THE 
STUDENTS’ GUIDE 
IN 
Quantitative Analysis. 
INTENDED AS AN AID TO THE STUDY OF 
FRESENIUS’ SYSTEM. 
BY 
I 
H. CARRINGTON BOLTON, Ph.D., 
PROFESSOR OF chemistry in trinity college, 
HARTFORD, CONN, 
ILLUSTRATED. 
/ w V* V 
THIRD EDITION, WITH ADDITIONS AND CORRECTIONS 
SECOND THOUSAND 
NEWYORK; 
JOHN WILEY & SONS 
1899. COPYRIG.IT, 1881, 
By H. Carrington Boltom. 
Printed by 
Braunworth, Munn & Barber, 
Brooklyn, N. Y.. U. S. A. PREFA CE. 
A portion of the following pages originally appeared in 
the columns of the American Chemist, under the title: 
“ Schemes of Analyses executed in the School of Mines, 
Columbia College.” Numerous applications for copies in 
book form have induced the author to publish the Schemes 
under a more general title. 
Since writing the articles the author has been called to 
another sphere of labor, and the circumstances which led 
to their compilation are explained in the following para- 
graphs, quoted from the prefatory remarks accompanying 
the original publication. 
“ The system of instruction in Quantitative Analytical 
Chemistry, organized in the School of Mines, Columbia 
College, by Dr. C. F, Chandler, has been developed by the 
Assistants, who have had charge of the Laboratory for 
Quantitative Analysis, Mr. Alexis A. Julien, Dr. Paul 
Schweitzer, and the writer. 
The practical examples and the methods of analysis were 
originally selected by Prof. Chandler; the latter have been 
modified by the Assistants, and from time to time they 
have introduced new processes, conforming to the advances 
made in this department of chemical science. VI 
PREFACE. 
The plan of the Students’ Guide is similar to that 
in the excellent papers of Mr. Alexis A. Julien entitled: 
“Examples for Practice in Quantitative Analysis,” the 
details, however, are the result of observing the needs of 
students during my five years’ experience in teaching 
large classes. 
The fragmentary character of many portions of the 
notes is accounted for by the fact that they are intended 
to serve in part as lecture notes, and to indicate to the 
student the points to be studied. Fresenius’ “ System of 
Instruction in Quantitative Chemical Analysis” (American 
edition, by Profs. O.D. Allen and S. W. Johnson; New York, 
iBBi)is placed in the hands of each student on entering the 
laborator}'-, but many students are perplexed by the peculiar, 
though systematic, arrangement of this classic work, and 
are at a loss to know how to begin work, what to study, and 
where to find the information appropriate to particular 
cases. To aid the student in the study of Fresenius’ work, 
and not to displace it, is one of the objects of the Students’ 
Guide. It is then scarcely necessary to state that very 
free use has been made of Fresenius’ System; acknowl- 
edgment is, however, made in all cases. By occasional 
references to original papers the student’s attention is 
directed to methods, as detailed by their authors, with the 
hope of encouraging the student in research.” 
Trinity College, 
H. C. B. LIST OF ANALYSES. 
List of Analyses. Constituents to be determined. 
1. Baric chloride, Ba, Cl, H2O. 
2. Magnesic sulphate, MgO, S03, H2O. 
3. Ammonio-ferric sulphate, SOs, NH3, Fe203 by ignition, by pre- 
cipitation and volumetrically. 
4. Potassic chloride, K, Cl, 
5. Hydrodisodic phosphate, Na20, P2Ofl, H2O by direct weight. 
6. Silver coin, Au, Ag, Cu, Pb. 
7. Dolomite, CaO, MgO, Si02, Fe203, C02 by loss 
and by direct weight. 
8. Bronze, Cu, Sn, Zn. 
9. Coal, H2O, volatile matter, fixed carbon, 
ash, S. 
10. Copper pyrites, Cu, in duplicate. 
11. Alkalimetry, Soda ash, pearl ash. 
12. Acidimetry, Vinegar, hydrochloric acid. 
13. Chlorimetry, Bleaching powder. 
14. Type metal, Pb, Sn, Sb, Zn. 
15. Zinc ore, Zn. 
16. Chromic iron ore, Cr2Os. 
17. Pyrolusite, Mn02. 
iS. Feldspar, Si02, A1203, KsO, Na20. 
19. Slag, Si02, A1„03, CaO, MgO, FeO, MnO, 
s, p2'o8. 
20. Hematite, Si02, Fe, S and P. 
21. Titaniferous iron ore, Complete analysis. 
22. Pig iron, Fe. Mn, graphite, combined C, P, 
S, Si. 
23. Nickel ore, Ni, Co. 
24. Arsenopyrite, As. 
vii viii 
LIST OF ANALYSES. 
List of Analyses, Constituents to be determined. 
25. Guano. P205, CaO, MgO, Fe203, SiOs, H,O 
NH3, S03, organic matter. 
36. Superphosphate of lime, P206 soluble, precipitated, and in* 
soluble. 
27. Water, CaO, MgO, Na20, K2O, SOs, Cl, 
Si02, organic matter. 
28. Specific gravity of a solid, Heavier, lighter than, and soluble in 
water, minerals and alloys. 
29. “ “ “ liquid, By the flask, by hydrometer, and by 
weighing a solid in the liquid. 
30. Sugar, C, H, O. 
31. Potassic ferrocyanide, N by Willand Varrentrapp’s, and 
Melsens’ methods. 
32. Oil of turpentine, C, H. 
33. Urine, Qualitative and quantitative. 
34. Milk, Water, butter, casein, sugar, ash. 
35. Raw sugar, Water, crystallizable cane sugat 
grape sugar, ash. 
36. Petroleum, Fractional distillation, specific grav 
ity, fire test. INTRODUCTORY NOTES. 
By means of Chemical Analysis we determine the com- 
position of any substance. 
The object of Qualitative Analysis is to determine the 
nature of the constituents of a body. 
The object of Quantitative Analysis is to determine the 
amount of these constituents. 
Quantitative Analysis includes two methods, Gravimetric 
and Volumetric Analysis. 
In Gravimetric Analysis we convert the known constitu- 
ents of a compound into such forms as will admit of their 
exact determination by weight. This is done chiefly in 
two ways: 
ist. By separating one of the constituents of a body as 
such {e.g., Cu by the battery). 
2nd. By converting an existing constituent into a. new 
form by exchange of elements {e.g., AgN03-f-HCl=AgCl 
+HN03). 
The forms must fulfil two conditions: 
ist. Must be capable of being weighed exactly. 
2nd. Must be of known and fixed composition. 
is X 
INTRODUCTORY NOTES. 
The choice of form of precipitate depends on two consid- 
erations. The most preferable are— 
Ist. Those most insoluble in the surrounding liquid. 
2nd. Those in which the proportion of the constituents 
to be determined is very small compared with the weight 
of the precipitate {e.g., Sin BaS04 is only 13.7 per cent). 
In Volumetric Analysis the amount of a constituent is 
estimated by the action of reagents in solutions of known 
strength and of determined volumes. (See Notes on Vol- 
umetric Analysis, p. 40). WORKS FOR REFERENCE AND FOR STUDY. 
Fresenius. A System of Instruction in Quantitative Chem- 
ical Analysis. Editions: American, John Wiley and Sons, New 
York, 1881 ; last English ; last German. 
Thorpe. Quantitative Chemical Analysis. New York, last 
edition. 
Rose, H. Traite Complet de Chimie Analytique. Paris, 
1859-62. 2 vols. 
Rose H., and Finkener. Handbuch der analytischen Chemie. 
Leipzig, 1867. 
Mohr. Lehrbuch der chemisch-analytischen Titrirmeth- 
ode. Braunschweig, last edition. 
Sutton. Systematic Handbook of Volumetric Analysis. 
London, last edition. 
Rammelsberg. Leitfaden fur die quantitative chemische 
Analyse. Berlin, 1863. 
Crookes. Select Methods in Chemical Analysis. London, 
last edition. 
Bolley and F. Kopp. Handtuch der technisch-chemischen 
Untersuchungen. Leipzig, last edition. 
Wohler. Die Mineral Analyse in Beispielen. Gottingen, 
1861. Also translation by Henry B. Nason. Philadelphia, 
1871. 
Prescott. Outlines of Proximate Organic Analysis. Van 
Nostrand, New York, last edition. 
Caldwell. Agricultural Qualitative and Quantitative Chem- 
ical Analysis. New York, last edition. xii 
WORKS FOR REFERENCE AND FOR STUDY, 
Wanklyn. Water Analysis. London, last edition. 
Bunsen. Anleitung zur Analyse der Aschen und Mineral- 
wasser, Heidelberg, 1874. 
Ricketts. Notes on Assaying and Assay Schemes. New 
York, Wiley & Sons ; last edition. 
Storer. First Outlines of a Dictionary of Solubilities of 
Chemical Substances. Cambridge, 1864. 
Heppe. Die Chemische Reactionen der wichtigsten anor- 
ganischen und organischen Stoffe. (Tabellen, etc.) Leipzig, 
1875- 
Zeitschrift fur Analytische Chemie, Fresenius. Wiesbaden, 
1862 to date. 
Jahresbericht iiber die Fortschritte der Chemie. Giessen, 
1847 to date. 
Bulletin de la Socidte Chimique de Paris. Paris, 1864 to 
date. 
Chemical News. Crookes. London, 1860 to date. 
American Chemist. Chandler. New York, 1870-77. 
American Journal of Science and Art. J. D. and E. S. 
Dana. New Haven, 1819 to date. 
Journal of Analytical Chemistry. Edward Hart. Easton, 
1887 to date. THE 
STUDENTS’ GUIDE 
IN 
QUANTITATIVE ANALYSIS. 
Analysis No. i.— Baric Chloride, 
BaCl2 + 2H20. 
See Fres. Quant. Anal., § 141, I, a, and pages 790 tc 
795. (References are to Fresenius’ Quantitative Analysis, 
American edition, 1881.) 
A. Determination of Chlorine. 
Weigh out 0.8 to 1 grm. of powdered BaCl2 -f- 2H20 and 
dissolve in cold water in a beaker; add a slight excess of 
AgN03 previously acidulated with HN03; stir well, and 
warm. When the precipitate of AgCl has entirely settled, 
and the supernatant liquid is quite clear, pour off through 
a No. 2 filter; then add boiling water slightly acidulated 
with HN03, to the precipitate in the beaker; stir, and, 
after the precipitate has settled again, pour off through 
the filter. Continue this washing by decantation three or 
four times; then bring the precipitate on the filter by 
means of a glass rod or a feather; wash it down into the 
point of the filter; wash lastly with a little non-acidified 
water; cover the funnel with paper; label properly, and set 
aside to dry. Weigh a clean porcelain crucible; transfer 14 
QUANTITATIVE ANALYSIS. 
the precipitate to this crucible, removing the AgCl from 
the paper as completely as possible. Wrap a clean plati- 
num wire around the rolled-up filter, forming a “cradle;” 
burn the filter in the cradle over the inverted crucible 
cover ; do not let the ashes fall into the crucible. Moisten 
the ashes with cone. HN03 (one drop); heat one minute; 
add a drop of cone. HCI; evaporate cautiously, and heat 
the contents of the crucible and cover until the AgCl is 
partly fused, avoiding carefully a higher temperature than 
necessary. See Fres., § 82, b. Weigh the crucible and 
contents. For calculation, see D. 
AA.— Second Method.— Compare Fres., § 115,1, a,/3. 
Take to 0.2 to 0.5 grm. BaCh, -f- H2O; dissolve in warm 
water; acidulate with HN03 (free from chlorine); pour 
into a “parting flask;” add AgN03 in slight excess; cork 
the flask, and shake well. When well settled, wash the 
precipitate in the flask by decantation with warm water, 
without filtering. Invert the flask, covered with a watch- 
glass, over a weighed porcelain crucible, placed in a large 
porcelain dish, and filled with water. Withdraw the watch- 
glass carefully, allow the precipitate of AgCl to fall into the 
crucible, and remove the parting flask. Pour the water out 
of the crucible, remove the last portions with filter paper, 
and dry on a water-bath. Ignite to incipient fusion, and 
weigh. 
Note.— The precipitate settles best in presence of an 
excess of AgN03. 
B.—Determination of Barium. 
See Fres., § 132,1, 1, and § 101, I, a. Dissolve Ito 1.5 
grm. substance in warm water ; acidulate with HCI; dilute 
to about 250 c.c,; heat to boiling; when boiling hard, add 
dilute H3S04 in slight excess; boil some minutes and then CALCULATION OF ANALYSIS 
15 
keep warm while the precipitate settles. Test with a 
drop of H2S04; wash with boiling water by decantation ; 
then bring the precipitate on a No, 2 filter; wash well; dry 
and ignite precipitate in a platinum crucible; burn filter in 
a cradle as above, and add ashes to contents of crucible. 
See Fres., § 71, a. 
Note. Wash until the filtrate gives no precipitate with 
AgNOs. When estimating barium in the presence of 
nitrates, chlorides, etc., these salts are sometimes carried 
down with the BaS04. Since it is impossible to remove 
these by washing with water alone, treat the precipitate 
with very dilute HCI, or ammonic acetate. Cf. Crookes’ 
Select Methods, page 312. 
C. Determination of Water (by Ignition).— 
In a weighed crucible weigh out 1 to 1.5 grms. substance; 
heat very gently at first over a small flame, and increase 
the temperature very gradually; finally, heat to low redness; 
then cool, weigh, and repeat the operation until the weight 
remains constant. Caution: avoid too high a temperature, 
else the Cl will be expelled. When substances contain large 
percentages of water, as magnesia sulphate, hydrodisodic 
phosphate, alum, etc., begin to expel the water at ioo° C. 
in an air-bath. 
D. Calculation of Analysis.— 
See Fresenius, page 795, also § 196. Make two state 
ments, the first to determine the amount of the desired 
constituent in the precipitate obtained: 
Iw, - ) At. Wt. of the t Actual ) Actual ) 
nrecioitate f : constituent \ = weight of V ; weight of I 
P P j desired ) precipitate ) constituent. J 16 
QUANTITATIVE ANALYSIS. 
The second statement determines the percentage of the 
desired constituent in the substance taken: 
Wt. of sub- I . Actual weight of 1 _ Percentage of the 1 
stance taken f * constituent j 00 ' constituent. 
To check work, compare with theoretical percentages 
when possible. 
Theoretical composition of crystallized barium chloride. 
Ba= 56.15 
Cl2 = 29.09 
2HsO = 14.76 
100.00 
Use of Fresenius' Tables for the calculation of analyses. 
Compare Table 111, Fres., page 854. 
Examples: Fe203 X 07= 2Fe. 
BaOS03 X 0.34335 = S03. 
Consult Table IV, Fres,, pages 856, et seg., also page 840. 
