207.8 325.311 11 11 5015.5 10 215.5 ... 11 203 325 10 475 10.989 4812.5 10 12.5 ... 11 311.845 10 261.4 10.545 4800 10 10 425 311.035 10 248.3 10.517 4629.7 9 309.7 10 254.7 300 10 69.2 10.144 4563.9 9 243.9 10 188.9 295.737 10 10 4375 9 55 10 283.495 9 281.3 9.586 4320 9 9 382.5 279.930 9 223.5 9.466 4244 8 404 9 306.5 275 9 143.4 9.299 4107.5 8 267.5 9 170 266.163 9 9 3937.5 8 97.5 9 255.146 8 301.2 8.628 3858.1 8 18.1 8 358.1 250 8 217.7 8.453 3840 8 8 340 248.828 8 198.6 8.414 3651.1 7 291.1 8 151.1 236.590 8 8 3500 7 140 8 226.796 7 321.0 7.669 3472.3 7 112.3 7 409.8 225 7 291.9 7.608 3360 7 7 297.5 217.724 7 173.8 7.362 3194.7 6 314.7 7 132.2 207.016 7 7 3086.5 6 206.5 ? 24 200 6 366.1 6.763 3062.5 6 182.5 7 198.447 6 340.9 6.710 2880 6 6 255 186.621 6 149 6.310 2738.4 5 338.4 6 113.4 177.442 6 6 2700.7 5 300.7 6 75.7 175 5 440.4 5.917 2625 5 225 6 170.097 5 360.8 5.752 2400 5 5 212.5 155.517 5 124.1 5.259 2314.9 4 394.9 5 127.4 150 5 34.6 5.072 2282 4 362 5 94.5 147.869 5 5 2187.5 4 267.5 5 141.748 4 380.7 4.793 1929 4 9 4 179 125 4 108.8 4.227 1920 4 4 170 124.414 4 99.3 4.207 1825.6 3 385.6 4 75.6 118.295 4 4 1750 3 310 4 113.398 3 400.5 3.834 EQUIVALENTS OF WEIGHTS AND MEASURES. 469 EQUIVALENTS OF WEIGHTS AND MEASURES.—Continued. Weights, Customaey. Metric Weight and Measure. Gm] [Co. Measuees, Customaey. Grains. oz. Troy. grains. lbs. Avoirdupois Fluid | ounces, minims. Fluid- ounces and fractions. OZ. grains. 1543.2 3 103.2 3 230.7 100 3 183.1 3.381 1440 3 3 127.5 93.310 3 74.5 3.155 1388.9 2 428.9 3 76.4 90 3 20.8 3.043 1369.2 2 409.2 3 56.7 88.721 3 3 1312.5 2 352.5 3 85.049 2 420.4 2.876 1234.6 2 274.6 2 359.6 80 2 338.5 2.705 1157.4 2 197.4 2 282.4 75 2 257.3 2.536 1080.3 2 120.3 2 205.3 70 2 176.1 2.367 960 2 2 85 62.207 2 49.7 2.103 925.9 1. 445.9 2 50.9 60 2 13.8 2.029 912.8 1 432.8 2 37.8 59.147 2 2 875 1 395 2 59.699 1 440.3 1.917 771.6 1 291.6 1 334.1 50 1 331.5 1.691 617.3 1 137.3 1 179.8 40 1 169.2 1.353 480 1 1 42.5 31.1035 1 24.8 1.052 463 1 25.4 30 1 6.9 1.014 456.392 1 18.89 29.574 1 1 437.5 1 28.350 460.1307 0.959 385.8 ... 25 405.8 0.845 308.6 20 324.61 0.676 154.3 10 162.31 0.338 15.4324 1 16.23 0.034 1 0.06479 1.0517 0.0022 0.9508 ... 0.06161 1 0.0021 470 HANDBOOK OF PHARMACY. EQUIVALENTS OF WEIGHTS AND MEASURES.—Continued. From 1 Troy Ounce down. Grains. Metric Weight and Measure. Gm.] [Cc. Minims (of Water at 4° C.). Grains. Metric Weight and Measure. Gm.] [Cc. Minims (of Water at 4° C.). 480 [1 5 31.103 504.8 240 [4 3 15.551 252.4 478.4 31 503.1 231.5 15 243.4 475.4 30.805 500 228.2 14.786 240 463.0 30 486.9 218.75 [lav. 14.175 230.1 456.4 29.573 480 216.1 oz’ 14 227.2 450 29.159 473.3 210 13.607 220.9 447.5 29 470.7 200.6 13 211 437.5 28.350 460.1 199.7 12.938 210 432.1 427.9 oz. 28 27.724 454.4 450 185.2 12 194.8 420 n s 27.214 441.7 180 [3 3 11.663 189.3 416.7 27 438.2 171.1 11.090 180 401.2 26 422 169.8 11 178.5 399.3 25.876 420 154.3 10 162.3 390 25.271 410.2 150 9.719 157.8 385.8 25 405.7 142.6 9.241 150 380.3 24.644 400 138.9 9 146.1 370.8 370.4 24.028 24 390 389.5 123.5 8 129.8 360 [6 3 23.327 378.6 120 [2 3 7.775 126.2 354.9 23 373.3 114.1 7.393 120 342.3 22.180 360 109.37 |-|av. 7.088 115.9 339.5 22 357.1 108.0 oz- 7 113.6 330 21.383 347.1 100 6.480 105.2 324.1 21 340.8 95.1 6.161 100 313.8 20.331 330 92.6 6 97.4 308.6 20 324.6 80 77.2 76.1 61.7 5.184 5 4.928 4 84.1 81.1 80 64.9 300 [5 3 19.440 315.5 60 [1 3 3.888 63.1 293.2 19 308.4 57.0 3.696 60 285.2 18.483 300 54.69 av. 3.544 57.5 277.8 18 292.1 47.5 oz- 3.080 50 270 17.495 284.0 50 3.240 52.6 262.3 17 275.9 46.3 3 48.7 256.7 16.635 270 42.8 2.772 45 246.9 16 259.7 40 38.0 33.3 30.9 2.592 2.464 2.156 2 42.1 40 35 32.5 471 EQUIVALENTS OF WEIGHTS AND MEASURES. EQUIVALENTS OF WEIGHTS AND MEASURES.—Continued. Continuation of Table of Equiva- lents from 1 Troy Ounce down. Equivalents of Weights from 5 Grains down. Grains. Metric Weight and Measure. Gm.] [Cc. Minims (of Water at 4° C.). Grammes. Grains in decimal fractions. in common fractions (approximate) 30 [J 3 1.944 31.6 0.324 5 5 28.5 1.848 30 0.291 4.5 4i 23.8 1.540 25 0.259 4 4 20 1.296 21.0 0.226 3.5 34 19.0 1.232 20 0.194 3 3 15.4324 1 16.23 0.162 2.5 24 0.130 2 2 0.097 1.5 14 15 0.972 15.9 0.065 1 1 14.3 0.924 15 14 0.907 14.7 13.3 0.862 14 0.061 0.94 H 13 0.842 13.7 0.060 0.93 12.4 0.801 13 0.057 0.88 12 0.775 12.6 0.053 0.82 11.4 0.739 12 0.050 0.77 11 0.713 11.6 0.049 0.76 % 10.5 0.678 11 0.045 0.69 H 0.040 0.62 0.036 0.56 A 10 0.648 10.5 0.032 0.5 V 9.5 0.616 10 9 0.583 9.5 8.6 0.554 9 0.028 0.43 TF 8 0.518 8.4 0.025 0.39 7.7 0.5 8.1 0.024 0.37 ■1 7.6 0.493 8 0.020 0.31 f¥ 7 0.454 7.4 0.016 0.24 X 6.7 0.431 7 0.012 0.18 A 6 0.389 6.3 0.008 0.12 % 5.7 0.370 6 0.004 0.06 A 0.0032 0.05 1 T7T 0.0027 0.04 To 5 0.324 5.3 0.0022 0.033 TO 4.8 0.308 5 0.0018 0.028 A 4 0.259 4.2 0.0016 0.025 A 3.8 0.246 4 0.0013 0.02 A 3 0.194 3.2 0.0011 0.017 TT 2.9 0.185 3 0.001 0.015 TT 2 0.130 2.1 0.0006 0.01 TTT 1.9 0.123 2 0.0005 0.008 TTK 1 0.065 1.0517 0.0004 0.0065 0.9508 0.06161 1 0.0003 0.005 Af 0.0002 0.003 FFF 0.0001 0.0015 FTF EQUIVALENTS OF MEASURES OF LENGTH. Centi- meters. Inches. Centi- meters. Inches. Milli- meters. Inches in decimal fractions. in 32ds. 150 59.06 55 21.65 25.4 1. tt 145 57.09 53.3 21 25 0.98 140 55.12 50.8 20 24 0.94 139.7 55 50 19.69 23.8 0.94 it 135 53.15 48.3 19 23 0.90 H 130 51.18 45.7 18 22.2 0.87 H 127.0 50 45 17.72 22 0.87 125 49.21 43.2 17 21 0.83 120 47.24 40.6 16 20.6 0.81 H 115 45.28 40 15.75 20 | 0.79 114.3 45 38.1 15 19.1 0.75 110 43.31 35.6 14 19 0.75 105 41.34 35 13.78 18 0.71 101.6 40 33.0 13 17.5 0.69 ft 100 39.37 30.5 12 17 0.67 99.0 39 30 11.81 16 0.63 96.5 38 27.9 11 15.9 0.62 H 95 37.40 25.4 10 15 0.59 93.9 37 25 9.84 14.3 0.56 ii 91.4 36 22.9 9 14 0.55 90 35.43 20.3 8 13 0.51 88.9 35 20 7.87 12.7 0.50 86.4 34 17.8 7 12 0.47 85 33.46 15.2 6 11.1 0.44 H 83.8 33 15 5.91 11 0.43 81.3 32 12.7 5 10 0.39 80 31.50 10.2 4 9.5 0.37 78.7 31 10 3.94 9 0.35 ... 76.2 30 9 3.54 8.7 0.34 75 29.53 8 3.15 8 0.31 73.6 29 7.6 3 7.9 0.31 71.1 28 7 2.76 7.1 0.28 9 70 27.56 6 2.36 7 0.28 68.6 27 5.1 2 6.4 0.25 A 66.0 26 5 1.97 6 0.24 65 25.59 4 1.57 5.6 0.22 63.5 25 3 1.18 5 0.20 61.0 24 2.54 1 4.8 0.19 6 60 23.62 2 0.78 4 0.16 58.4 23 1 0.39 3.2 0.13 55.9 22 3 0.12 2.4 0.09 A 2 0.08 1.6 0.06 •A 1 0.04 0.8 0.03 if 0.1 0.0039 ... Customary and Metric. 472 INDEX. A. Abbreviations, metric, 17 misleading, 378 used in prescriptions, 380 Abstracta, 349 Abstracts, 349 Acetic acid, titration of, 428 Aceta, 248 Acicular, 146 Acetum plumbicum, 236 saturninum, 236 Acid, acetic, titration of, 428 arsenous, assay of, 239,433 carbolic, estimation of, 444 citric, titration of, 428 hydrochloric, normal, 420 hydrocyanic, assay of, 431, 432 hypophosphorous, estima- tion of, 443 oxalic, decinormal, 421 oxalic, normal, 420 phosphoric, titration of, 428 sulphuric, normal, 420, 422 sulphurous, assay of, 433 tartaric, titration of, 428 Acids, Altering, 178 solvent properties, 129 volumetric estimation, 427 Acidimetry, 427 Adapters, 88, 91, 92 Agents, emulsifying, 297 Air bath, 84 Air, effect of exposure of chemi- cals, 154 Alcohol, contraction of, when mixed with water, 133 minims to fluidrachm, 13 solvent properties, 129 Alkali carbonates, assay of, 424 hydrates, assay of, 421 Alkalies, organic salts, assay of, 424 Alkalimetry, 422 Alligation, 139, 140 Alums, crystallizing, 146 Amorphous, 143 Amorphous precipitates, 157,158 Analysis, volumetric, 413 Angle of crystal, 143 Animal charcoal, use of, 180 Apothecary, 1 Apothecaries’ measure, 12 weight, 10 Apparatus, Currier’s extrac- tion, 208 for generating gases, 131 for upward filtration, 178, 179 Lewin’s extraction, 207 percolating, 193, 196, 199 siphon, 163, 188 Soxhlet’s extraction, 291 Approximate measures, 14 Aqua ammoniae, 222 ammoniae fortior. 222 amygdalae amarie, 221 amygdalarum amararum, 221 chlori, 223 chloroformi, 222 Aqua creosoti, 222 destillatie, 217 explanatory text, 221 preservation of, 220 hydrogenii dioxidi, 224 laurocerasi, 222 phimbica, 237 saturnina, 237 Aquae, 217 medicatee, 217 table of, 225,226 preservation erf, 220 Araeometer, 40-44 weighing, 41 Arsenous oxide, assay of, 239, 433 Assay, alkali carbonates, 424 alkali hydrates, 421 aqua ammonia, 223 aqua calcis, 422 aqua chlori, 223 arsenous oxide, 239, 433 extract nux vomica, 346 ferri carbonas saccharatus, 438, 443 ferric salts, 435 ferrous carbonate, 443 ferrous salts,437, 442 ferrous sulphate, 438, 442 Fowler’s Solution, 239 hydrocyanic acid, 431, 432 hydrogen dioxide, 442 hypopliosphites, 443 hypophosphorous acid, 443 hyposulphites, 433, 439 iodine, 435 Labarraque’s Solution, 241, 435 liquor ferri chloridi, 231, 436 liquor plumbi subacetatis, 236 Lugol’s Solution, 235 metallic iron, 437, 443 organic salts of alkalies, 424 phenol, 445 potassii bitart ras, 425 potassii et sodii tartras, 425 potassium cyanide, 432 potassium iodide, 439 soda, 240 sodii benzoas, 426 solution of ferric acetate, 229 solution of ferric citrate, 232 solution of hydrogen per- oxide, 225 solution of potassa, 238 solution tersulphate of iron, 234 spirit of nitrous ether, 253 sulphites, 433 sulphurous acid, 433 syrupus acidi hydriodici, 278 syrupus ferri iodidi, 281 thiosulphates, 433 tincture of iodine, 263 tincture of iron, 262 tincture opium, 263 Asymmetric system. 146 Atomic weights, table of, 447 Attenuations, homoeopathic,388 Automatic washing of precip- itates, 165 Auxiliary, the, 376 Avoirdupois, term, 10 weight, 10 Axes, crystallographic, 143-146 B. Bacilli, 316 Bag, straining, 168 Balance, analytical, 23 arms of, 22 army, 25 beam of, 22 care of, 24 counter, 25 delicacy of, 23 dispensing, 23, 26, 29 hydrostatic, 35 loading, 24 maxims for handling, 34 prescription, 23 the, 21 torsion, 29 for weighing solutions, 27 Balances, proscription, 23, 28, 29 Balsam Peru, emulsion of, 301 Barium sulphate, solubility, 128 Barthel’s lamp, 53 Basham’s Mixture, 233 Basis, the, 376 Bath, air, 84 oil, 83 sand, 82, 83 Baths, 81-84 saline, 83 water, 81, 82 Baurad degrees, table of, 43 hydrometers, 43 Beads, Lovi’s specific gravity, 48 Beaker glasses, 159 Beam, triple graduated, 29 Beck’s still, 99 Black wash, 228 Blackmann’s suppository mould, 367 Blast lamp, 57 Blowpipe, 67 flame, 68 Blue mass, 313 Bodies, explosive, 390 Boiling, 62 point, 62 at different pressures, 74 Bolus, 318 Bottle, specific gravity,38, 39, 40 spritz, 165 wash, 165 weighing, 134 Bougie press, 370 Bougies, 370 cacao-butter, 370 gelatin, 370 Bromine, estimation of, 435 volumetric solution deci- normal, 445 Bumping, 97 Bunsen burners, 54, 55 473 474 INDEX. Bunsen flame, 55 sectional view, 66 Burettes, 