•Example: 1.2685 grms. MgS04 yielded a precipitate 
of BaSQ4, which weighed 1.2074 gnns. From the table 
we have: 
1 0.34335 
.2 0.06867 
.OO 0.00000 
.007 0.00240 
.0004 0.00013 
1.2074 0.41455 = 803 
0.41455 
=32.78 per cent. S03. 
1.2685 REPORTING ANALYSES, 
17 
E. Reporting Analyses.— 
Analyses may be reported on blank forms printed on let- 
ter paper 8" x 10", having following headings ; 
Hartford, , 188 . Report of . Analysis 
of . Determination of . Grammes taken 
. Method of Analysis . These headings are 
printed in vertical column; in one horizontal line 
are placed following headings: Precipitates, Actual 
Weights, Constituents, Calculated Weights, Per- 
centages, Theoretical Percentages ; under each a blank 
space is left of 2 1-2 inches. Under “ precipitates ” place 
formulae of precipitates obtained; under “actual weights" 
place actual weights of precipitates ; under “ constituents ” 
place formulae of constituents to be reported; under “ cal- 
culated weights ” place the amounts of constituents existing 
in precipitates; under “percentages” place percentages of 
constituents actually obtained —in short, the results of 
analyses. The last column, “ theoretical percentages,” can 
be filled only in the case of few pure chemical salts. 
The words special remarks are printed about two inches 
from the bottom of the sheet, leaving room for remarks on 
processes employed, etc.* 
Notes to the Analysis of Barium Chloride. 
Reactions, (i) BaCl2 -f- H2S04 = BaS04 -}- 2HCI. 
(2) BaCl2 + 2AgN03 = 2AgCI + 8a(N03)2. 
The chloride of silver precipitate changes color on expos- 
ure to light, losing chlorine and forming Ag2CI; the change, 
however, is only superficial, but Mulder says the loss of 
weight is appreciable. 
* See specimen blank at the end of this book. l8 
QUANTITATIVE ANALYSIS. 
When one part of silver is thrown down as AgCl in 
1,000,000 parts of water, a slight bluish milkiness may still 
be seen. This cloudiness disappears on adding an excess 
of HCI. 
Barium sulphate requires more than 400,000 parts of 
water for solution. The solubility is not perceptibly 
increased by the presence of NaCl, KCI03 or 8a(N03)2, 
but HCI produces a sensible increase. (Cf. Storer’s Diction- 
ary of Solubilities.) 
Barium sulphate thrown down in a solution containing 
ferric salts is often contaminated with iron. This becomes 
evident by the reddish color of the precipitate after ig- 
nition. The precipitate may be purified by washing with 
ammonium acetate, or by solution in cone. H2S04, and re- 
precipitation by pouring into water. BaS04 dissolves in 
cone. H2S04 in the ratio of 5.7 parts to 100, and in Nord- 
hausen sulphuric acid as 15.9 to 100. 
Analysis No. 2.—Magnesic Sulphate. 
MgS04+7H20. 
See Fres., § 132, I, 1. Dissolve 1 to 1.5 grm. of sub- 
stance in warm water, acidulate with HCI, dilute to about 
250 c.c.; boil hard; add BaCl2 carefully, avoiding a large 
excess; boil a few minutes; let the precipitate of BaS04 
settle; wash by decantation and on the filter, and continue 
as in Analysis I, B. 
A. Determination of Sulphuric Acid. 
B.—Determination of Magnesium. 
Fres., § 104, 2. Dissolve about 1.2 grm. of substance 
in 150 c.c. cold water, in a beaker; add 30 c.c. NH4CI, DETERMINATION OF WATER. 
*9 
10 c.c. NH4HO, and a slight excess of HNa2P04. (Should 
a precipitate form on adding NH4HO, add NH4CI until it 
redissolves.) Stir the contents of the beaker well, avoiding 
touching the sides with the glass rod. Cover, and set aside 
for 12 hours, without warming. Filter and wash with cold 
water, to which one-fourth its volume of NH4HO has 
been added, until the filtrate acidified with HN03 gives 
only a slight opalescence with AgN03. Dry thoroughly on 
the filter, ignite in a platinum crucible, gradually increasing 
the heat; burn the filter on a cradle until quite white before 
adding the ashes to the contents of the crucible. If the pre- 
cipitate or ash is not white, moisten with a drop or two of 
cone. HN03, evaporate, and ignite cautiously. (See Fres., 
§ 74, b and c.) Weigh the precipitate as Mg2P207. 
C. Determination of Water. 
Heat i to 1.5 grm. salt in a weighed platinum crucible, 
and proceed exactly as in A7talysis I, C. 
Notes to Analysis of Magnesia Sulphate. 
On the solubility of ammonio-magnesic phosphate in 
water and saline solutions, Cf. Fres. page 816, paragraphs 
31-35- 
15 3°° parts of pure water. 
One part of 44300 “ “ ammoniated water, 
precipitate 7548 “ “ strong sol. of NH4CI. 
dissolves in 15600 “ “ water containing NH4HO 
and NH4CI. 
For a discussion of the solubility of the ammonio-magnesic 
phosphate, consult Cladding’s letter in Chem. News, vol. 
47, p. 71 (1883). 2C 
QUANTITATIVE ANALYSIS. 
Reactions.—By precipitation we have : 
2MgS04 + NH4CI 2NH4HO + 2HNa2P04= 
Mg2(NH4)2P208 + NH4CI + 2Na2S04 + 2H20. 
On heating we have: 
(NH4)2Mg2P2Os = Mg2P207 + 2NHj + H2O. 
Theoretical Composition— 
MgO 16.26 
S03 32.52 
7Ha° 51-22 
100.00 
Analysis No. 3.—Ammonia-Iron-Alum, 
Fe2(NH4)2(S04)4+24H20. 
A. —Determination of Sulphuric Acid, 
Dissolve 1 gr. to 1.5 grms. in water, add 5 c.c., dilute 
HCI to prevent ferric hydrate from precipitating with «-he 
BaS04, heat to boiling, add BaCl2 and proceed exactly ss 
in Analysis 2, A. 
B.—Determination of Ammonium. 
(Fres., § 99, b, 2, 0.) 
(1.) Dry the salt, if necessary, before weighing, by press 
ing the powder between folds of bibulous paper. Dissolve 
about 1.5 grms. in a little cold water in a casserole, add a 
little dilute HCI and an excess of PtCl4. Evaporate nearly 
to dryness on a water-bath scarcely heated to boiling. Add DETERMINATION OF IRON 
21 
50 to 80 c.c. alcohol to the casserole while still warm ; do 
not stir; let stand several hours. The supernatant liquid 
should be colored by an excess of PtCl4. 
(2.) Place a No. 1 Swedish filter in a small funnel, wash 
with very dilute HCI, then with water thoroughly; dry in 
the funnel, then remove the filter and place it on watch- 
glasses with clip; dry in an air bath ioo° C. exactly, for 
one hour precisely; then close glasses and weigh the whole. 
(3.) Bring the yellow crystalline precipitate on the 
weighed filter by means of a clean feather, wash with al 
cohol carefully, not too much, dry on funnel. Then trans- 
fer to clip, dry at ioo° C. as before, and weigh. Dry and 
weigh again, repeating until constant; calculate results. 
Precipitate has the composition (NH4)2PtCI6. 
[ln the case of potassium determinations, wash with a 
mixture of alcohol and ether; also concentrate filtrate and 
washings, filter from the secondary precipitate and add to 
the former.] 
(4.) Transfer the precipitate to a weighed crucible, burn 
the filter and add the ashes; ignite gradually and strongly. 
Weigh the Pt remaining as a check on the first determi- 
nation. 
[ln the case of potassium, add a little oxalic acid in pow- 
der to the contents of the crucible, ignite, wash residue 
with water, dry on water-bath, ignite, and weigh. (See 
Fres., § 97, 3, /?.)] 
For solubility of ammonio-platinic chloride, see Fres. 
p. 812, paragraph 16. 
(J. Determination of Iron. 
I. By Ignition.—(Fres., § 113, 1, e.) Expose 1.0 grm. of 
the salt in a weighed covered platinum, or porcelain 22 
QUANTITATIVE ANALYSIS. 
crucible, to a moderate heat, gradually raise the temper* 
ature till all the water is expelled; then heat intensely be- 
fore the blast-lamp. Weigh the residue as Fe203; heat 
and weigh again. Test the residue for H2S04. 
11. By Precipitation. (Fres., § 113, 1, a.) Dissolve 
about 1 grm. of the salt in question in a large beaker with 
about 250 to 300 c.c. of water, acidify with HCI, heat nearly 
to boiling, add NH4HO in excess; let settle after stirring; 
wash hot by decantation. (N.B. Wash out NH4CI com- 
pletely, lest on subsequent ignition a portion of the iron 
volatilize as chloride. One grm. of ferric hydrate requires 
nearly one gallon of water.) Bring precipitate on filter, dry 
thoroughly on funnel, ignite and weigh. Burn filter and 
precipitate separately. (See Fres., § 53.) 
Ammonia acts on the ferric solution in accordance with 
the equation: 
2[Fe2(So4)3] + i2NH4HO = 2Fe2033H20 + 
6[(NH4)2SO4] + 3H20. 
111. Determination of Iron by Marguerite’s Meth- 
od.— See Fres., § 112,2, a. Compare Mohr’s Titrirmethode, 
pages 180 to 204, also Crookes’ Select Methods, page 73. 
(l.) Standardization of the Solution of Potassium Per■ 
inanganate. Dissolve 13 grms. K2Mn208 in two litres of 
distilled water, shake, let settle over night, and siphon off 
into a bottle. Fill a Gay-Lussac burette with this solution 
up to the zero mark. 
Dissolve exactly 0.2 grm. of piano-forte wire, previously 
cleaned with sand-paper, in a closed flask with cone. H2S04 
and sufficient water. Boil until dissolved; cool suddenly 
under the faucet, but to avoid collapse of flask wait a few DETERMINATION OF IRON. 
23 
moments before allowing the cold water to fall upon it. 
The flask should be provided with a Kronig caoutchouc 
valve. This is made by inserting a short glass tube through 
a cork in the neck of the flask, and fitting to the projecting 
end of the tube a piece of caoutchouc tubing about 10 cm. 
long. A slit 4 to 5 cm. long is cut lengthwise in the 
caoutchouc tubing, and the open end stopped with a piece 
of glass rod. The valve is then complete. (Fig, 1.) 
Fig. 1. 
Fig. 2. 
In place of the Kronig valve, another form may be used. 
The projecting end of the glass tube, fitted to the cork in 
the neck of the flask, is passed through another cork until 
just even with its surface. Over the end of the cork and 
tube a small piece of sheet caoutchouc is fastened by means 
of pins, the rubber acting as the valve. (Fig. 2.) Having 
effected the complete solution of the iron wire in one of 24 
QUANTITATIVE ANALYSIS. 
these flasks, pour the solution into a large beaker contain- 
ing about 300 to 400 c.c. H2O, placed upon a sheet of 
white paper; wash flask carefully, and add to beaker. Now 
pour the solution of K2Mn2Os from the burette, drop by 
drop, stirring continually, and continue until the pink hue 
first permanently colors the whole liquid. Read the burette 
and calculate as follows for the standard: 
c.c. used: I c.c. = grms. Fe : or, or standard. 
Repeat the titration until two concordant results are ob- 
tained. Correction : To allow for the impurities in the 
iron, multiply the amount taken by 0.997. 
(2.) Reduction of the Ferric Solution. Dissolve 4.0 
grms. ammonia-iron-alum in water, dilute to exactly 500 
c.c.; mix well, and divide in halves. 
Place a piece of amalgamated zinc and a strip of plat- 
inum foil in each reduction bottle; pour in the solutions 
and washings; add a little cone. H2S04, and cover the 
bottles with watch glasses. The reduction requires six to 
eight hours. If the platinum foils are new, scour them 
with silica, rub them with KHO solution, then with HN03, 
and wash carefully. Removal of the polished and possibly 
greasy surface hastens the evolution of hydrogen and con- 
sequently the reduction. 
Reaction : 
Fe2(S04),+Zn+H!S04=2(FeS04)+ZnS04+HIS04. 
(3.) Performance of the Analysis.—When the reduction 
is complete, ascertained by testing a few drops with am- 
monium sulphocyanide, pour the contents of each reduction DETERMINATION OF IRON. 
25 
bottle into a large beaker, add H2S04, and K2Mn208 from 
the burette until a permanent pink color is obtained. (See 
Fres., § 112, 2, a.) The two determinations, one in each 
bottle, should not vary more than 0.2 per cent. 
(4.) Calculation of the Analysis. No. of c.c. used >< 
standard a or amount Fe. 
a X ioo , , . 
■■ j—rr—s— = per ct. of iron, 
wt. of salt taken 
IV. The STANDARD OF THE SOLUTION of potassium 
permanganate may be determined in several ways. 
{a.) Mohrs Method. Weigh out 1.4 grm. ammonio- 
ferrous sulphate, dissolve and titrate as usual. One-seventh 
of its weight = iron. Ammonio-ferrous sulphate = FeS04 
+ (NH4)2SO4 + 6H20. 
In both this and the preceding method the reaction is 
the same. 
ioFeS04+BH2S04+K2Mn20B=5Fe2(S04)3+K2S04+ 
2MnS04 -\- 8H20. 
(bi) Hempel's Method. Weigh out 6.3 grms. pure, 
dry oxalic acid, dissolve in one litre of water, making 
N 
a decinormal (—) solution. Dilute 50 c.c. of this solu- 
tion, add 6 to 8 c.c. cone. H2S04, warm and titrate. 
The reaction in this case is as follows : 
5 H2C204 3H2504 -j- K2Mn203 ioC02 -f- 2MnS04 -f- 
K2S04+8H,0. 2 6 
QUANTITATIVE ANALYSIS. 
D-— Determination of Water. 
Water may be determined by difference. 
Theoretical composition: 
(NH4)2o=z 5.39 
Fe203=:i6.60 
4503=33.20 
24^0=44.81 
100.00 
Analysis No. 4.— Potassium Chloride. 
KCI. 
Expel hydroscopic moisture carefully by heating and 
stirring in a porcelain dish over a Bunsen burner, before 
filling the weighing tube. 
A- Determination of Chlorine. 
Dissolve about 0.8 grm. in warm water and proceed ex- 
actly as in Analysis No. 1, A. 
B. —Determination of Potassium. 
Sec Fres., § 97, 3, a, and Crookes’ Select Methods, page 1. 
Dissolve about 0.5 grm. in a little cold water in a casse- 
role, and proceed exactly as in the determination of ammo- 
nia, Analysis No. 3, B, paying especial attention to the sen- 
tences in brackets. 
For solubility of potassio-platinic chloride, see Fresenius1 
Quant. Analysis, p. 811, paragraph No. 8. DETERMINATION OF SODIUM. 
2 7 
Theoretical composition: 
K 52.41 
Cl 47-59 
100.00 
Analysis No. 5.— Hydrodisodic Phosphate. 
Na2HP04+ i 2H20. 
A-— Determination of Sodium. 
Cf. Fres., § 135, a, /?.—Dissolve about 1 grm. salt in 20c 
c.c. water in a large beaker. 
Weigh off about 0.6 grm. clean piano-forte wire, place in 
a flask, add cone. HCI with some HNOa, boil hard (undei 
a hood); when fully dissolved, continue boiling until excess 
■of HN03 is removed, then dilute, and, if necessary, filter 
through a filter previously washed with dilute HCI. 
Add this solution of pure Fe2Cl6 to that of the hydrodiso- 
dic phosphate, and immediately an excess of NH4HO. 
Heat and let the precipitate stand some hours; wash by 
decantation with boiling water very thoroughly. Evap 
orate the filtrate with a slight excess of dilute HCI on 
a water-bath to dryness. Heat with care until fumes 
of NH4CI cease to come off; dissolve the residue in 
water; filter through a very small filter into a small 
weighed dish, platinum preferred. Add a few drops 
of dilute HCI; evaporate to dryness on a water-bath; 
ignite very cautiously, not too long, and weigh the NaCl. 
If the residue is not perfectly white and soluble in water 
without residue, dissolve, filter through a very small filter 
into another weighed dish. Evaporate and ignite again. 
Test residue. 28 
QUANTITATIVE ANALYSIS. 
B.~Determination of Phosphoric Acid. 
Fres,, § 134, I, b, «. Dissolve about 1.2 grms. of the 
salt in question in cold water; add “ magnesia mixture ”in 
excess and NH4HO; set aside for twelve hours, and then 
continue exactly as in Analysis No. 2. Consult Fres., 
Exp. 32, p. 817. 
C.—Determination of Water. 
(1) By ignition.—Weigh out about 0.8 gramme; place 
it in a weighed crucible, in an air-bath, until partially de- 
hydrated ; then heat cautiously over a Bunsen burner, ig- 
nite eventually to redness, and weigh. 
(2) By direct weight. Weigh out about 0.7 gramme 
substance, and introduce it into the weighed ignition bulb 
by means of a very narrow piece of folded paper. Weigh 
CaCl2 tube, and arrange apparatus, as shown in Fig. 25, 
page 61, of Fres. Quant. Analysis (American edition, 1881), 
substituting aspirator for gasometer if more convenient. 
Heat cautiously, aspirating continually, and raise the tem- 
perature to a low red heat for three minutes. In driving 
the water into the CaCl2 tube be careful not to burn the 
cork. Aspirate while cooling, not too rapidly. Weigh 
CaCl2 tube after cooling and the ignition bulb as a check. 
Consult Fres., § 36. 
Theoretical Composition: 
When water is determined by heating to redness, the 
calculation must be based on two molecules of the salt. 
2Na20 = 17.32 
Pa05 = 19.83 
25H20 = 62.85 
100.00 SILVER COIN. 
29 
Analysis No. 6.—Silver Coin. Scheme. Au(?) + Ag + Pb + Cu. 
Clean the coin by friction with wood ashes and weigh it. Dissolve in HNOs in a covered casserole, expel 
excess of acid by evaporation to small bulk on a water-bath, add water, filter, and wash thoroughly. 
Residue a. 
Dry on filter, ig- 
nite, and weigh as 
Au (?)-f- Ag3S. 
Filtrate a. 
Heat filtrate together with wash water to boiling; add dilute HC1 in excess, agitate well, 
let settle till perfectly clear, filter and wash. 
Precipitate b. 
Dry, ignite sepa- 
rately from filter, 
and treat exactly 
as in Analysis No. 
i* A. 
Weigh as AgCl, 
and calculate Ag. 
Cf. Fres., § 115, 
1, a, P, also Fres., 
$ 82, b. 
Filtrate b. 
Add 3 c.c. dilute H2S04 to filtrate + washings; evaporate nearly to 
dryness on a water-bath ; filter through a No. 1 filter, wash with as little 
water as possible, and yet completely. 
Precipitate c. 
Dry, ignite in 
porcelain crucible, 
burning the filter 
on cover. Weigh 
as PbS04. 
Cf. Fres., § 116, 
3, a, p, also Fres., 
§ 83, d. 
See also Crookes’ 
Select Methods, p. 
209. 
Filtrate c. 
Heat to boiling in a casserole, concentrate if ne- 
cessary, add pure KHO solution in excess, boil some 
minutes, or until the bluish precipitate becomes quite 
black, wash hot by decantation, bring on filter, 
cleanse casserole with a rubber-tipped glass rod, or 
with the tip of your little finger. 
Precipitate d. 
Dry, ignite, and weigh 
as CuO. If some CuO is 
reduced by filter paper, 
add a drop of HNOs, evap- 
orate and ignite; this 
may, however, occasion 
loss. Cf. Fres., § 119, 1, 
a, a. 
Filtrate d. 
Test with H,S, passing 
the gas through solution 
some minutes; if precipi- 
tate forms let settle, collect 
on filter, dry and ignite. 
Weigh as CuO. (By roast- 
ing CuS is largely oxi- 
dized.) See Fres., § 85, by 
and § 119, 3, a. Analysis No. 7.—Dolomite. Skeleton Scheme. 
CaC03 + MgCOa. 
Dissolve, evaj orate, and filter. (See Note 1.) 
Residue a. 
Filtrate a. 
SiO,. 
Throw down iron and alumina. (Note 3.) 
(See Note 2.) 
Precipitate b. 
Fe203 -f- AHOg. 
Filtrate b. 
Throw down calcium. (Nnfp c.'l 
For determination ol 
CO, see Note 8. 
Dissolve, reprecipitate 
and add filtrate to Fil- 
trate b. 
Precipitate c. 
CaC204. 
Filtrate c. 
Throw down magnesium, 
{Note 7.) 
{Note 4.) 
Note 6. 
For calculation see Note 9. 
NOTES TO FOREGOING SCHEME. 
Note I. — Take 1.5 to 2.0 grammes finely powdered mineral, dissolve in dilute HC1 in a 
casserole ; heat, add a little HNOs to oxidize iron and sulphides ; evaporate to dryness on a 
water-bath ; moisten with HC1, add water, digest, and filter from the Si02 -f- Silicates. Dry 
on funnel, ignite, and weigh. See note 2. 
30 
y U ANTI TATI VE ANALYSIS. ANALYSIS OF DOLOMITE. 
31 
Note 2.—If it is desirable to determine the Si02 in the 
silicates present, “ Residue a ” must be treated as follows : 
Dry and ignite (with filter), mix in a platinum crucible with 
about six parts of Na2C03 (anhydrous), and fuse at a red 
heat. Cool, remove the fused mass with boiling water, add 
an excess of HCI, evaporate to dryness on a water-bath, 
heat in an air-bath until the HCI is completely expelled ; 
again moisten with HCI, dissolve in water, and filter from 
the residue. The residue which is now pure hydrated Si02, 
is dried, ignited, and weighed. The filtrate must be added 
to “ Filtrate a.” Examine Fres., § 140, 11, b,a, and § 93, 9. 
Note 3.— Heat the filtrate from “ Residue a,” add NH4CI, 
and NH4HO in slight excess. (The NH4CI may be omit- 
ted if the “ Filtrate a” is very acid.) Heat until excess of 
NH4HO is expelled, filter quickly, and wash hot. See Fres., 
§ 113, 1, a, and § 105, 1, a. 
Note 4.—“ Precipitate b” is partly washed, and then, while 
moist, dissolved in a little warm dilute HCI on the filter, the 
solution is reprecipitated by NH4HO and the precipitate 
brought on the same filter, washed thoroughly, dried, and 
ignited. Weigh as Fe2034-Al203. The second filtrate is 
added to “ Filtrate bd 
Note 5.—Concentrate “ Filtrate badd some NH4CI un- 
less present already, add (NH4)2 C 204 in considerable ex- 
cess, and some NH4HO. Let stand 12 hours in a warm 
place. Wash partially and filter. See Fres., § 154, 6, a ; 
also § 103, 2, b, a. 
Note 6.—Dissolve the partially washed “ Precipitate c ” 
in HCI, reprecipitate with NH4HO and a little (NH4)2C2Q4. 
Filter and wash hot, add filtrate and washings to “ Filtrate 
cd Dry precipitate on funnel, transfer to crucible, burn fil- 
ter, add ashes, add a few drops of cone. H2SQ4 to contents of 32 
QUANTITATIVE ANALYSIS. 
crucible, ignite cautiously to low redness, and weigh as 
CaS04. Compare Fres., § 103, 2, b, a. 
Note 7.—If care has been taken to avoid undue excess of 
NH4CI in the preceding steps, the magnesium may be 
thrown down in “ Filtrate c ” immediately. Otherwise the 
NH4CI must be expelled as follows ; Concentrate the liquid, 
add 3 grms. of HNOs for every grm. of NH4CI supposed 
to be in the solution, warm gently (6o° C.) and eventually 
heat to boiling. 
Concentrate “ Filtrate c” add NH4HO and Na2HP04 
and proceed as in Analysis 2. B. See Fres., § 104, 2, and 
§ 74- 
Notes on the Decomposition of NH4CI by HN03 in solu- 
tion. Comptes Rendus, October 13, 1851 (Maumene). 
J Lawrence Smith in American Chemist, Vol. 111, p. 201. 
Also Am. Jour. Sci. (2), Vol. 15, note, page 240, which is as 
follows : “ The character of the decomposition which takes 
place is somewhat curious and unexpected: it was first 
supposed that equal volumes of Cl, NzO, and N were given 
off, but it is shown that nearly all the NH4HO, with its 
equivalent of HN03, is converted into N2O, the liberated 
HCI mixing with the excess of HN03. A little of the 
NH4CI+HN03 does not undergo the decomposition first 
supposed, and in this way only can the small amounts of N 
and Cl be accounted for.” “ Some nitrous or hyper-nitrous 
acid forms during the whole process if cone. HN03 is used 
little or none if dilute HNOs.” 
The action of NH4N03 on NH4CI is theoretically as 
follows: 
2(NH4NO3j+NH4CI=SN+CI+6H2O. ANALYSIS OF DOLOMITE. 
33 
The following are possible reactions : 
8NH4CI + ioHN03=9N20+8C1 + 2iH20, 
2HN03+2NH4CI=N2O+2CI+2N + 5H20, 
HN03+NH4Cl=HCl+N30-f2HaO, 
and 
2HN03+NH4CI=N2O+CI+NO2+3H2O, 
and 
HCI+3HNO3=NO + Cl+NoCla+No3+4Cl + 5HaO. 
Note 8. Determination of C02.—/. By loss. Fres., § 139, 
11., d, bb, and cc. 
Weigh out 1.0 to 2.0 grms., place 
in the Geissler apparatus, fill the 
proper portions of the apparatus with 
HCI (dil.) and with H2S04 (cone.) 
respectively. Weigh apparatus. Cau- 
tiously let the HCI flow on the min- 
eral, warm gently, heating at the last 
till the solution begins to boil. Cool 
apparatus and weigh. For details 
consult Fresenius, as above. Do not 
hurry this process too much. 
Fig- 3- 
ll.—By direct weight. Consult Fres., § 139, 11., c, 
Arrange apparatus as in Fig. 4. Suspend tubes by wire 
loops on nails. 
a contains soda-lime. 
c is a flask of about 200 c.c. capacity. 
d contains cone. H2S04. 
e contains pieces of pumice-stone saturated with cone. 
h2so4 ; avoid much liquid in the bend. 
/contains pumice-stone saturated with anhydrousCuS04, QUANTITATIVE ANALYSIS. 
34 
N.B.—Make a strong hot solution of CuS04-[-5H20, add 
pieces of pumice-stone, boil hard, evaporate to dryness and 
ignite well. The product should be nearly white. 
g contains in outer tube, soda-lime ; in inner tube, (h) 
pumice-stone saturated with H2S04 ; weigh these together 
both before the absorption and after. 
Place 1.0 to 1.5 grms. mineral in c, weigh g and h, and 
connect apparatus ; ais not attached at first. Pour a little 
water through the funnel tube into c, then add gradually 
HCI, diluted one-half with water. Attach a, and aspirate 
gently. Heat cautiously to incipient ebullition ; maintain 
this a few moments, and let cool while the aspiration 
continues. Weigh increase of weight gives C02. 
Fig. 4. 
Note 9. Calculation.—Normal dolomite contains ; 
30.4 per cent. CaO. 
47.8 “ CO. 
21.8 “ MgO. 
100.0 
Having estimated these constituents, calculate the ANALYSIS OF BRONZE. 
35 
amounts of CaC03 and MgCOs, and report under “ Special 
Remarks,” thus : 
CaO; C02 = CaO found; C02 required or M. 
MgO ; C02 = MgO found : C02 required or N. 
and M + N must= C02 found, nearly. 
Analysis No. 8 Bronze. 
To be determined, Sn, Pb, Cu, Zn. 
A.—Determination of Tin. 
Dissolve about 0.6 grm. bronze filings, carefully freed 
from accidental impurities, in moderately dilute HN03, in 
a flask in the neck of which is placed a small glass funnel. 
After complete solution (except the Sn02), transfer con- 
tents to a porcelain dish, evaporate to dryness, moisten 
with HN03, add H2O, and filter from the Sn02. Dry this 
residue, ignite in porcelain, and weigh. Fres., § 126, 1., a, 
and § 91. 
B.—Determination of Lead. 
To filtrate from A add dilute H2S04, evaporate until 
fumes of H2S04 appear, or the residue is nearly dry, let 
the dish cool, then add water, and filter from the PbS04. 
See Fres., § 163, 2, and § 116, 3, a, /?. Dry, ignite, and 
weigh precipitate. See Fres., § 83, d. 
C. Determination of Copper. 
The filtrate from B. should not measure more than 100 
c.c. Place the solution in a large platinum dish, arrange 
the Bunsen cells of a galvanic battery, connect the zinc QUANTITATIVE ANALYSIS. 
element with the platinum dish, and the carbon element 
with a small piece of platinum foil which is immersed in 
the liquid. Let the battery run four or five hours. Take 
out a drop of the solution with a pipette, place on a watch 
glass and test for Cu with H2S. Pour out the solution 
when the precipitation is completed, and wash thrice with 
small quantities of water. Then wash the copper film 
with alcohol twice, dry in the hand, over a Bunsen burner, 
at a very gentle heat, and weigh quickly. 
N.B. —lt is advisable to test solution for Cu before 
proceeding further. 
D. Determination of Zinc. 
Heat the filtrate and washings from C to boiling, add 
excess of Na2C03, boil a few minutes, wash by decantation 
hot, then on filter, Dry, ignite, and weigh as ZnO. P'res., 
§ 108, 1, a, and § 77. 