415 Burner, Erlenmeyer’s, 55 solid flame heating, 56 C. Cachet wetter, 306 Cachets, 305 sealing and filling, 306 Calcination, 70 Caloric, 52 Camphor, emulsion of, 300 Capillary tubes for melting- point determination, 64 Capsule filler, Acme, 309 Davenport’s, 308 Haymond’s, 309 moulds, 307 Capsules, gelatin, 307 suppository, 371 Carbonization, 70 Casein emulsion, 299 preparation of, 299 Celsius’ thermometer, 58, 59 Centigrade thermometer, 58,59 Centigramme, 17 Centiliter, 17 Centinormal potassium hy- drate V. S.,429 volumetric solutions, 413, 429 Centimeter, 17 Centrifugal machine, 213 uses of, 213, 215 Centrifuge, 213 uses of, 213, 215 Cerata, 357 Cerates, 357 preservation, 357 table of, 357 Chambers draught, 80 Charcoal, aluminized, 186 animal, use of, 186 Charta potassii nitratis, 362 sinapis, 362 Chart®, 362 Chemicals, effects of exposure on,155 Chemists’ cover, 176 Chlorine, estimation of, 435 water, preparation of, 132 Chloroform, minims to fluid- rachm, 13 solvent properties, 129 Circulatory displacement, 131 solution, 130 Citric acid, titration of, 428 Clarification, 184 by albumen, 184 by alcohol, 185 by fermentation, 185 by gelatin, 184 by heat, 184 by insoluble bodies, 184 Classification of pharmaceutical preparations, 216 Closet, drying, 109 Coating pills, 326 Coefficient. 130 Colation, 168 Collodia, 292 Collodions, 292 table of, 292 Colloids, 141 Column apparatus, 96, 97 Combustion, 52 Comminution, 115 Compressed suppositories, 368 tablets, 335 tablet moulds, 339 Condenser, air, 89 inverted, 94 Liebig’s, 88 Mitscherlich’s, 102 Condenser, reflux, 94 spherical, 94 worm, 88 Condensers, 85, 87, 88, 89 Cone, perforated platinum, 182 Confectio rosie, 312 senna?, 312 Confectiones, 312 Confections, 312 Congealing point of fats and waxes, 65, 66 Conserve, 312 Constitution, water of, 151 Construction, grammatical, 376 Continuous filtration, 166,178 Contusion. 116 Cork borer, 92, 93 file, 93 presses, 94 Corrective, the, 376 Counter balance, 25 Cover, chemist’s, 176 Crucibles, 68 Crystalline, 143 fracture, 143 Crystallizable, 143 Crystallization, 143 by chemical interaction, 149 by cooling of fused masses, "147 by cooling of vapors, 147 by spontaneous evapora- tion, 147 conditions of, 147 effect of solvent on, 151 fractional, 149 from hot solutions, 147, 148 intermediate, 149 through deposition, 147 water of, 151 Crystalline precipitates, 157 Crystallizing, 143 proper precautions in, 147- 148 vessel, 150 Crystallographic axes, 143-146 Crystallography, systems of, 143-146 Crystalloids, 141 Crystals, 143 ' draining, 150 growing, 149 Cubic centimeter, drops to, 13 Cubic decimeter, 8 Cubic inch of water, weight, 8,10 Curdy precipitates, 157 Curran’s still, 101 Currier’s extraction appara- tus, 208 Curtman’s still, 98 Cutting tubing, 89, 90 Cylinders, measuring, 415 D. Decantation, 161 Decigramme, 17 Deciliter, 17 Decimeter, 17 Decimal system, 15 Decocta, 247 Decoction, 189 Decoctions, 247 table of, 247 Decoloration, 186 Decant ing on filter, 175 Decantation with siphon, 163 with washing, 161 Decinormal bromine V. S., 443 iodine V. S., 432 oxalic acid V. S., 421 potassium dichromate V.S., 436 Decinormal potassium perman- ganate V. S.,439 silver nitrate V. S., 429 sodium hyposulphite V. S., 434 volumetric solutions, 413, 429 Decrepitation, 151 Definition, pharmacopoeia!, 5 Deflagration, 70 Dekagramme, 17 Dekaliter, 17 Dekameter, 17 Deliquescence, 154 Deliquescent salts, 154 Dense precipitates, 157, 158 Densimeter, Rousseau’s, 42 Density, 34 of solutions, 133 Description, pharmacopoeial, 5 Desiccation, 71, 108, 114 Desiccator, Hempel’s, 112 vacuum, 112 Desiccators, 111, 112 Dessertspoonful, 14 Destructive distillation, 97 Determination of boiling point, 62 of melting point, 63 of solubility, 134-136 of specific gravity, 34 of specific volume, 49 Diagram, metric, 18 Dialysates, 142 Dialysed iron, 142 Dialyser, 141, 142 Dialysis, 141 Diffusate, 141 Diffusion, 141 Digestion, 189 Dilution, rules for, 138-140 Dimetric system, 144 Dimorphous, 146 Disc, perforated porcelain, 182 Dispensatory, 1 Dispensing,"homoeopathic, 388 the art of, 375 general instructions, 397 Displacement, 191 circulatory, 131 Distillation, 71, 85-104 with current of steam, 95 destructive, 97 under diminished pressure, 76 fractional, 95 Doses, 379 Double normal volumetric so- lutions, 413 Drachm, 10 Draining crystals, 150 Draught chambers, 80 Drop, 13 Dropping fluids, methods of, 13, 14 Drops in fluidrachm, 15 Drug, degree of fineness for percolating, 196 Drug-mill, Enterprise, 116 Hance’s, 117,118 Drug-mills, handling of, 118 Drugs,storage and preservation, 110 Drying closet, 109 drugs, 108, 109, 110 gases, 113 liquids, 112 loss of drugs in, 108,109 ovens, 110, 111 E. Edel’s still, 99,100 Edge, of crystal, 143 Efflorescence, 154 INDEX. 