Analysis No. 9. Coal. (Proximate Analysis.) 
To be determined, Moisture, Volatile and Combustible 
Matter, Fixed Carbon, Sulphur, and Ash. 
A-— Determination of Moisture. 
Pulverize the coal very finely, heat one to two grms. in a 
half ounce platinum crucible for fifteen minutes at H5°C. 
in an air-bath, cool and weigh. Repeat this desiccation in 
the air-bath, weighing at intervals of ten minutes, until the 
weight is constant or begins to rise. Loss of weight gives 
moisture. In reporting, give exact temperature at which 
it was determined. N.B.—The increase in weight is due 
to oxidation of the coal; it generally begins after heating ANALYSIS OF COAL. 
37 
thirty to ninety minutes in the air-bath. Anthracite coal 
may be heated an hour or more. See Chem. News, Am. 
Repr., Vol. V., p. 80, 
B.—Determination of Volatile Combustible Matter. 
Heat the same crucible with contents, closely covered, 
to bright redness over a Bunsen burner, exactly three and 
one-half minutes, and then without allowing the crucible 
to cool, heat strongly before the blast-lamp, exactly three 
and one-half minutes more. Cool and weigh. The loss 
gives the volatile and combustible matter, and includes half 
the Sin the FeS2. See F below. 
C- —Determination of Fixed Carbon, 
Heat crucible and contents, uncovered, over Bunsen 
burner, until all carbon is burned off and the weight is 
constant. This takes from one to four hours or more. 
Loss in weight = fixed carbon, including half the S. 
D- Determination of the Ash. 
The difference between the weight last obtained and that 
of the crucible gives the weight of the ash. Note color of 
the ash. 
B. Determination of Sulphur. 
Secure a sample of anhydrous Na2C03, shown to be ab- 
solutely free from S by the silver test. 
Weigh out about two grms. coal in fine powder, mix 
with about ten grms, NaN03 and ten grms. Na2CQ3 on 
glazed paper. The sodium salts need not be weighed ac- 
curately ; KN03 may be used in place of NaN03. Deflag- 
rate in a covered two-ounce platinum crucible, heating over 38 
QUANTITATIVE ANALYSIS. 
a Bunsen burner; add the mixed coal and sodium carbonate 
little by little, replacing the cover of the crucible quickly 
each time. Do not expect to effect a perfect fusion. Place 
the crucible and contents in a casserole, add water, and 
digest until the mass is disintegrated, and the crucible can 
be removed. Add cautiously an excess of HCI, heat to 
boiling, and throw down the H2S04 with BaCl2 as usual. 
If flocks of Si02 remain insoluble in HCI, evaporate to 
dryness on water-bath, heat until HCI is expelled, add 
water, filter, and proceed as above. If the BaS04 is red- 
dish after ignition, wash with solution NH4C2H30, and 
then with pure water, dry, ignite, and weigh again. The 
BaS04 may also be purified by solution in cone. H,SO4 and 
reprecipitation with water. 
Second Method for Determining Sulphur. Put two to 
five grms. powdered coal in a flask holding a litre; add 
ioo c.c. HNOj and five grms. powdered KCI03, heat to 
boiling, adding more reagents as needed; continue until all 
the carbon is oxidised. Transfer to a dish, evaporate to 
dryness, add HCI and water, throw down H2S04 with 
BaCl2, and proceed as usual. Consult Hayes’s article in 
Am. Chem., Feb., 1875, also Wittstein’s article in Am. 
Chem.y April, 1876. 
F. Calculations. 
Theoretically we should deduct half S from the volatile 
combustible matter (because iron pyrites loses one-half its 
sulphur at a red heat), one-eighth S from the fixed car- 
bon, and three-eighths from the ash. (2FeS become Fe2Os, 
or 8 X 4 32 reduces to 8 X 3 24.) 
Practically half the amount of sulphur is deducted from 
the volatile combustible, and half from the fixed carbon; 
reports should be made out accordingly. ANALYSIS OF COPPER PYRITES. 
39 
G. Estimation of Carbon and Hydrogen. 
Ignite one grm. of coal with PbCr04 in a hard glass 
tube 0.25 metre long. Pass the H2O, C02 and H2S04 
formed through two U-tubes, one containing ignited CaCl2, 
and the other a solution of Pb(NO3)2, and through a potash 
bulb. The increase in weight of the first U-tube gives the 
H2O, and that of the potash bulb the C02. 
Calculation of Calorific Power. One part of carbon in 
burning yields 8,080 calorific units, and one part of hydrogen 
in burning 34,460 calorific units. Hence to calculate total 
calorific units in a coal, multiply the percentage of C by 
8,080 and divide by 100; also multiply the percentage of 
Hby 34,460 and divide by 100. Add the quotients. 
(A calorific unit is the amount of heat necessary to raise 
one grm. of water from o° to i° C.) See Chem. Newsy 
XXXIV, p. 233. 1876. 
Analysis No. 10. Copper Pyrites. 
Determination cf Copper. 
Pulverize very finely. Weigh out exactly 2 grms., place 
it in a flask of about 300 c.c. capacity and covered with a 
small funnel, the stem of which is slipped into the neck of 
the flask. Add 20 c.c. cone. HN03, 5 c.c. cone. HCI, mix- 
ing these in flask under the hood. Digest some minutes, 
then add cautiously 20 c.c. cone. H2S04 and boil hard un- 
til fumes of H2S04 appear abundantly. Cool, add water 
with caution, dilute not too largely, filter from residue (Sio2, 
CaS04, etc.), and wash. Test residue for copper before 
the blow-pipe. Dilute filtrate to 200 c.c. exactly, mix well 
by pouring into a dry beaker and back again three or four 
times; divide in halves by taking out 100 c.c. with a pipette QUANTITATIVE ANALYSIS. 
and place in a platinum dish previously weighed. (N.B.—■ 
Volumetric apparatus as sold is rarely reliable, therefore 
test pipette and flask before measuring as above.) Arrange 
two cells of a Bunsen battery, placing the “ battery acid ” 
(one part of H2S04 diluted with 8 to 10 of water) in the 
outer cell and “battery fluid ” (K2Cr2O7+H2SO4-l-H2O) in 
the inner. Connect the zinc (~\~) pole with the platinum 
dish, and the carbon (—) pole with a piece of platinum 
foil which is immersed in the liquid. Cover the platinum 
dish with two pieces of glass plate, one each side of the 
platinum foil, to prevent loss by spattering. Or use the 
cone or spiral described in Chem. News, XIX, p. 222 (1869). 
See also Crookes Select Methods, pages 187-200. 
It is best not to let the battery run all night; prepare 
the solutions on one day and start the battery the next 
morning. Four hours or more usually suffice for complete 
precipitation. 
Test a few drops of the solution with H2S. 
When precipitation is complete, pour off liquid, wash 
copper with distilled water three or four times (work rap- 
idly), then with strongest alcohol twice; drain the alcohol 
off, dry the copper at a very low heat, holding the plati- 
num dish in the hand over a small flame, which must not 
touch the dish, and weigh immediately. Next treat the 
remaining 100 c.c. solution likewise; the two determina- 
tions should agree to about 0.2 per cent. 
Analyses No. II and No. 12. 
Definition. “ Volumetric Analysis is a form of quantita- 
tive analysis in which we seek to estimate the amount of 
a substance from the determinate action of reagents in 
Introductory Notes on Volumetric Analysis. VOLUMETRIC ANALYSIS. 
41 
solutions of known strength, the amount of the reacting 
substance being calculated from the volume of the liquid 
used.” The first principles and method of procedure have 
been foreshadowed in Analysis No. 3, HI., Determination 
of Iron by Marguerite’s method. For explanation of gen- 
eral volumetric methods, see Fres. § 54, and consult Sut- 
tons Handbook of Volumetric Analysis, also Mohr’s Lehr- 
buch der chemisch-analytischen Titrirmethode. 
Principles. When volumetric analysis first came into 
use, the standard solutions were so prepared as to give 
results in percentages ; thus in Alkalimetry, one standard 
solution of acid was used for potash, another for soda, etc. 
The modern system is based on the fact that acids and 
alkalies (as well as other reagents) neutralize each other in 
the proportion of their molecular weights, or of simple 
multiples of the same ; consequently standard solutions are 
.so prepared that one litre contains one-half or the whole 
of the molecular weight of the reagent weighed in grins. 
For example, the molecular weight of HCI being 36.5 and 
that of KHO 56.1, 36.5 grms. of HCI exactly neutralize 
56.1 grms. of KHO, and if these respective amounts be 
dissolved in one litre of water, the whole of one solution 
will not only neutralize the whole of the other, but any 
aliquot part of one will exactly neutralize a similar aliquot 
part of the other. And by using graduated vessels, (bu- 
iettes,) the amount of reagent used is determined by the 
volume of the solution. (Before employing burettes, 
pipettes, and graduated flasks, care should be taken to test 
the accuracy of the graduation.) 
Standard Solutions. Solutions containing the molecu- 
lar weight of the reagent expressed in grms. per litre are 
called normal solutions ; in the case of di-basic acids 
{H2SO4, H2C204 etc.) and of “ di-acid ” alkalies (Na2CO3) 42 
QUANTITATIVE ANALYSIS. 
one-half the molecular weight of each is taken, making 
half normal solutions. 
The standard solutions of the following reagents are 
made with the quantities indicated : 
Oxalic acid 
H2C2044-2 aq. 
63 grms. per litre 
Sulphuric acid 
h2so4 
49 “ 
Hydrochloric acid 
HC1 
36.5 “ 
Sodium carbonate 
Na2C03 
53 “ 
Potassium hydrate 
KHO 
56,1 “ “ 
Ammonia 
NH3 
17 “ “ 
The point of neutralization or end reaction is determined 
by adding to the solutions some organic coloring-matter 
which changes in hue under the influence of an alkali or 
an acid. The “ indicators ” commonly used are litmus 
solution and cochineal solution. 
Alkalimetry, 
(Cf. Sutton’s Handbook.) 
1. Preparation of Litmus Solution.—Digest 5 to 6 
grms. litmus with about 200 c. c. water for half an hour or 
more; decant the clear liquid or filter; add very dilute 
HNOj drop by drop, until the color is changed to violet. 
If properly neutralized less than one-tenth c.c. of stand- 
ard acid should distinctly redden one c.c. litmus in 100 
c.c. of water. 
2. Sulphuric Acid.— Mix about 60 grms. cone. C.P. ALKALIMETRY. 
43 
H2S04 of sp. gr. 1.840 with three or four times its volume 
of distilled water ; cool and dilute to one litre. The ex- 
act standard of this solution is determined by testing with 
sodium carbonate, as below. 
3- Sodium Carbonate Solution. Weigh off about 12 
grms. anhydrous C.P. Na2C03; heat in a porcelain dish 
to low redness, stirring until moisture is expelled; place in 
a desiccator to cool. Weigh out accurately 10.6 grms. of 
this, and dissolve in distilled water. Dilute to exactly 200 
c.c. This gives a half normal solution, each c.c. of which 
contains 0.053 grm. of sodium carbonate, as shown by this 
simple calculation: 
Na2 = 46 
C =l2 
03 =4B 
Mol. wt. of Na2C03 106 
One-half the mol. wt. = 53 
200 c.c. : 1 c.c. == 10.6 grms.: 0.053 grros. 
This solution serves to standardize the sulphuric acid. 
Standardizing the Sulphuric Acid.—Take of the Na2C03 
solution, 20, 30, or 40 c.c., accurately measured, place in a 
wide-mouthed flask of about 300 c.c. capacity ; add litmus 
solution, and run in H2S04 solution from a burette until 
a wine-red color is obtained; boil hard to expel C02, and 
add more acid until the color is permanent. Read off the 
c.c. used. Repeat the process. Suppose 30 c.c. Na2C03 
solution required 25 c.c, H2S04 solution. Then 5 c.c. 
(30 25) water must be added to every 25 c.c. of the acid 
solution to make it normal. Measure, therefore, the 
H2S04 solution carefully and add the necessary amount of 
water. Suppose the H2S04 solution measures 900 c.c., 
since 900=25X36, then 36 X 5, or 180 c.c. water must 
be added. Add the water, mix well, and again determine 44 
QUANTITATIVE ANALYSIS. 
the standard : one c.c. of the Na2 C03 solution should ex- 
actly neutralize one c.c. of the H2S04 solution. In case of 
difficulties the exact standard of the acid should be deter- 
mined gravimetrically by precipitating 10 or 20 c.c. with 
BaCl2, and calculating from the BaS04 obtained the 
amount of H2S04 in one c.c. 
Carminic acid being stronger than carbonic acid, a solu- 
tion of cochineal is sometimes substituted for litmus, in 
which case boiling may be dispensed with. The dyestuff 
tropaeoline has recently been proposed as an indicator in 
alkalimetry. Cf. Ber. d. chem. Ges. XI, 460 (1878). 
Dcci-normal Solution of Acid.— Call the above normal 
solution “No. Itake 100 c.c. of No. 1, put into a litre 
flask, and dilute to one litre. Call this deci-normal solution 
“ No. 2.” 
A.—Valuation of Soda Ash. 
(Determination of Na2C03.) 
Place about 12 grms. powdered sample in a platinum 
crucible or porcelain dish ; heat moderately for some min- 
utes over a Bunsen burner, until all moisture is expelled; 
cool, weigh out exactly 10 grm.; dissolve in water; dilute 
to one-half litre and mix well. Take out 50 c.c. solution 
(which contains one grm. soda ash), and determine the 
amount of normal acid needed to neutralize, adding litmus 
as before, and boiling to expel C02. 
Suppose 50 c.c. solution soda ash required 15 c.c. stand- 
ard acid, then lO° = 79-5 Per cent. Na2C03. 
See Fres., § 195, p. 692. These results are only 
approximative and preliminary, and the operation must 
be repeated, finishing with the deci-normal solution No. 
2, as below. Take another 50 c.c. of soda ash solution; 
run from a burette 12 c.c. of solution “No. 1,” and then ACIDIMETRY. 
45 
finish with solution “No 2.” Of course, in calculating, 10 
c,c. of No. 2 equals one c.c. of “ No. i.” 
B-— Valuation of Pearl Ash. 
Proceed as before; weigh quickly the salt cooled in a 
desiccator, for it is very hydroscopic. In calculating, use 
the factor 0.0691. 
The Residual Method of Titration.— This method has 
great advantages over the foregoing method, especially 
when carbonates are in question ; the sharpness of the end 
reaction being much increased by the absence of C02. 
The process is as follows: Super-saturate the soda ash 
solution with normal acid in excess; then add normal pot- 
assic hydrate (and decinormal also) until the neutral point 
is reached. (The normal KHO is mentioned in the next 
paragraph.) Since one c.c. acid = one c.c. alkali, substract 
the number of c.c. of standard alkali from the number c.c. 
of standard acid added in the first place, and then calculate 
as usual. 
Acidimetry. 
Generalities.—The value of strong acids, especially HCI, 
HN03, H2S04, is frequently deduced from the Specific 
Gravity as determined by the hydrometer. See tables in 
Fres., pp. 690, 691, showing percentages of acids in solu- 
tions of different densities. When titration is desirable, 
standard KHO solution is used, and in accordance with 
the principles already stated. 
Preparatioit of Standard Alkali.—Take about 60 grms. 
KHO, dissolve in 1 litre of water, add Ca(HO)2 to throw 
down carbonates, boil, let settle, and syphon off. Deter- 
mine the exact standard of this with normal and deci- 
normal acid. 46 
QUANTITATIVE ANALYSIS. 
A.—Valuation of HCI. 
Take 5 to 50 c.c. acid, according to strength, dilute to a 
definite volume, take an aliquot part, add litmus and run in 
the standard KHO as described. 
In calculating multiply the number of c.c. of KHO 
added by .0365 X 100, and divide this product by the num- 
ber of c.c. of acid taken X Specific Gravity of the solution 
as determined by the hydrometer. 
Example.—Took 10 c.c. HCI solution, having a Specific 
Gravity = 1.025 » since 1 c.c. of water weighs 1 grm., the 
weight of acid taken 10.25 grms. 
The acid solution required 8 c.c. KHO, whence 
8 X .0365 X 100 
= 2.84 per cent. 
10.25 
B.—Analysis of Vinegar. 
A. Determine the acetic acid by titration, using cochi- 
neal solution, or with methylaniline violet, as in the “ Witz 
method” {Am. Chem., Vol. VI, page 12), or use Mohrs 
method, as follows: 
Add to a known quantity of acid a weighed quantity 
(in excess) of pure precipitated dry CaC03. After de- 
composition is nearly complete in the cold, boil to expel 
C02, filter, and wash the excess of CaC03 in hot water. 
Dissolve the CaC03 in excess of normal HCI, and deter- 
mine the HCI remaining by means of normal KHO, or 
NaHO and litmus solution. The results with dark 
colored vinegars are good. 
B. Determine water by drying at 1000 C. to constant 
weight, and allow for alcohol and acetic acid. CHLORIMETRY. 
47 
C. Determine alcohol by neutralizing about 300 c.c. 
vinegar with CaC03 and distilling off some measured 
amount, say 150 c.c. Then determine specific gravity by 
weighing, and from this calculate the per cent, of alcohol. 
D. Determine the grape sugar. (See Analysis No. 33.) 
Analysis No. 13.—Chlorimetry. 
Constitution of Bleaching1 Powder. 
Bleaching powder is formed thus : 
2CaH202 + 2C12 = 2H20 + CaCl202,CaCl2. 
The composition of bleaching powder is variously given. 
The following are some of the formulae. 
“ Quelques Chimistes,” CaCI2 + H202. 
Watts, CaCIO -f- CaCl, Ca20 -{- 2H20. 
Bloxam, CaO C120 CaCl2 2CaO -f- 4H20. 
Roscoe, CaCl202. 
Muspratt, CaO Cl2 2H20. 
Fownes, CaCl2 -j- CaCl202. 
Calvert, 2CaCl2 -f- CaCl202. 
Thorpe, Ca3H606Cl4 = CaCl202 -f- CaH202 -f- CaCl2 -f- 
-2H2O. 
Kolb, (2Ca0,C12H20), CaH202. 
Rose, (CaCl2, Ca202) Ca02Cl2 + 4H20. 
Stahlschmidt’s theory of its formation; Bericht D. 
Chem. Ges., 1875 : 
3CaH2O2 + 4CI = CaCl2 -f CaCl2o2 + CaH202 -f 2H20. 
See paper on Constitution of Bleaching Powder, by Dr, 
Lunge in American Chemist, Vol. V, page 454. 48 
QUANTITATIVE ANALYSIS. 
When allowed to stand in contact with air and light, it 
decomposes, CaCl2 increasing, and the CaCIO decreas- 
ing. Dry chloride of lime, at 50° C, decomposes thus : 
(Thorpe.) 
3Ca3H606C14 = SCaCI2 + Ca(ClO3)2 + 3CaH2O2 + 6H20. 
By the action of water chloride of lime decomposes 
thus: 
Ca3H606Cl4= CaH202 + CaCl2 + CaCl202 + 2H20. 
The value of the commercial article depends wholly 
upon the amount of “ available chlorine,” viz.: the Cl in 
the hypochlorite, which is thus constantly varying. 
The strongest contains 38.5 per cent available chlorine. 
One or two per cent, of this is present as calcium chlorate, 
which is without bleaching power. 
Action of Acids on Bleaching Powder. Action of hy 
drochloric acid: 
(CaCl2o2 + CaCl2) + 2HCI = 2CaCl2 + 2(HC10). 
Action of dilute sulphuric acid: 
(CaCl202 + CaCl2) + H2S04 = CaS04 + CaCl2 -f 
2(HC10). 
Further action of concentrated sulphuric acid: 
CaS04 + CaCl2 + 2(HC10) + H2S04 = 2(CaSO4) -f 
4CI + 2H20. CHLORIDE OF LIME. 
49 
Valuation of Chloride of Lime. 
Penot's Method. From Fresenius’ Quant. Analysis, 
§ 200. Based on the conversion of an alkaline arsenite. 
into an arseniate by a solution of chloride of lime. 
As203 + CaCl202 = As205 ~f- CaCl2. 
The end reaction is determined by KI and starch, un- 
decomposed hypochlorite turning this mixture blue. 
(a.) Preparation of KI Starch Paper. Boil three grms. 
starch, in 250 c.c. water, add one grm. KI, one grm. 
Na2C03 -j- aq.; dilute to 500 c.c. Moisten paper with 
this solution and dry. 
(b.) Preparation of Solution of As203. Dissolve ex 
actly 4.95 grms. pure sublimed As203 with 25 grms. 
Na2CQ3 aq. (free from S) in 200 c.c. water. Boil until 
dissolved and dilute to one litre. Make a solution. 
10 
Since it is difficult to weigh out exactly this amount, take 
any number and dilute proportionately. If 5.013 grms., 
then 
4-95 : 1000= 5.013 grms, : 1012.7. 
Add then 12.7 c.c. to the litre. One c.c. of this solu- 
tion = 0.00355 Cl. 
(Ic.) Process of the Determination. Mix sample well; 
weigh out 10 grms., rub in mortar with 50 or 60 c.c. water; 
settle; decant turbid liquid into a litre flask. Repeat. 
Fill up to mark, and mix. 
Fill a burette, take 50 c.c., run it into a beaker, add the 
standard As203 solution, stirring until a drop of the so- 50 
QUANTITATIVE ANALYSIS. 
lotion no longer gives a blue mark on the KI starch paper. 
Repeat on fresh amount. Caution: Shake, and draw off 
turbid liquid. 
(d.) Calculation. 
c c. As20, solution usedXo.oo3ss X 100 „ 
* = per cent. Cl. 
Amount taken 
[French chlorimetrical degrees represent the number of 
litres of Cl at o.°C. and 760 m.m,, which one kil. of sample 
should yield. Now one litre of Cl weighs 3.177 grms.; 
hence 31.77 per cent. = 100 degrees. See foot-note on 
p. 700 of Fres. Quant. Anal.] 
The amount of calcium chloride present may be de- 
termined by first estimating the hypochlorite as above, and 
then adding to the second portion of 50 c.c. a slight excess 
of NH4HO and warming. 
3 CaCl202 + 4 NH3 = aCaCI2 + 6H20 + 4N. 
Neutralize the solution with HN03 and determine the 
Cl by AgN03. 
The amount of chlorate may be determined by heating 
a third portion with ammonia, then acidulation with pure 
H2S04 and digesting with Zn. 
Ca(ClO3)2 -f 12H = CaCl2 + 6H2Q. 
Again determine the Cl by AgN03, and the increased 
amount over the second determination gives the Cl exist- 
ing as chlorate, (Thorpe.) TYPE METAL. 
5i 
Analysis No. 14. — Type Metal. To be determined Pb, Sb, Sn (Zn and Fe?). 
Dissolve about 1 grm. clippings in moderately cone. HNO,, adding enough H„C4H40„ to hold up the antimony, 
and heating gently. Digest and add acid until all but the SnO„ is dissolved. * See Fres., § 164, 14, b. Expel 
excess of HNOs by concentration of liquid, but not to dryness. Filter and wash. See Note 1. 
Residue a. 
Sn02 (+Sb?) 
Dry, ignite, 
and weigh. 
Test for lead. 
Solution a. 
Sb, Pb, Zn (Fe). Add H,S04 and evaporate to small bulk, add alcohol and let stand 
12 hours. See Fres., § 116, 3, a, a, and § 83, d. Filter and wash with water containing a little 
H.SO,, and then changing recipient of filtrate, wash thoroughly with alcohol. Be careful to 
expel all HsSO, from filter. 
See Fres., 
§ 126, 1, a, and 
§ 9li «• 
See also Note 
2, below. 
Precipitate b. 
PbS04. 
Dry, ignite in 
Filtrate b. 
Sb, Pb, Zn (Fe). Saturate with H2S gas, warming solution with a current 
of steam. Filter and wash. See Fres., § 164, A, 1. 
porcelain, and 
weigh. 
See Fres., 
§ 83, d. 
Solution c. 
Zn and Fe. 
(To determine 
Precipitate c, . 
Sb.jS, -(- PbS. Digest with yellow NH4HS, filter, repeat 
digestion, filter and wash. See Fres., § 164, 14, b. 
these, throw 
down Fe as 
basic acetate, 
Residue d, 
PbS, oxidize 
with HNO?j, 
dry, ignite, and 
weigh as PbS04. 
Solution d. 
Add excess of HC1 and wash. 
and Zn as car- 
bonate. Fres.. 
§ 10S, 1, a, and 
§ 77> «•) 
Solution e. 
NH4C1. 
Reject. 
Precipitate e. 
Treat precipitate of Sb,S3 -f- S 
on filter (to remove S), by wash- 
ing with CS2, transfer to a 
weighed porcelain crucible, add 
fuming HN03, heat, add more 
acid, evaporate to dryness, ig- 
nite, and weigh as Sb204. If dark 
colored add more HN03, heat, 
ignite, and weigh again. Fres., 
§ 125, 2, b, a. See Note 1. QUANTITATIVE ANALYSIS. 
Note 1. Some of the tin may go into solution as 
nitrate of tin, if the nitric acid be dilute, and thus appear 
in Precipitate c mixed with the sulphide of antimony; in 
this case they should be separated by F. W. Clarke’s 
method, which is based on the solubility of the sulphide 
of tin in oxalic acid, and details of which may be found in 
Crookes’ Select Methods, page 249. For another method 
see Fres., § 165, 4, a, also § 165, 7, a. 
Note 2. —On the other hand, some of the antimony 
and lead may refuse to dissolve and remain with Residue a, 
in which case proceed as follows : after igniting and weigh- 
ing the Sn02 -f Pb? -f Sb ? fuse with Na2C03 and sulphur 
in a porcelain crucible. Dissolve in warm water and filter 
from the residue of PbS, which may be treated with HN03 
in a porcelain crucible and weighed as PbS04. To the 
alkaline solution add slight excess of HCI and collect 
precipitate of SbS3 + SnS2 -j- Son filter; dry and remove 
excess of S by washing with CS2, transfer to porcelain 
capsule, oxidize with PIN03 evaporate to dryness, fuse 
with NaPIO in a silver dish, dissolve the mass in a mixture 
of three volumes of alcohol and one of water, and filter 
from the antimoniate of sodium. For details, see Fres., 
§ 165, 4, a To the solution containing stannate of sodium, 
add HCI, saturate with H2S, and treat the precipitated 
SnS2 as usual. See Fres., § 126, I, c, and § 91. 
Consult article on the Estimation of Antimony, by E. 
H. Bartley, in American Chemist, Vol. V, page 436; also 
paper by Dr. Clemens Winkler, in Fresenius’ Zeitschrift 
fur Analytische Chemie, PI eft 2, 1875. DETERMINATION OF ZINC. 
53 
Analysis No. 15.—Zinc Ore, 
Pulverize finely; heat about 2 grms. ore with 10 c.c. 
Boil till fumes of H„S04 appear. Cool, add IIaO carefully, 
Determination of Zinc. 
HC1 -f 5 c.c. HN03 -f- 10 c.c. H,S04 in a flask, 
warm and filter, wash thoroughly. 
Residue a. 
Si02 + PbS04, 
CaSOt, etc. 
Solutio?i a. 
Nearly neutralize with cryst. Na2C03, dilute, add NaC2H302 (about 5 grms.), boil ten 
minutes and filter hot. Wash hot by decantation. See Note 1 below, and Fres., § 113, 1, d. 
Testfor zinc, and. 
if found, treat again 
with acid. 
Precipitate b. 
Fe203 + A1203 as 
basic acetates. 
Filtrate h. 
Add Br water to the liquid, and digest for some time. Repeat so long 
as Mn02 is precipitated. Fres., § 159, 4. a. 
Precipitate c. 
Mn02 + xH20. 
Filtrate c. 
Expel Br by boiling, add a little IIC2II302, saturate 
with H2S gas. wash the ZnS with II,S water on the 
filter, carefully covering the funnel with a watch-glass. 
Cf. Fres., § 108, 1, b. See Note 2. 
Filtrate d. 
Examine carefully for 
Zn, and if present repeat 
as with Filtrate c. 
Precipitate d. 
Dissolve on filter with 
warm dilute HC1, add a 
very little KCIO, boil to 
oxidize the ZnS, filter from 
S if necessary, and add 
Na2COs. Fres., § 108, 
1, a. and § 77. Wash, dry, 
ignite, and weigh as ZnO. 
Note 1.—For the precipitation of Fe as basic acetate, the solution must be very carefully neutralized with 
crystallized Na2C(D3, ending with a dilute solution of Na2COs, and striking as deep brown-red a color as possible. 
Cf. Note 11, Analysis No. 21. 
Note 2.—For properties of ZnS and various methods of determining Zn, see article by Hugo Tamm in 
American Chemist, Vol. II, p. 298. 54 
QUANTITATIVE ANALYSIS, 
Analysis No. 16. — Chromic Iron Ore. Scheme I. 
May contain FeO, A1203, Cr„03, Mn203, CaO, MgO, bi02(Ti02). 
Fuse 0.5 grms. ore, ground to an impalpable powder, in a large platinum crucible with 6 grms. KHS04 for 
twenty minutes; add H2S04 from time to time, and fuse again at a higher temperature. Add 3 grms. pure 
Na2C03 and 2 grms. NaN03, adding the latter in small portions at a time during an hour, at red heat, then heat 
fifteen minutes to bright redness. A little KHO added to this fusion facilitates it. Cool, remove the mass from 
the crucible with hot water, filter hot, and wash the residue. Fres., § 160, 8, a. 