475 Efflorescent salts, 154 Elaeometer, 44 Elieosacchara, 311 Electuary, 312 Elixiria, 285 Elixirs, 285 Elixir phosphori, 285 Elutriation, 126 Emplastra, 358 table of, 361 Emplastrum plumbi, 361 Emulsa, 295 table of, 302 Emulsification of special drugs, 300 Emulsifying agents, 297 Emulsion, casein, 299 extract of malt, 299 gelatin, 300 Irish moss, 298 pancreatin, 300 quillaja bark, 299 tragacanth,297 yolk of egg, 298 Emulsiones, 295 Emulsions, 295 artificial, 295 continental method, 296 English method, 296 gum-resin, 295 natural, 295 notes on, 301 oil, 295 seed, 295 Enterprise drug-mill, 117 press, 212 Equivalents of Imperial in U. S. fluid measure, 12 metric and U. S., 18, 19 Erdmann float, 418 Estimation of alkali hydrates, 421 Ether, nitrous, spirit, 251 solvent properties, 129 Evaporating flame, 76 inflammable liquids, 79 kettle, 82 vessels, 75, 76 Evaporation, 71-84 conditions governing, 71 rapidity of, 71 rapid, 78, 79 spontaneous, 80 Evaporator, cascade, 73 Hempel’s, 79 Excipients, pill, 322-324 Exercise, alkali hydrates, assay, 421 ammonium acetate, 227 aqua ammonite fortior, assay, 223 aqua ealcis, assay, 422 assaying extract nux vom- ica, 347 bromides, assay, 435 chlorides, assay, 435 oleates, 289 liquor ferri acetatis, 229 chloridi, 231 citratis, 233 tersulphatis, 234 plumbi subacetatis, 236 potassie, 238 potassii arsenitis, 239 citratis, 240 sodie ehloratie, 242 zinei chloridi, 243 spiritus letheris nitrosi, 254 standardizing extract nux vomica, 344 syrupus acidi hydriodici, 279 syrupus ferri iodidi, 282 Exercises in alligation, 139, 140 Exercises in dilution and forti- fication, 138, 140 in solubility, 136 in specific gravity, 36, 37, 38, 50 in specific volume, 50 volumetric solutions, 419 Exhaustion of drug, 199 Explosive bodies, 390 mixtures, 390 prescriptions, 392 Expression, 210 Exsiccation, 71,153 Extracta, 341 causes of precipitation in, 273 fluida, 269 menstruum, 269 preservation of, 273 valuation of, 274 Extract, Goulard’s, 236 malt, emulsion, 299 mix vomica, 344 nux vomica, assay, 346 Extraction, 189 apparatus, 291, 207, 208 hot, 207 with hot solvents, 207 Extracts, 341 explanatory text, 344 physical characters, 343 preservation of, 343 table of, 343,344 yield of, 341 Extractum nucis vomicie, 344 nucis vomicie, assay, 346 F. Faces of crystal, 143 Fahrenheit’s thermometer, 58, 59 Fairbank’s druggists’ scale, 27 Fats, determination of melting and congealing point, 65, 66 specific gravity, 48, 49 Ferri carbonas saccharatus, estimation, 438, 443 Ferrous carbonate, estimation of, 443 sulphate, estimation of, 438, 442 Filter, folded, 172 paper, 170 hardened, 171 toughened, 171 plain, 171 plaited, 172 Squibb’s, 179 Filtering apparatus, automatic, 166 caustic fluids, 178 cone, 179 dense liquids, 179 maxims, 174 plates, 182 stands, 175 Filtrate, 170 Filtration, 170, 178 continuous, 166, 178 hot, 179 large quantities of fluids, 178,179 pressure, 180 rapid, 180 upward, 178 Flame, 52 blowpipe, 68 Bunsen, 55, 67 Flask, separating, 187 Spritz, 165 suction for rapid filtration, 182 wash, 165 Flasks, measuring, 415 Float, Erdmann’s, 418 Flocculent precipitates, 157 Fluids, filtering large quanti- ties, 179 Fluid extract, cinchona, 271 extracts, 269 causes of precipitation in, 273 menstruum, 269 preservation of, 273 valuation of, 274 Fluidounce, Imperial, 11, 12 U. S., 12 Fluid pint, 12 Imperial, 11 Fluidrachm, 12 drops in, 15 Imperial, 12 minims to, 13 Folded filter, 172 Foreign prescriptions, 383 Formula, symbolic, 4 Fortification, rules for, 138-140 Fowler’s Solution, 238 Fractional crystallization, 149 distillation, 95, 96 percolation, 270 precipitation, 159 Fractionat ing apparatus, 63 flask, 83, 86 Fracture, crystalline, 143 Frame, strainer, 168 Freezing mixtures, 133 Fuels, valuation of, 52, 53 Fulcrum, 21, 22 Funnel, coil jacket, 180 cover, 176 Dieterich’s, 180 fluted, 177 parts of, 176 proper shape, 177 ribbed, 177 steam coil jacket, 180 Funnels, 176 separating, 187 jacketed, 180 various kinds, 176,177 Fusion, 69 G. Gallon, ale, 11 corn,11 Imperial, 11, 12 wine, 10, 12 wine measure, 12 Gas stoves, 56 Gases, drying, 113 generating, 131 solubility of, 132 solution of, 131, 132 washing, 113, 114 Gay-Lussac's automatic filter- ing apparatus, 166 Gelatin capsules, 307 empty, 308 emulsion, 300 hard, 307 soft, 307, 308 suppository capsules, 371 Gelatinous precipitates, 157 Glass, soluble, 242 Glycerin, solvent properties, 129 suppositories, 364, 373 Glycerita, 286 table of, 286 Gorham’s dispensing balance, 26 Goulard’s extract, 236 Graduates, 32, 33 testing accuracy of, 33 Grain, 8, 9, 10, 11 origin of, 10 Gramme, 16, 17 drops to, 13 476 INDEX. Granular effervescent salts, 152 precipitates, 157 Granulation, 152, 335 Granules, 318 Grinding, 116 Growing crystals, 149 Guiding-rod, 161 H. Hance’s, drug mill, 117,118 Hand scales, 24 Heat, 52 measurement, 57 Heater, water, 56 Hectogramme, 17 Hectoliter, 17 Hectometer, 17 Hexagonal system, 143, 144 Homoeopathic dispensing, 388 Honeys, 284 Hot extraction, 207 filtration, 179 Hunter’s filter and mixer, 120 Hydraulic press; 212 Hydrocyanic acid assay, 431,432 Hydrogen dioxide, estimation of, 442 Hydrometer, 40-44 Baume’s, 42, 43 Nicholson’s, 41 Sykes’, 43 Tralles’, 43 Twaddell’s, 43 weighing, 41 Hydrometers, scale, 41, 42 Hydrostatic balance, 35 press, 212 Hypodermic injections, 226 Hypophosphites, estimation of, 443 Hypophosphorous acid, estima- tion of, 443 Hyposulphites, assay of, 433 I. Ignition, 69 Imperial fluidounce, 11 gallon, 11, 12 measure, 12 minim, 12 ounce, 12 pint, 11 pound, 11 standards, 10 system, 11, 12 Incompatibility, 394 chemical, 394 in prescriptions, 404 mechanical, 396 pharmaceutical, 396 in prescriptions, 402 prescription, general con- sideration of, 397 therapeutic, 397 Incompatibles, 394 acacia, 394 alkalies, 394 alkaloids, 394, 396 