Residue a. 
Filtrate a. 
Digest with HC1, 
and filter from res- 
idue. 
Evaporate with excess of NH4N03 on a water-bath nearly to dryness, and heat until 
all free NH4HO is expelled. Add HaO, digest, and filter. Fres., § 160, 8, «, 77- 
The HC1 solution is 
rejected. 
If much undecom- 
posed ore remains, fuse 
again as before. 
Residue b. 
A1203 S i O ,(T i O „) 
Mn203, also Cr203. 
Re-fuse and treat as 
before. Add second 
. Filtrate b. 
Boil with HC1 and alcohol, expel excess of alcohol; when 
fully reduced add NH4HO, boil, filter hot, wash thoroughly by 
decantation. Fres., § 106, x, a. 
filtrate to filtrate b. 
Filtrate c. 
Precipitate c. 
' 
Reject if colorless, 
or contains no Cr2Os. 
Cr203. Dry, ignite, and weigh. 
Fres., § 76. CHROMIC IRON ORE. 
55 
Analysis No. 16.—Chromic Iron Ore. Scheme II. 
Pulverize very finely, take 0.5 grm., fuse as in Scheme I. Dissolve in water and filter. 
Residue a. 
FeaOs, A1203, undecomposed ore, etc. Treat with 
HC1, digest, filter, and wash. 
Filtrate a. 
Contains Na2Als04, Na2Cr04, Na2Mn04, Na3SiOs, etc. 
Add (NH4)2C03, and heat nearly to boiling. 
Filtrate b. 
Fe203, etc. 
Reject. 
Residue b. 
If not very small in quantity, 
must be re-fused as before and 
added to filtrate a. 
Residue c. 
Al203Si03, etc. 
Filtrate c. 
Na2CrO, solution must be yel- 
low. Neutralize with UNO,, 
and add a neutral solution of 
Hg(N03)2. Wash the precip- 
itate with dilute solution of 
Hg(NOs)2. Dry, ignite the 
HgCr04, and weigh the Cr203 
resulting. 
For other methods, see Fresenius’ Quant. Analysis, § 106, 2 d. Consult also paper by E. 
F. Smith, in American Journal of Science, [3] xv, p. 198. 56 
QUANTITATIVE ANALYSIS. 
Analysis No. 17. Pyrolusite. 
Determination of Mno2. 
Employ P'resenius and Will’s method as described in 
Fres. Quant. Analysis, edition of 1881, pages 705-709, 
§ 203, A. See also Mohr’s Titrirmethode § 215, pp. 617- 
638 (ed. 1874). 
Take 3.955 grms. of ore, and use Geissler's carbonic 
acid apparatus if available. 
Consult also the following article: “On the Estimation 
of Peroxide of Manganese in Manganese Ores,” by E. 
Scherer and G. Rumpf, Chemical News, American Re- 
print, Vol. VI, page 82, February, 1870. 
Analysis No. 18. Feldspar. 
A-— Determination of Alkalies. 
Prof. J. Lawrence Smith’s method. See Am. J. Sci. 
[3] I, 269. Also Fres., § 140, 11, b, y. 
Pulverize well in an agate mortar. Weigh out one grm. 
of the silicate. Mix well in an agate mortar, first, with 
about one grm of NH4CI (pure enough to sublime without 
residue), and, secondly, with about eight grms. C. P. pre- 
cipitated CaC03; add the latter in three or four portions, 
mixing well after each addition. Transfer the mixture by 
means of glazed paper to a platinum crucible. 
Apply the heat of a Bunsen burner to the upper portion 
of the crucible first and gradually carry the flame toward 
the lower part, until the NH4CI is completely decomposed, 57 
DETERMINATION OF ALKALIES. 
which ensues in four or five minutes. Then heat before 
the blast-lamp, not too intensely, for thirty to forty min- 
utes. 
This operation is greatly 
facilitated by using a special 
apparatus devised for the pur- 
pose by Prof. J. Lawrence 
Smith, and represented in 
Fig- 5- 
The stand H supports on 
its rod G a cast-iron plate B 
perforated by a hole large 
enough to admit the some- 
what elongated crucible A; 
the bottom of the crucible 
projects within the sheet iron 
chimney C which is held in 
its place by the hook N, 
When heat is applied to the 
bottom of the crucible by the 
flattened burner F the decom- 
Fig. 5. 
position proceeds regularly and is completed in about one 
hour. 
Cool the crucible, place it in a porcelain casserole, and 
digest the semi-fused mass with boiling water until tho- 
roughly disintegrated. This may take some hours. Then 
filter from the residue (Sio2, Fe203, A1203, Mn203(?), 
CaO, etc.), and wash well with about 200 c.c. of water. 
All the alkalies of the silicate are converted into chlorides 
and are now in the water solution. Add to this solution 
NH4HO and (NH4)2CO3 with a few drops of (NH4)X2O4. 
Evaporate without filtering, on a water-bath, to about 50 
c.c., add a little NH4FtO, and filter through a small filter 
(No. 2) into a weighed platinum dish. Evaporate to dry- 58 
QUANTITATIVE ANALYSIS. 
ness on a water-bath, ignite very gently to drive off a little 
NH4CI, and weigh. If the residue is not perfectly soluble 
in water, and quite white, dissolve, filter off, evaporate, 
ignite, and weigh again. This gives the weight of the 
KCI + NaCl. 
Next determine the K, either by separating it with PtCl4 
and alcohol in the usual manner, or by gravimetric or vol- 
umetric estimation of the total Cl in the weighed chlorides. 
For calculation, see Fres., page 841, 3, a. Consult also 
Crookes’ Select Methods, pages 13 and 14. 
B. Determination of Si02, ALO3, Fe2Oa, CaO, 
and MgO. 
Fuse two grms. mineral with six grms. K2C03 -f- six 
grms. Na2COs. Moisten with water, digest, add excess of 
HCI, evaporate to dryness, expel HCI in air-bath, add 
water and HCI, and filter from SiOz. Continue exactly as 
in Analysis No. J. SOLUBLE SILICATES. 
59 
Appendix to Analysis No. 18. — Analysis of Soluble Silicates. 
May cbhtain Si02, A1203, FeO, CaO, MgO, Na20, K20, H20. Pulverize, weigh out four grms., moisten 
with water in casserole, add cone. HC1, evaporate to dryness on water-bath. Dry in air-bath at ioo°-ii5° C. 
Moisten with HC1, add water, digest, and filter. 
Residue a. 
Si02, dry, ig- 
nite before the 
blast lamp, and 
weigh. 
Oxidize the FeO if necessary, 
Solution a. 
dilute to 400 c.c., and divide into two equal portions. 
Solution a}. 
200 c.c. De- 
termine A1203, 
Fe2Oa, CaO and 
MgO, exactly as 
in Analysis No. 
7, Dolomite. 
Solution a‘!, 200 c.c. 
Add solution of Ba(HO)2 in excess and filter. Fres., §153, B, 4, a, a. 
Residue a. 
A1A, Fe,Os, 
MgO, etc. Re- 
ject. [Fe may be 
determined here 
volumetrically.J 
Solution b 
Add (NH4)2COs, boil and filter. 
Residue c. 
CaC03 BaCO„ 
etc. Reject. 
Filtrate c. 
Add HC1 cautiously. Evaporate to 
dryness, and heat gently over Bunsen 
burner until all NH,C1 is expelled. 
Dissolve residue in water, filter into 
weighed dish. Evaporate, dry, ignite, 
and weigh as NaCl-|-KCl. Dissolve 
in water and determine K directly as 
K2PtCl„, or indirectly by estimation of 
Cl, in the mixed chlorides. See Fres., 
p. 841, 3, a, for calculation. QUANTITATIVE ANALYSIS. 
Analysis No. 19. Iron Slag. 
To be determined: Si02, FeO, MnO, A1205, CaO, 
MgO, S, P2Os. 
Pulverize finely; weigh out exactly five grms.; mix 
011 glazed paper, by means of a horn spatula, with 
fifteen grms. anhydrous Na2C03 and fifteen grms. K2C03, 
together with one grm. NaN03. These fluxes need not 
be accurately weighed. Put one-third the mixed slag 
and fluxes into a two-ounce platinum crucible, and heat 
over a Bunsen burner until by settling down room is 
made for more. Heat twenty minutes or more before 
the blast-lamp. Cool suddenly, place in a casserole, 
and treat with boiling water until thoroughly disinte- 
grated. Remove the crucible and add excess of PI Cl 
little by little, avoiding loss of liquid by violent efferves- 
cence; evaporate to dryness on water-bath, expel HCI 
completely by drying (not above 1150 C.) in an air-bath. 
Moisten with water, add HCI, digest, and proceed as per 
scheme on following page. IRON SLAG. 
6i 
Filter the solution obtained as directed on page 60. 
Residue a. 
Si02. Dry, ig- 
nite, and weigh. 
N.B. — Check 
Si02 by fusing i 
grm. slag as a- 
bove and follow- 
ing details there 
given. 
Filtrate a. 
Dilute to 500 c.c. and divide into three portions. 
Solution a1. 
100 c.c. 
AddBaCl,and 
treat the BaS04 
in the usual 
manner. 
Report S. 
Filtrate from 
BaSO* may be 
kept for deter- 
mining Fe in 
case of accidents. 
Solution a'2. 
100 c.c. 
Add excess of 
NH4HO, wash, 
dissolve in 
H2S04, and de- 
termine the Fe 
with K2Mn2Os. 
Cf. Note iS, 
Analysis No. 21. 
Solution a3. 300 c.c. 
Cool, nearly neutralize (in a large flask) with cryst. 
Na2CO, + 10IRO, add about 15 grms. NaC2H302. dilute to 
about 2 litres, heat to boiling, and filter hot. Wash well. 
See Note 11 to Analysis No. 21. 
Precipitate b. 
Fe203-j-Al303as basic acetates; also 
P205. Wash, dissolve in strong HC1, 
and divide into two unequal portions. 
Filtrate b. 
Mn, Ca, Mg. 
Proceed exactly as 
in ''''Filtrate g,” 
in Analysis No. 
21, Scheme II. 
Omit, however, 
the treatment with 
Br. if Mn is known 
to be wanting. 
Solution bx. f. 
To determine 
P20, proceed ex- 
actly as with ''•So- 
lution gx” in A- 
nalysis No. 21. 
Solution b2. -Jj. 
To determine 
A1203 proceed ex- 
actly as with 11So- 
lution g2” in A- 
nalysis No. 21. 
Note. — If the slag contains much manganese, the solution of the fused mass will be strongly colored green 
from the formation of sodium and potassium manganates; on boiling this solution it becomes of a violet color in 
accordance with the following reaction : 3K„Mn04 -4-311,0 — MnO„II20 -f- K,Mn,08 -f-4KHO. 
On adding HC1 to the permanganate solution it loses its color owing to following reactions : 
KJMn808+8HCl=3(Mn02HJ0)+2KCl-f2H,0-j-6Cl, and Mn0„H80-f4llCl=MnU.J+:,H,0-f-20’ 63 
QUANTITATIVE ANALYSIS. 
Analysis No. 20.—Hematite. 
Determination of Fe, SiOj, S, and p.—Pulverize very finely, and weigh out on a watch-glass exactly 5 
grms., mix on glazed paper with 25 grms. pure Na2C03-{-2 grms. NaNOs and fuse in 2 oz. platinum crucible. 
(Consult Note 2. Analysis No. 21.). Cool suddenly, place in a casserole, and treat with boiling water until 
thoroughly disintegrated. Remove the crucible (Note 3, Analysis 21), and add carefully excess of HC1. Evapo- 
rate to dryness on water-bath, expel HC1 in air-bath at no0-ii5° C. Add HC1, digest, dilute, and filter. 
Residue a. 
Filtrate a. 
Si02. Dry, ignite 
thoroughly, and 
Dilute to 500 c.c., and divide into 3 portions. 
weigh. 
If not white after 
ignition repeat the fu- 
sion and treat as be- 
fore. 
Solution a1. 
100 c.c. 
Determine S as BaS04 in 
the usual manner. 
The filtrate from BaS04 
may be reserved for dupli- 
cating the Fe. 
Solutioti a2. 
100 c.c. 
Add excess of NH4HO, 
wash to remove NH4C1, do 
not bring on filter, dissolve 
in H2S04, reduce and deter- 
mine Fe by K2Mn208. 
See Note 18, Analysis No. 
21. 
Solution a3. 
300 c.c. 
Add NH,HO in excess, 
and proceed for determina- 
tion of P exactly as with 
“solution g” in Analysis 
No. 21, 
Quick Method for the Determination of Iron only.—Sample, pulverize, fuse 1 grm. Na2C03X 1 grm. 
NaN03 about 20 minutes. Plunge crucible while hot into cold water in a casserole; boil, and after removing 
crucible neutralize carefully (C02 escapes) with cone. H2S04; add excess of acid, filtrate, if much remains undis- 
solved, dilute to 500 c.c., divide in halves, reduce with amalgamated zinc and platinum foil, and titrate with 
K2Mn208 as usual. See for details of the latter steps, Notes to Analysis No. 21, Scheme II. TITANIFEROUS IRON ORE, 
63 
Analysis No. 21.—Titaniferous Iron Ore. Scheme II.-* 
Prepare an average sample for analysis. (Note i.) Pulverize in an agate mortar to an impalpable powder. Make 
a qualitative examination for H,0— Ti02— Cu — 
As and Cr. If Cu — As or Cr are present, see Scheme I. 
To be determined: TiO,— Si02 — Fe- 
-ALO3 —Mn-CaO-MgO —S-P —HsO. 
Weigh out exactly 5 grammes, mix with 20 to 30 grammes Na2COs and 2 to 5 grammes NaNO,, and fuse in a 
platinum crucible. (Note 2.) Cool suddenly, place in a casserole and treat with boiling water until the mass is 
thoroughly disintegrated. (Note 3.) Filter and wash with hot water. {Note 4 and Fres., § 160, 8, a.) 
1. Water Solution. 
It must be perfectly clear but may be colored 
and may contain Si02 — SO, — P2Oc — and ALO,- Add 
carefully an excess of I1C1, evaporate on water-bath to dryness, heat in an air-bath at ioo° C. to 115° C. till odor 
of HC1 is no longer perceptible. {Note 5.) Moisten residue with HC1, add water, digest, filter, and wash hot. 
Residue a. 
Filtrate a. 
SiO, To be added 
to and re-fused with 
Dilute to 500 c.c. and divide into three portions. 
Residue b. 
Solution a1—300 c.c. 
Solution a2— 100 c.c. 
Solution a3 — 100 c.c. 
Put into a large flask to 
be afterwards combined with 
Filtrate f. 
Add BaCl2 and determine 
H2S04 as BaSO., {Note 8 
and Fres., § 132.) 