antipyrin, 394 aqu® ammoni®, 222 aqua chlori, 223 arsenous acid, 394 bismuth, 394 bromides, 394 calomel, 395 chloral, 395 chlorates, 391 chlorides, 395 chlorine water, 395 corrosive sublimate, 395 Donovan’s solution, 228 emulsions, 301 hydrogen peroxide, 395 Incompatibles, iodides, 395 iodine, 395 iron, reduced, 395 iron salts, 395 lead acetate, 395 lead subacetate, 395 lime water, 395 liquor fern chloridi, 231 liquor iodi comp., 235 liquor plumbi subaceta- tis, 236 liquor potass®, 238 liquor potassii arsenitis, 238 liquor sod® chlorat®, 241 pepsin, 395 potassium permanganate, 392-396 quinine salts, 396 salicylic acid, 396 silver nitrate, 396 strychnine, 396 syrupus acidi hydriodici, 278 syrupus ferri iodidi, 281 tannin, 396 tartar emetic, 396 tinctura ferri chloridi, 262 Indicator, 414 Indicators, 414 Infusa, 244 Infusion, 188 mugs, 245 Infusions, 244 from fluid extracts, 245 preservation, 245 table of, 246 Injectiones hypodermic®, 226 Injections, hypodermic, 226 Inscription, the, 375, 376 Insolubility, 128 Intermediate crystallization, 149 Interstitial water, 151 Iodine, assay of, 435 decinormal solution, 432 Irish moss emulsion, 298 Iron dialysed, 142 ferric, estimation of, 435 ferrous, estimation of, 437, 442 metallic, estimation of, 437, 443 Isometric system, 144 Isomorphous, 146 J. Jacketed funnels, 180 Jar, receiving, 196 Joints, fitting, 90 Jolly’s specific gravity balance, 47 Juices, 262 K. Karat, 8 Keratin coating, pills, 329, 330 Keratin, preparation of, 330 Kilogramme, 8, 17 standard, 16 Kiloliter, 17 Kilometer, 17 Koppeschaar’s Solution, 443 L. Labarraque’s Solution, 241 Lactometer, 44 Lamp, alcohol, 52 blast, 57 Latin, valueof, in pharmacy, 3, 375 Lead plaster, 361 water, 237 Length, units of, 6 Levigation, 125 Lewin’s extraction apparatus, 207 Liebig’s condenser, 88 Light, action of, on chemicals, 154 precipitates, 157, 158 Lime water, 228 Linimenta, 293 Liniments, 293 table of, 293 Liquid, supernatant, 156 Liquids, alcoholic, minims to fluidrachm, 13 caustic, filtering, 178 drying, 112 ethereal, minims to the fluidrachm, 13 immiscible, separation of, 187 specific gravity of, 38 weighing, 24 Liquor acidi arsenosi, 227 ammonii acetatis, 227 arseui chloridi, 227 arseniet hydrargyri iodidi, 227 calcis, 228 calcis saccharatus, 280 ferri acetatis, 228 chloridi, 230 citratis, 231 et ammonii acetatis, 233 nitratis, 233 perchloridi, 230 sesquichloridi, 230 subsulphatis, 233 tersulphatis, 234 hydrargyri nitratis, 234 iodi compositus, 235 magnesii citratis, 235 plumbi subacetatis, 236 subacetatis dilutus, 237 potass®, 237 potassii arsenitis, 238 citratis, 240 sod®, 240 chlorat®, 241 sodii arsenitis, 242 silicatis, 242 trinitrini, 255 zinci chloridi, 242 Liquores, 227 Liter, 17 standard, 16 Lixiviation, 190 Lotio flava, 228 nigra, 228 Lovi’s specific gravity beads, 48 Lozenge-cutter, 316 board, 315 Lozenges, 314 Lugol’s Solution, 235 Lupulin, emulsion of, 301 Lycopodium, emulsion of, 301 Lysimeter, tne, 135, 136 M. Maceration, 189 Machine, centrifugal, 213 uses of, 213, 215 Magma, 157 Magnesia, heavy, 158 light, 158 Mass, 6 blue, 313 Vallet’s, 313 Massa copaib®, 312 ferri carbonatis, 313 hydrargyri, 313 INDEX. 477 Massse, 312 Masses, 312 Massing inorganic salts, 324 organic salts, 325 Maxims, in filtering, 174 Measure, cubic centimeter, 33 Imperial, 12 U. 8. liquid, 12 wine, 12 Measures, 32, 33 approximate, 14 equivalents of, table, 466 minim, 33 Measuring cylinders, 415 flasks, 415 Mediation, pulverization by, 119 Medicated papers, 362 pencils, 371 waters, 217 explanatory text, 221 preservation, 220 wines, 256 table of, 257 Mel despumatum, 284 Mell it a, 284 Melting point, 63 determination, appara- tus, 65, 66 of fats and waxes, 65, 66 Meniscus, 417 Menstruum, 190, 198 Meter, 7, 16, 17 Meter, standard, 16 Metric abbreviations, 17 diagram, 18 measures of capacity, 17 of length, 17 prefixes, 17 prescriptions, 385 system, 15 units, equivalents of, 18, 19 weights, 17 Micromillimeter, 17 Mill, drug, Enterprise, 116 Hance’s, 117, 118 Milligramme, 17 Milliliter, 17 Millimeter, 17 Mills, drug, 116, 119 handling of, 118 Mina, Greek, 8 Minim, 12, 13 Imperial, 12 Misturse, 294 Mitscherlich’s condenser, 102 Mixture, Basham’s, 233 Mixtures, 294 explosive, 390 freezing, 133 table of, 294 Mohr’s cork borer, 93 specific gravity balance, 46 Moistening and packing, 197 Molecular weights, table of, 455 Monoclinic system, 145 Monometric system, 144 Monosymmetric system, 145 Monsei’s Solution, 233 Mortar, levigating, 125 Mortars, 121, 123 agate, 123 cleansing, 123 glass, 122 iron, 122 porcelain, 122, 123 wedgwood, 122, 123 Mother-liquor, 148 Mould, tablet triturate, 331 Moulds, compressed tablet, 339 Mucilages, 248 table of, 248 Muller, 125 N. Nitrometer, 253 Nomenclature, pharmacopceial, 3, 4, 5 Normal hydrochloric acid, 426 oxalic acid, 420 potassium hydrate, 426 sulphuric acid, 422 volumetric solutions, 413 Nux vomica, pulverization of, 120 O. Oblique system, 145 Oil bath, 83 Oils, filtration of, 178, 179 fixed, minims to fluid- rachm, 13 volatile, minims to fluid- rachm, 13 solvent properties, 129 Ointment bases, 352 citrine, 355 mercurial, 355 mercury, nitrate, 355 pad, 353 spatula, 353 Ointments, 352 dispensing, 354 explanatory text, 355 incorporation of various substances, 353 masking odor of, 354 methods of preparation, 352 preservation, 354 table of, 354 Oleata, 287 Oleates, 287 dry, 287 Oleopalmitates, 288 Oleoresime, 290 Oleoresins, 290 table of, 291 Oleosacchara, 311 Oleosaccharates, 311 Orthorhombic system, 144 Ounce, 8, 9, 10,13 apothecaries’, 10 avoirdupois, 10 fluid, Imperial, 13 U. 8., 12, 13 Imperial, 12 Troy, 10 Ounces, various, 10, 13 Ovens, drying, 110, 111 Ovoids, 316 Oxymellita, 284 P. Packing and moistening, 197 Pancreatin emulsion, 300 Paper, filter, 170 Paper, mustard, 362 Usego, 306 Papers, medicated, 362 Pastilli, 314 Pellicle, 148 Pencils, medicated, 371 Pennyweight, 8, 9 Percentage solutions, 137 tables, 138 Percolate, 191 Percolation, 191 apparatus for, 193, 196, 199 fractional, 270 history of, 191 in vacuo, 273 menstruum for, 198 official, 192, 196 pressure, 204 vacuum, 206 versus maceration, 190 Percolation with expression, 272 with hot solvent, 207 Percolator .Christ- Dieterich ,200 conical, 193, 194 cylindrical, 193, 194 for volatile solvents, 290 packing, 194, 195 pressure, Lentz’s, 205 Real’s, 191 shape of, 194 Squibbs’ siphon, 201-203 well-tube, 201-203 with air-pump, 206 Percolators, 193, 199, 200, 201, 203 dimensions of, 194 pressure, 204 Perfection suppository ma- chine, 369 Pestles, 121-123 Pharmaceutical incompatibili- ty, 396 Pharmaceutical stills, 98 Pharmacopoeia, 1 Pharmacopoeia! Latin, 3 nomenclature, 3, 4, 5 Pharmacopoeias, 2, 3 history of, 1 table of, 2 Pharmacy, 1 Phenol, estimation of, 445 Phosphoric acid, titration of, 428 Pill, blue, 313 coater, Maynard’s, 329 Patch’s, 329 excipients, 322, 323, 324 finishers, 322 machine, 321 mortar, 320 pestle, 320 press, 321 roller, 320 rolling, 320 rounders, 322 silverer, 327 spatula, 320 tiles, 320 Pills, 318 coating, 326 gelatin coating, 328 general observations on making, 318, 319 gilding, 327 inorganic salts, 324 keratin coating, 329, 330 organic salts, 325 organic substances, 325 pearl coating, 328 salol coating, 329, 330 silvering, 327 sugar-coating, 327 varnishing, 327 Pihite, 318 Pinch-cocks, 89, 90 Pint, Imperial, 11 U. 8., 12 Pipette, 33, 164 capillary, 188 Pipettes, 164, 188 Plain filters, 171 Plaited filter, 172 Planes, of crystal, 143 Plaster block, 359 forms, 359 iron, 359 lead, 361 perforator, 360 press, 321 spatula, 358 Plasters, 358 explanatory text, 361 perforation of, 360 spreading, 358 table of, 361 478 INDEX. Plates, porous, for filtering,182 Polymorphous, 146 Porphyrizatiou, 125 Potassii bitartras, assay of, 425 et sodii tartras, assay of, 425 Potassium cyanide, assay of, 432 dichromate, volumetric so- lution, decinormal, 436 hydrate, volumetric solu- tion, centinormal., 429 hydrate, volumetric solu- tion, normal, 426 iodide, assay of, 439 permanganate, volumetric solution, decinormal, 439 Pound, ancient and modern standards, 9 apothecaries’, 8, 10 avoirdupois. 10 British standard, 8 commercial, 8 Imperial, 11 monetary, 8 Saxon, 8 Troy, 9, 10, 11 Powder dividers, 304 folders, 305 moistening of, 195 Powders, 303 degrees of fineness, 121 dividing, 304 external use, 303 folding, 304 granulating, 335 internal use, 303 liquefying, 303 percolating, 192, 195,196 specific gravity of, 36 triturating, 303 weighing, 24 Precipitant, 156 Precipitate, 154-161 Precipitates, amorphous, 157, 158 continuous washing of, 165 crystalline, 157, 158 curdy, 157 dense, 157, 158 flocculent, 157 gelatinous, 157 granular, 157 light, 156-158 rinsing out, 164 washing, 164-165 Precipitating jar, 160 Precipitation, 156 causes of, 156 fractional, 159 from cold solution, 158 from hot solution, 158 objects of, 157 order of mixing the solu- tions, 158 Prentiss’ still, 99, 100 Preparations, galenical, classifi- cation of, 216 Prescription, Latin construc- tion of, 376 parts of, 375 phrases, foreign, 385 scales, 23, 28, 29 the, 375 Prescriptions, abbreviations used in, 380 explosive, 392 foreign, 383 German, 383 homoeopathic, 389 measures used in, 379 metric, 385 obsolete terms used in, 384 signs sometimes employed, 384 typical, 399 weights used in, 379 Press-cloth, 210 Press, cork, 94 differential-arm, 211 Enterprise screw, 212 hydraulic, 212 hydrostatic, 212 knee lever, 212 tincture, 211 Witts’ pharmaceutical, 211 Presses, screw, 210-212 Pressure filtration, 180 percolation, 204 pumps, 181 Prismatic, 146 system, 144 Pulveres, 303 table of, 310 Pulverization, 119 by mediation, 119 precautions in, 119 Pulverizing nux vomica, 120 works, Poulain’s, 115 zinc, 120 Pump-pressure, 181 water, 181 Pycnometer, 38, 39, 40 Squibb’s, 40 Pyramidal system, 144 Q. Quadratic system, 144 Quillaja bark emulsion, 299 Quinine oleate, 289 R. Rapid evaporation, 78, 79 filtration, 180 improvised apparatus, 183 Real's press percolator, 191 Rdaumur thermometer, 58, 59 Receiver, 88, 91 Receiving jar, 196 Recipe, 375 Recrystallization, 149 Rectification, 96 Regular system, 143, 144 Remington’s still, 100 Repercolation, 270 Resinas, 350 Resinoids, 350 table of, 351 Resins, 350 emulsion of, 300 table of, 350 Retort stand, 140 Retorts, 87, 97 with adapters, 92 Rhombic system, 144 Rhombohedric system, 144 Rice’s still, 102, 103 Rod-guiding, 161 Rousseau’s densimeter, 42 Rule, specific gravity, 35 specific volume, 49 Rules for converting thermo- metric degrees, 59 for dilution and fortifica- tion, 138-140 for fixing strength of ex- tract nux vomica, 346 S. Saccharometer, 