Add to Solution F, as a 
little Fe often enters the 
water solution. 
•Scheme I may be found in A merican Chemist Vol. I, p. 323. Both schemes are modifications of one originally drawn up by Dr. C. F. Chandler, 
(See preface to this work.) 64 
QUANTITATIVE ANALYSIS. 
2. Insoluble Residue. 
It may contain SiO,—TiOa—P2Or,—Fe203—A1203— Mn,Os—CaO—MgO (and Pt from the crucible). 
Dry the residue on the filter, transfer to a casserole, burn the filter and add the ashes. Moisten with water, add 
cone. HC1, evaporate to dryness, heat till HC1 is expelled; add cone. HC1, then water. (Note 9.) Digest with 
occasional stirring, filter, and wash. (Fres., § 140.) 
Residue b. 
Contains Sl02—Ti02, 
etc. Combine with Residue 
a, fuse with 5 parts Na2COs, 
remove fused mass from 
crucible with hot water, acid- 
ulate with HC1, evaporate to 
Filtrate b or Hydrochloric Acid Solution. 
Combine with Filtrate c. Dilute to 500 c.c. and divide into 3 portions. 
Solution F—300 c.c. 
Saturate thoroughly with H2S gas and filter from 
the PtS3 and S. 
Solution b'2. 
100 c.c. 
Combine with 
Solution 
F. 
100 c.c. 
dryness not above ioo° C. 
{Fres., § 140, II, a.) Add 
HCland boiling water, filter 
Filtrate e. 
Boil with KCIO3 to oxidize FeO. 
Solutions a3 and d2, 
add excess of 
NH4HO, wash by 
To be 
combined 
with solu- 
ana vvasn. 
Filtrate f. 
Cool, combine with Solutions a1 and dl in large 
flask. Add Na.CO, almost to neutralization and 
about 20 grammes sodic acetate, dilute to about 2.5 
litres, and boil ten minutes. (Note 11 and Fres., 
§ “3, 1, d.) 
decantation twice, 
dissolve in H2S04. 
dilute largely, part- 
ly neutralize with 
Na2CO„, saturate 
with H„S gas, boil 
5 to 7 hours, adding 
water and II2S wa- 
ter, filter and wash. 
(For ppt. h and fil- 
trate k see next 
page.) 
t ion d3 
Residue c. 
Dry on fun- 
nel, fuse with 6 
parts KHS04; 
dissolve in about 
Filtrate c. 
Add this 
filtrate and 
washings 
to Filtrate 
b. 
and re- 
served for 
accidents. 
300 c.c. com 
ter. filter 
wash cold. 
wa- 
and 
Precipitate g. 
Contains Pe203 and 
ALO3 as basic acetates 
and perhaps P,Ob and 
Ti02. Wash thorough- 
ly, dissolve in strong 
HC1 and divide into 2 
portions, g1 and g2. 
Filtrate g. 
Contains Mn—Ca and Mg’. 
Concentrate to small bulk, 
add Br, digest until excess 
of Br is expelled, filter and 
wash. (Fres., § 109, 1, d.) 
(For ppt. h and filtrate h 
see next page.) 
Residue d. 
Dry. ig- 
nite and 
weigh as 
SiOa. 
Filtrate d. 
Dilute to 500 
c.c. and divide 
into 3 portions. 
dl, d- and da. TITANIFEROUS IRON ORE. 
65 
Solution 
Solution 
Solution 
Solution 
Solution 
Fred pi- 
Filjrate h 
Precipi- 
Filtrate k. 
d1 
d3 
d3 
S' X- 
g2 H- 
tate h. 
Contains Ca and Mg. 
tate k 
Expel the 
300 c.c. 
Add to 
100 c.c. 
Add to 
1 JO c.c. 
Add to 
Add NH4HO 
in iarge excess, 
wash twice by 
decantation 
and re-dissolve 
Add 
(NH4)HO 
D i s- 
solve in 
Add NH4HO NH4C1 
and (NH4)2C304, let 
stand 12 hours, filter 
Consists 
of TiO,. 
H2S by boil- 
ing with 
Filtrate 
Solution 
Solution 
in excess to 
HC1 on 
and wash hot. 
Dry, ig- 
nite and 
KCIO,, 
/• 
b* 
b3 
precipitate 
filter and 
Precipi- 
Filtrate 
co n c e n 
- 
inconc.HN03. 
Fe,0,-f-Al,- 
wash. 
tate i. 
i. 
weigh. 
trate fil 
Boil down to 
o;+p„o; 
Boil, add 
If dark 
ter, dilute 
small bulk, add 
V+TiOa). 
Na„CO, 
Dissolve 
Add 
colored. 
to soo c. c. 
NH4N03 and 
Boil till all 
in ex- 
ppt. in 
NH4HO 
fuse with 
and divide 
50 c. c. 
(NH4),Mo04 
+HNO,). 
free NH, is 
expelled, 
filter, wash 
thoroughly, 
cess, 
boil, ftl- 
HC1. re- 
precipi- 
tate with 
NHiHO 
and 
Na2HP04. 
let stand 
6 pts.' 
khso4, 
into 2 por- 
tions. 
Warm and set 
aside 24 hours. 
ter and 
was h. 
12 hours, 
filter. 
dissolve 
in cold 
Solution 
k'. 
Solution 
k'1. 
Filter, test fil- 
trate, wash 
with the diluted 
precipitant {% 
and %). Dis- 
solve ppt. in 
NH4HO in 
original beak- 
er, filter 
through same 
filter, add 
magnesia 
mixture” and 
determine 
P2Os as usual. 
(Free., § 134 
dry, ignite 
and weigh. 
(Fres. § ioc 
and §113,1, 
a, and Note 
13.) From 
this weight 
deduct P20n 
found in g1, 
together 
with the 
Fe203calcu- 
lated from 
P and TiO, 
Dry ig- 
nite and 
weigh as 
Mn304 
(Fres., 
§ 109, 
1. a.) 
(Com- 
pare 
Note 
16.) 
wash 
(add fil- 
trate to 
filtrate 
/.) Dry 
ppt., 
burn fil- 
ter sepa- 
rately, 
moisten 
with 
H2S04in 
crucible 
wash,dry 
and 
ignite. 
Weighas 
Mg2P207. 
(Fres., 
§ 104, 2.) 
water, 
filter and 
reprecip- 
itate by 
boiling, 
filter, 
wash, ig- 
nite and 
weigh 
again as 
TiO,. 
(Fres,, § 
107.) 
See Sun- 
Reduce 
the 
Fe,03 
by amal- 
gamated 
Zn and 
Pt foil 
and de- 
termine 
Fo 
volumet- 
rically by 
Margue- 
Treat in 
exactly 
the same 
way as 
solution 
P and 
average 
the re- 
sults. 
(Com- 
pare 
Note 18.) 
I., <5, /3.) (Com- 
found in 
and ignite. 
dry Sug- 
rite’s 
pare Note 12.) 
difference 
=ALO.% 
Weigh as 
CaS04. 
{Free., 
§ 103,2, b.a.) 
gestions, 
No. 4. 
process. 
(Fres., 
§ 112, 
2, a.) 
Special Determination. Determine H20 in 1 grin 
of ore by direct 
weight. {Fres., § 36,1 
\ 66 
QUANTITATIVE ANALYSIS. 
Notes to the Preceding Scheme. 
Note i. Sampling the ore.—Break up in an iion mortar 
forty or fifty pounds into pieces that will pass through a tin 
sieve with half-inch holes. Thoroughly mix the fine and 
coarse. Break up about ten pounds of average quality, so 
that it will pass through a tin sieve with quarter-inch holes, 
Mix well, take one pound, and pulverize in the iron mortal 
until it will pass through a brass sieve of 60 meshes to the 
linear inch. Mix well, take out about 50 grammes, pul 
verize in agate mortar, pass through muslin bolting cloth, 
and put into a small bottle, tightly corked, for analysis and 
special determinations. It is yet necessary that every 
portion of this required for the main analysis or a special 
determination should be further pulverized, as needed, in 
an agate mortar, to an ivzpalpable powder. 
Note 2. Preliminary fusion.—Thoroughly mix the ore 
and its fluxes on glazed paper, put about a third of the 
mixture in a two-ounce platinum crucible, the lower portion 
of whose interior surface has been previously lined with a 
thin layer of Na2C03, and heat over a common Bunsen 
burner with strong flame until the greatest violence of the 
effervescence has ceased. Then add and treat the two- 
thirds remaining successively and with the same precaution. 
Finally, heat strongly over the blast-lamp until the mass is 
in complete and quiet fusion, adding a little more Na2C03, 
should it not readily fuse. The time required for this 
fusion varies fron 30 to 50 minutes. 
Certain highly aluminiferous ores obstinately resist this 
method of attack ; in such cases mix with the flux a known 
weight (two or three grammes) of chemically pure precipi- 
tated silica which has been strongly ignited just before 
weighing. The amount of silica added is afterwards 
deducted from the total amount found in Residue d. Note 3. Removal of the fused mass.—Let the crucible 
cool until just below red heat, then chill it suddenly by 
plunging it into cold water contained in a porcelain cas- 
serole, lay the crucible on its side and digest with boiling 
water. The fused mass will generally become detached 
from the crucible and come out in a cake. Then remove 
the crucible, wash it, treat in a small beaker with a little 
cone. HCI to remove any adhering particles of the mass, 
and add this solution to that of the Insoluble Residue 
(2), Should any portion of the fused mass, thicker than a 
film, obstinately resist solution in the hot water, it ought to 
be removed only by patience and long boiling; and no 
attempt should be made either to dig it out or to dissolve 
it in HCI; lest by the formation of Aqua Regia or free Cl 
(in the presence of NaN03, or Mn203) the crucible be 
attacked and injured. 
NOTES TO THE PRECEDING SCHEME. 
Note 5. Separation of Si02.—ln order to render the 
Si02 entirely insoluble, it must be perfectly dehydrated. 
The evaporation should be carried to dryness, the residue 
heated until odors of HCI can no longer be detected, and 
the mass is hard and crumbly. Since the residue is to be 
re-fused with Residue b, the drying may be completed, at a 
temperature somewhat higher than ioo° C., in an air-bath. 
Note 8. Precipitation of BaS04.—Avoid the addition 
of a large excess of BaCl2 solution. Add only 5 c.c. at first, 
and then after complete subsidence of precipitate, add a 
few drops to determine if any H2S04 remains unprecipi- 
tated, etc. Then proceed as in Fres., § 132, I, 1. After 
decanting the clear supernatant liquid, boil the precipitate 
with water, allow to subside, decant, filter, and wash with 
hot water. These precautions are necessary to dissolve 
out any other salts of barium, which are always carried 
down on the first precipitation. If the precipitate of BaS04 
is dark colored after ignition, dissolve in the crucible in 68 
hot cone. H2S04, pour into cold water, and collect the pre 
cipitate as before. 
QUANTITATIVE ANALYSIS. 
Note 9. Separation of Si02.—Evaporate as in Note 5. 
Then add HCI quite freely and warm for some time before 
adding any water, as the high heat may have produced 
anhydrous Fe203, forming an oxychloride which is very 
slow to dissolve, especially in dilute acid. Should the acid 
already added be too dilute, concentrate by evaporation, 
add cone. HCI, and digest at a moderate heat. 
Note 11. Precipitation of the basic acetates.—Fil- 
trate f combined with Solutions a 1 and dx must be very 
carefully neutralized with sodium carbonate. (If ammonium 
carbonate were used, bromide of nitrogen might form in 
Filtrateg.) To neutralize the greater portion of the acid 
use crystallized sodium carbonate, and complete the neu- 
tralization with a very dilute solution of the carbonate, add- 
ing it drop by drop, agitating to dissolve the precipitate, 
until the liquid assumes a deep mahogany-red color. If a 
permanent precipitate forms, add a little hydrochloric acid, 
and repeat as above. Then dilute the solution to about 1 
litre for each gramme of the sesquioxide present, add about 
20 grammes sodium acetate dissolved in a small quantity of 
water, and heat the whole to boiling. 
It is sufficient to boil from ten to fifteen minutes for the 
complete precipitation of the acetates. The filtering should 
be done rapidly on a ribbed filter, keeping the fluid hot. and 
disturbing the settled precipitate as little as possible™ 
When available the Bunsen pump may here be used with 
advantage. After the supernatant fluid has been poured 
through the filter, throw on the precipitate and wash it with 
boiling water containing a little sodium acetate. Should 
any basic acetate separate upon concentrating the filtrate, 
add some sodium acetate, boil, filter, dissolve the precip- 
itate in HCI, and unite to the solution of the main body. 69 
In boiling Filtrate e with KCI03 to oxidize FeO, be 
careful to decompose the whole of the chlorate by heat- 
ing with excess of HCI. 
NOTES TO THE PRECEDING SCHEME. 
Note 12. Determination of P2Os.—To remove the HCI 
in Solutiofi g1 add NH4HO in large excess, wash the pre- 
cipitates of ferric hydrate and ferric phosphate by decanta- 
tion two or three times, and redissolve in hot cone. HN03. 
Evaporate this solution down to small bulk (150 c.c. to 100 
c.c.), partially neutralize with NH4HO, and add about 50 
c.c. of solution of ammonium molybdate in nitric acid. If 
the solution is very acid, ammonium nitrate is formed by 
the partial neutralization as above, otherwise add a small 
quantity of the salt. Warm the solution, do not boil, and 
let stand 24 hours or more. Then filter from the yellow 
granular precipitate of ammonium phospho-molybdate with- 
out bringing it all on the filter, and wash the precipitate 
with a solution prepared by mixing 100 parts of the precipi- 
tant with 20 parts of HNOs (sp. gr.= i.2) and 80 parts of 
water. Dissolve the yellow precipitate by pouring a small 
quantity of dilute NH4HO through the filter into the 
original beaker, and determine the phosphoric acid in the 
ammoniacal solution by means of magnesia mixture (5 c.c.) 
in the usual manner. Magnesia mixture is preferably made 
with magnesium chloride. If the crystalline ammonio- 
magnesium phosphate falls mixed with flocculent magne- 
sium hydrate, add HCI until dissolved and reprecipitate 
with NH4HO. 
Reserve the filtrate and washings of the yellow precipi- 
tate, and test for phosphoric acid by adding a little more 
of the ammonium molybdate solution, heating and allowing 
to stand 12 hours. If a yellow precipitate forms, pour 
through a separate filter, dissolve in dilute NH4HO and 
add to the ammoniacal solution. 
If the yellow precipitate first obtained was not suf 70 
QUANTITATIVE ANALYSIS. 
ficiently washed, a red residue of oxide of iron may remain 
on the filter, in which case pour dilute HN03 upon it, 
allow it to pass into the amraoniacal solution, acidulate 
that with HNOs, warm, add more of the precipitant, and 
set aside as before; filter and wash several times with the 
diluted precipitant, then dissolve the precipitate on the 
filter and that adhering to the beaker in as little dilute 
NH4HO as possible. 