44 Saline baths, 83 Salol coating for pills, 329, 330 emulsion of, 300 Salts, deliquescent, 154 efflorescent, 154 granular effervescent, 152 Sand bath, 82, 83 Saturated solution, 128 Scale, army, 25 Scale, vest-pocket, 27 salts, 149 Scales, analytical, 23 care of, 30 counter, 25, 26, 28, 29 hand, 24 prescription, 25 torsion, 29 Screw presses, 210-212 Scruple, 10 Sediment, 161 See’s suppository mould, 367 i Semi-normal volumetric solu- tions, 413 I Separating funnels, 187 Separation of immiscible liquids, 187 ' Separator, 187 , Sifter, Hunter’s, 120 , Sifting, 120 I Signature, the, 375, 380 Signs, apothecaries’ weight, 10 avoirdupois weight, 10 cabalistic, 384 liquid measure, 12 Troy weight, 9 Silver bromide, solubility, 128 nitrate volumetric solution, decinormal, 429 Siphon, 162 apparatus, 163, 188 percolator, 201-203 ! Slightly soluble, 128 Soaps, insoluble, 361 soluble, 361 Sodii benzoas, assay of, 426 Sodium hyposulphite, volu- metric solution, decinor- mal, 434 Solids, specific gravity, 35, 41 ! Soluble, “ slightly,” 128 “ very,” 128 ’ Solubilities, Attfield’s table of, 390 table of, 448 Solubility, 128 barium sulphate, 128 coefficient of, 130 conditions of, 128 of contact of body and solvent, 130 determination of, 134 effect of presence of dis- solved bodies, 130 effect of temperature on, 129 exercise in determination, 135 of gases, 132 of silver bromide, 128 table of curves, 130 Solution, 128 acetate of iron, 228 ammonium acetate, 227 arsenous acid, 227 Burnett’s disinfecting, 242 change in volume by, 133 of temperature bv, 133, 134 chlorinated soda, 241 circulatory, 130 citrate of iron, 231 direct, 128 Donovan’s, 227 ferric chloride, 230 ferric nitrate, 233 Fowler’s, 238 gases, 131, 132 iodide of arsenic and mer- cury, 227 iodine compound, 235 iron and ammonium ace- tate, 233 Koppeschaar’s, 443 Labarraque’s, 241 lime, 228 I Lugol’s, 235 INDEX. 479 Solution, magnesium citrate, 235 mercuric nitrate, 234 Monsel’s, 233 potassium citrate, 240 saturated, 128 simple, 128 sodium silicate, 242 sodium arsenate, 242 sodium hydrate, 240 subacetate of lead, 236 subacetate of lead,dilute,237 subsulphate of iron, 233 tersulphate of iron, 234 unsaturated,128 Valangin’s, 227 Volhard’s, 431 of zinc chloride, 242 Solutions, 227 aqueous, 217 aqueous, minims to flui- drachm, 13 balance for weighing, 27 density of, 133 homoeopathic, 388 percentage, 137 standard, 413 supersaturated, 131 table of, 243 volumetric, 413 Solvent, 128 effects of, on crystallization, 151 for crystallizing, 148 nature of, 129 Solvents, pharmaceutical, 129 used in pharmacy, 129 Soxhlet’s extraction apparatus, 291 Spatula, horn, 124 ointment, 124 pill, 124 plaster, 358 powder, 124 Spatulas, 124 Specific gravity, 34 balance (Jolly’s), 47 Mohr’s, 47 Westphals’, 45 beads, 48 bottle, 38-40 by displacement, 36 exercises, 36-38, 50 of fats, 48, 49 of liquids, 38 of powders, 36 separation of different bodies by means of, 36 of solids, 35-38 of solids (light), 37 of solids (soluble), 38 table, 51 tube, Sprengel’s, 47 by weighing volumes, 48 rule, 35 Specific volume, 49 exercises, 50 Spirit lamp, Barthel’s, 53 nitrous ether, 251 nitroglycerin, 255 Spirits, 250 explanatory text, 251 table of, 250, 251 Spiritus, 250 setheris nitrosi, 251 glonoini, 255 Mindereri, 227 Spontaneous evaporation, 80 Spreading plasters, 358 Sprengel’s specific gravity tube, Spritz bottle, 165 Squibb’s pycnometer, 40 siphon percolator, 201, 203 Squibb’s urinometer, 44 Stand, retort, 91 Stands, filtering, 175 Standard solutions, 413 volumetric solutions, pre- paration of, 419 Standards, ancient and mod- ern, 9 of Henry III, 8 Steatins, 357 Still, automatic, 101 Beck’s, 99 Curran’s, 101 Curtman’s, 98 Edel’s, 99, 100 Prentiss’, 90,100 Remington’s, 100 Rice's, 102, 103 Stills, laboratory, 98-104 pharmaceutical, 98 Stirring apparatus, 72 Storage of drugs, 110 Stoves, gas, 56 Strainers, 168 Straining, 168, 169, 178 bag, 168 frame, 168 Sublimation, 71, 105-107 Subscription, the, 375, 379 Succi, 262 Succussion, 355 Sulphites, assay of, 433 Supernatant liquid, 156 Supersaturated solutions, 131 Superscription, the, 375 Suppositoria, 363 Suppositories, 363 cacao butter, 364 compressed, 368 dispensing, 372 gelatin, 363 general remarks on, 372 glycerin, 364, 373 hand-rolled, 365 hollow cacao butter, 372 moulded, 365 various forms, 363 Suppository bases, 363 capsules, 371 machine, the Perfection,369 W.,T. & Co., 369 machines, 368, 369 mould, Blackmann’s, 367 See’s, 367 Suppository moulds.366,367,369 the Wellcome, 363 Sweet spirit of nitre, 251 Syke’s hydrometer, 43 Syllabus of tinctures, 267, 268 Synonym, the, 4 Syrup of almonds, 279 bulk resulting from solution in water, 275 ferrous iodide, 280 garlic, 279 hydriodic acid, 278 iodide of iron, 280 lime, 280 Syrupi, 275 Syrups, 275 classification of, 277 preparation of, 275 preservation of, 277 simple proportions for pre- paring, 274 table of, 283 Syrupus acidi hydriodici, 278 allii, 279 amygdalae, 279 calcis, 280 ferri iodidi, 280 System, asymmetric, 146 decimal, 15 dimetric, 144 hexagonal, 143, 144 isometric, 144 System, metric, 15 monoclinic, 145 monometric, 144 monosymmetric, 145 oblique, 145 orthorhombic, 144 prismatic, 144 pyramidal, 144 quadratic, 141 regular, 143, 144 rhombic, 144 rhombohedric, 144 tesseral, 144 tetragonal, 143, 144 triclinic, 146 trimetric, 144 Systems of crystallography, 143, 146 Tabellse, 314 Table of abbreviations, Latin, 380 atomic weights, 447 cabalistic signs, 384 cerates, 357 collodions, 292 curves of solubility, 130 decoctions, 247 degrees, Baume, 43 drops in fluidrachm, 15 emulsa, 302 extracts, 343, 344 foreign prescription phrases, 385 glycerites, 286 infusions, 246 liniments, 293 liquores, 243 loss in drying drugs, 108,109 medicated waters, 225 medicated wines, 256 mixtures, 294 molecular weights, 455 mucilages, 248 obsolete terms, 384 ointments, 354 ■ oleoresins, 291 percentage, 138 plasters, 361 powders, 310 resinoids, 351 resins, 350 solubilities, Attfleld’s, 390 solubilities, 448 specific gravities, 51 spirits, 250, 251 syrups, 283 thermometric equivalents, 461 tinctures, 259, 267-8 troches, 317 vinegars, 249 weights and measures, 20, 466 Tablet, compressed, moulds, 339 triturates, 331 Tablets, compressed, 335 Tablett®, 331, 335 Tablespoonful, 141 Tabular, 146 Talent, Greek, 8 Tartaric acid, titration of, Teacupful, 14 Teaspoonful, 14 Temperattire, change in, by solution, 133, 134 effect on solubility, 129 lowering of, by solution, 133 rise in, by solution, 134 Terms, foreign, in prescrip- tions, 385 Latin, used in prescrip- tions, 380 obselete, used in prescrip- tions, 384 480 INDEX. Tesseral system, 144 Test solution, Brazil wood, 414 cochineal, 414 litmus, 414 methyl-orange, 414 phenolphtalein, 414 potassium chromate,414 ferricyanide, 414 rosolic acid, 414 starch, mucilage, 414 Tetragonal system, 143,144 Therapeutic incompatibility, 397 Thermometer, 57 alcohol, 57, 60 calibration of, 61 Celsius’, 58, 59 Centigrade, 58, 59 Fahrenheit’s, 58 Reaumur’s, 58, 59 toluol, 60 Thermometers, 57-59 causes of variation, 60 conditions of delicacy, 60 graduating, 60, 61 normal, 60 testing accuracy of, 61 variation of, 60 Thermometric equivalents, table of, 461 Thiosulphates, assay of, 433 Time, unit of, 6 Tinctura ferri chloridi, 262 iodi, 262 iodi decolorata, 262 opii, 263 tincturae, 258 Tinctura; herbarum recentium, 261 Tincture chloride of iron, 262 iodine, 262 iodine, decolorized, 262 opium, 263 opium, assay, 263 opium, various strengths, 266 triturations, 389 Tinctures, 258 explanatory text, 262 fresh herbs, 261 homoeopathic, 388 menstruum, 258 preservation of, 261 preparation, 259 strength, 258 syllabus of, 267, 268 table of, 259, 267, 268 Titer, 413 Title, English, the, 3, 4 Latin, the, 3 Titration, 413 Tor refaction, 70 Torsion balances, 29 Tralles’ hydrometer, 43 Triclinic system, 146 Trimetric system, 144 Trimorphous, 146 Tripod, 83 Trituration, 121 Triturations, 310 homoeopathic, 388 Triturationes, 310 Troche-board, 315 -cutter, 315 Troches, 314 compressed, 314 Troches, moulded, 314 table of, 317 Trochiscation, 127 Trochisci, 314 Troy, term, derivation of, 8 weight, 9 Tubes for melting-point deter- mination, 64, 66 Tubing, bending, 90, 92 breaking off, 92 cutting, 89, 90 drawing out, 64, 90 properly and poorly bent, 92 Tumblerful, 14 Twaddell’s areometer, 43 Typical prescriptions, 399 U. Unguenta, 352 Unguentum hydrargyri, 355 hydrargyri nitratis, 355 Units, metric equivalents, 18, 19 Unsaturated solution, 128 Upward filtration, 178 Urinometer, 44 U. S. apothecaries’ or wine mea- sure, 12 fluid measure, 12 law relating to weights and measures, 12 V. Vacuum apparatus, 76-78 percolation, 206 Vallet’s mass, 313 Vaporization, 71, 84 Vehicle, the, 376 Very soluble, 123 Vessel, crystallizing, 150 Vials, for producing drops, 14 Vinegars, 248 table of, 249 Vina medicata, 256 Volhard’s solution, Volume, change in, by solution, 133 Volumetric analysis, 413 solution, bromine, decinor- mal, 445 hydrochloric acid, nor- mal, 420 iodine, decinormal, 432 oxalic acid,decinormal, 421 oxalic acid, normal, 420 potassium dichromate, decinormal, 436 potassium hydrate, centinormal, 429 potassium hydrate, normal, 426 potassium permangan- ate, dccinormal, 439 silver nitrate, deeinor- mal, 429 sodium hyposulphite, decinormal. 434 sulphuric acid, normal, 422 Volumetric solutions, 413 Volumetric standard solutions, preparation of, 419 W. Wafers, 305 Wash-bottle, 165 Wash, black, 228 yellow, 228 Washing by decantation, 161 of gases, 113, 114 of precipitates, 164,165 Watch glass, 111 Water, ammonia, 222 stronger, 222 baths, 81, 82 bitter almond, 221 cherry laurel, 222 chlorine, 223 chlorine, preparation, 132 chloroform, 222 of constitution, 151 creosote, 222 of crystallization, 151 heater, 56 hydrogen dioxide, 224 interstitial, 151 lead, 237 lime, 228 solvent properties, 129 weight of cubic inch, 10 Waters, distilled, 217 preservation, 220 medicated, 217 explanatory text, 221 preservation, 220 Waxes, emulsion of, 301 Weighing bottle, 134 Weight, 6, 8 ancient standards, 8, 9, apothecaries’, 10 apparent, 8 avoirdupois, 10 in vacuo, 8 troy,9 true, 8 unit of, 8, 9 Weights and measures, 6 Weights 21, 30, 31 aluminum, 31 analytical, 21,30 avoirdupois, iron, 30 block, 30 brass, metric, 31 coin, 31 cup, troy, 30 equivalents of, table, 466 handling, 24 metric, iron, 30 prescription, 30 Well-tube percolator, 201, 203 Westphal’s specific gravity bal- ance. 45 Wineglasstul, 14 Wine measure, 12 Wines, medicated, 256 Witt’s pharmaceutical press, 212 Yard, standard, 6,11 Yellow wash, 228 Yolk of egg emulsion, 298 Z. Zinc, pulverization of, 120