The yellow granular precipitate of ammonium phospho- 
molybdate is not sufficiently constant in composition to 
admit of directly weighing it in exact analysis ; it is there- 
fore dissolved in NH4HO and the phosphoric acid thrown 
down with magnesia mixture as just detailed. According 
to Nuntzinger’s analysis, after drying at ioo° C., it contains 
3-577 Per cent NH4HO 
3.962 “ P205 
92.461 “ Mo03 
100.000 
Lipowitz says the precipitate dried at 20° to 30° C. con- 
tains 3.607 per cent, of PA, Eggertz 3-7 to 3-8 per 
cent. P20s. When dried at 120° C., Sonnenschein found 
about 3 per cent. For properties of this precipitate see 
also Fres., § 93, i, foot-note. Consult also Finkener’s 
paper in Bericht d. d. chem. Ges XI, p. 1638 (1878), and 
Ghent. News, XLVII, p. 66 (1883). 
Note 13. Washing of 1'e2033H20.—Wash this precipi- 
tate by boiling up with water and decanting until the wash 
water shows very little alkaline reaction with litmus paper, 
and gives very little precipitate with solution of AgN03. 
Then transfer to filter, and wash thoroughly with boiling 
water. 
Note 16. Determination of Mn.—(Gibbs’ process, Am NOTES TO THE PRECEDING SCHEME. 
71 
your. Sci. [2] XLIV, p. 216.) To the HCI solution add 
NH4HO in excess and solution of Na2HP04 in large 
excess. Then add dilute H2S04 or HCI until the white 
precipitate redissolves, heat to boiling, and add NH4HO in 
excess. Digest near the boiling point about an hour, when 
the precipitate, at first white and gelatinous, becomes 
rose-colored and forms crystalline scales. Filter and wash 
with hot water. If tinged red, redissolve the precipitate in 
dilute HCI, and repeat the process. On ignition the pre- 
cipitate is converted into Mn2P207, a nearly white powder. 
If Zn is present, it must first be separated as in 
Scheme I, Am. Chem., Vol. I, p, 323. 
Note 18. Volumetric Determination of Fe.—Put 
Solution k\ which must be completely free from the KCI03 
used to oxidize Filtrate k, into a wide-mouthed reduction 
bottle holding about 250 c. c. Carefully let down into the 
bottle a lump of amalgamated zinc, free from iron, and a 
strip of platinum foil resting upon it, add about 10 c. c. 
cone. H2S04, cover with a watch-glass and set aside over 
night. To ascertain if the reduction is complete test the 
solution with ammonium sulpho-cyanide, which should 
give only a trace of pink color. 
Then introduce into a flask holding about 200 c. c., and 
fitted with a Krdnig valve, exactly 0.2 gramme iron piano- 
forte wire, add dilute H2S04, and heat until complete 
solution of iron. Cool the flask, pour and wash out the 
contents of the flask into a large beaker containing about 
400 c. c. cold water, add a little concentrated H2S04 and 
titrate with a solution of K2Mn2Os (13 grms. in 2 litres 
water) to determine its strength. Repeat, and average 
results. 
Now pour and wash out the contents of the reduction- 
bottle into a large beaker, add cone. H2S04, and titrate 
with the standard K2Mn208 as before. If the HCI was not 72 
QUANTITATIVE ANALYSIS, 
properly removed from Solution b'1 the dark brown-red 
ferric chloride formed will interfere with the end reaction 
of the permanganate. In such a case reprecipitate with 
NH4HO, wash thoroughly, and proceed as with Solution kl. 
Treat Solution kl in exactly the same manner, and aver- 
age the results. Cf. Analysis No. 3, C. 111. 
For method of repeating the titration in the same solu- 
tion, see Crookes’ Select Methods, p. 74. 
Sundry Suggestions.— 1. Solution a3 may be used for 
duplicating the determination of S, provided the absence 
of Fe is proved by the proper tests. Duplicate determina- 
tions of Ca and Mg can be made, if desired, in the filtrate 
from the precipitate formed by ammonium hydrate in 
Solution P, provided this precipitate be thoroughly washed. 
2. Duplicate determinations of Ti and of Fe can be 
made in Solution P; the Fe can also be estimated volu- 
metrically by dissolving in acid the weighed precipitate 
resulting from the treatment of Solution g2. In the latter 
case, however, the presence of Ti02 will impair the results. 
3. The purity of the Si02 obtained in Residue d may be 
tested, after weighing, by heating with fluoride of ammon- 
ium and concentrated sulphuric acid in a platinum crucible, 
whereby all the Si02 is expelled and is determined by the 
loss in weight, the residue being Ti02 probably colored by 
Fe. 
4. In fusing Residue c or Precipitate k, hydro-sodium 
sulphate may be substituted for KHS04, but since the for- 
mer contains water of crystallization it should be heated 
until the water is expelled before using in fusions. In 
either case avoid expelling the whole of the H2S04, or if 
the mass is heated to redness, partially cool, add cone. 
H3S04 and heat again at a lower temperature. In this NOTES TO THE PRECEDING SCHEME. 
73 
way the Ti02 will be held in solution by the excess of acid, 
and the resulting acid sulphate will dissolve out readily. 
For Special Determi7iations see Notes to Scheme I in 
American Chemist, Vol. I, pp. 323 et seq. 
Reactions.—A full discussion of the many and complex 
reactions which take place in the preceding scheme for the 
analysis of iron ores is superfluous. 
We add a few remarks and equations which may serve 
to throw light upon some points. 
A.—The action of potassium permanganate on ferrous 
sulphate has already been formulated in connection with 
the notes to Analysis No. 3. This action, however, may be 
regarded as taking place in two stages, as follows: 
ist stage. 2KMn04-f-H2S04=K2S044-2HMn04. 
2d stage. 2HMn04+7H2S04+ioFeS04=2MnS04. 
+S(Fe2(SO4)3)+BH2O. 
Solution F is treated with excess of NH4HO and the 
precipitate dissolved in H2S04 in order to remove the 
larger part of the HCI which might vitiate the results of 
the titration as indicated in Note 18. The presence of HCI 
is injurious also because it exerts a reducing action on the 
permanganate as shown in the equations following: 
2HMn04+i4HCl=2MnCla+BHaO+ioCl, 
and 2FeS04+HaS04+2Cl=Fe2(S04)3+2HCI. 
B.—When KCI03 is employed in acid solution as an 
oxidizing agent (as in the case of Filtrate e), the reaction 
which takes place depends upon the acid used and partly 
upon the strength of said acid. Concentrated sulphuric 
acid is said to act thus; 
6KCI03+3H2S04=2HCI04+2C1204+3K2S044-2H20 
and nitiic acid thus; 74 
QUANTITATIVE ANALYSIS. 
BKCI03 + 6HN03 = 2KCI04 + 6KNO3 + 6CI + 130 
+ 3H20. 
The action of hydrochloric acid on potassium chlorate is 
variously formulated; Bottger gives the equation (1) and 
Odling (2): 
(1) 2KCI03+6HCI=2KCI+C1203+4Cl+3H20. 
(2) 4KClo3+i2HCl=4KCl+3Cloa+9Cl+6H2o. 
In any of these cases the powerful oxidizing agency of 
KCI03 is evident. 
Appendix to Analysis No. 21. 
A.—Method for the Estimation of Fe and Ti only. 
Sample, pulverize, fuse 1 grm. ore with 3 grms. NaFl-f-i2 
grms. KHS04. Dissolve in large quantity of cold water; 
if there is any considerable residue re-fuse. Neutralize 
with Na2C03 until a slight precipitate forms, then add 
H2S04 until the ppt. redissolves and the liquid is slightly 
acid. Saturate with H2S gas, boil some hours, occa- 
sionally adding H2S water. Filter from the precipitate 
of Ti02-{-S, dry, ignite, and weigh, if dark colored re- 
fuse, etc. To filtrate add a little KCI03, boil to oxidize 
112S. Reduce the iron with amalgamated zinc and plat- 
inum foil, and titrate with K2Mn2Os as usual. As a result 
of the fusion we have 
4NaFI-fSiO,+4H.SO4=4NaHSO4+SiFI4+2HaO. flight’s method. 
7 5 
B.—Flight’s Method for the Separation of Iron, Alumina and Phosphoric Acid. 
(Journal of Chemical Society (2), XIII., 592, 1875. The solution of the three substances named must contain 
but little free hydrochloric acid. Boil the solution two or three hours with an excess of sodium hyposulphite, and 
filter. Wash thoroughly. 
Filtrate a. 
Contains all the iron and some of the P00B. 
(If but a small amount of P2Os is present in”the 
solution, this filtrate will contain no P„Ob and 
may be rejected after careful testing.) Add 
NH4HS saturated with H2S and warm. Filter 
quickly, wash with H,S water containing a few 
drops of NH4C1. 
Precipitate a. 
Contains all the Al203and most of the P2Ob.* Dissolve in HC1, 
add enough NaHO to completely redissolve the precipitate formed 
and throw down P2Ob with excess of BaCl2. Do not heat, but let 
stand a few hours covered. Wash with dilute NaHO. 
Precipitate c. 
Dissolve the Ba3P208 in HC1, add slight 
excess of H2S04 boil and filter. 
Filtrate c. 
A12Os in alkaline so- 
lution. 
Acidify with HC1 
and determine Al2Oa 
in the usual manner. 
Precipitate b. 
FeS. Dissolve in ITC1, 
oxidize with UNO, pre- 
cipitate with NH4HOand 
determine as usual. 
Filtrate b. 
P2Ob. Reserve to 
add to Filtrate d. 
Precipitate d. 
BaS04. Reject. 
Filtrate d. 
Combine with Fil- 
trate b and determine 
P,Ob with magnesia 
mixture in the usual 
manner. 
• Flight states that the P,Or. is carried down with the A1203 completely when the solution contains less than 45 per cent. PaOB. 76 
QUANTITATIVE ANALYSIS. 
Analysis No 22.—Pig Iron. 
To be determined: Iron, Combined Carbon, Graphite, Silicon, Sulphur, Phosphorus, and Manganese. 
A.—Determination of Graphite, Silicon, Sulphur, Phosphorus and Manganese. 
(Bj F. A. Cairns.)—Place 10 grms. of fine borings in a flask of about two litres capacity, add 25 to 35 grms. 
KCIO3. little by little, a few grms. at a time, pour in carefully and gradually concentrated HCI, using eventually 
about 300 c. c. Digest until the iron is completely dissolved, then pour contents of flask into a porcelain dish and 
evaporate to dryness on a water-bath. Moisten with HCI, add water, filter through a weighed filter, previously 
dried at ioo° C. 
Residue a. 
Grap/i{tcn.nA Silicon. Wash 
thoroughly and weigh on the 
filter after drying at IOO° C. 
Then transfer to a platinum 
crucible and burn oft' the 
graphite; weigh the residue 
as SiO„. See Note 2. 
If the residue contains 
iron, expel the SiO„ by heat- 
ing with NH4F1 and H,S04 
and weigh again. Compare 
A A , or the Second Method. 
Dilute to 1000 c. 
Filtrate a. 
c. and divide into three portions as follows : 
Solution a1. 
500 c. c. 
For determination of 
phosphorus proceed exactly 
as with 
Solution gl 
of Analysis No. 21, Scheme 
II. 
_ 
Solution ad. 
300 c. c. 
For determination of sul- 
phur partially neutralize 
with solution of Na2COs, 
and proceed as with 
Solution a2 
of Analysis No. 21, Scheme 
II. 
Solution a3. 
200 c. c. 
For determination of 
manganese proceed exactly 
as with 
Filtrate f and Filtrate g 
of Analysis No. 21, Scheme 
II. See Note 1. NOTES TO THE PRECEDING SCHEME. 
77 
Note I.—Care must be taken in dissolving the pig-iron in 
HCI-f-KClOj not to add the oxidizing agent all at once, nor 
too rapidly, otherwise some of the iron may remain unoxi- 
dized. Should a small portion of ferrous chloride remain 
in the solution, the subsequent precipitation of the iron as 
basic acetate (as in Filtrate f Analysis No. 21) will be 
imperfect; instead of an orange red flocculent precipitate 
resembling ferric hydrate, the iron will fall as a brick-red 
pulverulent precipitate, (anhydrous ferric oxide?) which 
has the property of running through filters. 
Note 2.—Si02 obtained in this manner, and dried at 
ioo° C., contains 6 per cent. H2O, which is expelled on 
ignition, and must be deducted from graphite after the 
Si02 has been determined. According to Allen (see 
Chemical News, Vol. XXIX., p. 91, Feb., 1874) the Si of 
the pig-iron is converted by the action of dilute HCI into 
leucone, 35i0.2H20. By fusing the mixture of leucone and 
graphite with KHO, the former goes into solution, and both 
may be estimated directly. 
AA-Determination of Graphite and Silicon. 
Second Method. (Eggertz, Client. News, XVIII., p. 
232.—Mix 10 c.c. H2S04 with 50 c.c. H2O, cool, add 5 
grms. fine borings, boil half an hour, evaporate one-third 
and cool. The reaction is as follows : 
2Fe4C+BH2S04=BFeS04+C2H4+H12. 
This equation, however, but imperfectly formulates the 
reaction, the S forming H,S and the P forming PH3, A 
large number of compounds of C and H are evolved in 
addition to the C 2H4 of the equation; according to Dr. 78 
QUANTITATIVE ANALYSIS. 
Hahn (Annalen der Chemie und Parmacie, Vol. 129, j». 57, 
1864) they include the following; 
f Ethylene, C 2H4. CEnanthene, C 7H14. 
Gaseous. -1 Propylene, C 3HB. Caprylene, C 8H18, 
[Butylene, C 4H4. . Elaene, C 9HtB. 
Liquid paramylene; CwHjo_ 
liautd /Am?lene’ C 5niO. Cetylene, Cl 6H33. 
q \ Caproylene, [ etc. etc. 
Next add 10 c. c. HN03 and boil 15 minutes. 
6FeS04+BHN03==2(Fe2(S04)3)+Fe2(N03)6+N202 
+4H2O. 
Evaporate on a water-bath until vapor ceases to come off 
and the mass is nearly dry. 
Add 75 c. c. H2o+i3 c. c. HCI and boil 15 minutes; 
add more HCI if any Fe203 remains undissolved. Filter 
through a filter washed with HCI, dried and weighed; wash 
first with cold water until no more iron appears in wash- 
ings, then with boiling water containing 5 per cent. HN03. 
Dry at ioo° C., and weigh the residue consisting of Si02-f- 
-graphite. Ignite and weigh again; the loss in weight gives 
the amount of graphite. Lest the residue contain some- 
thing besides Si02 it is well to determine the latter by 
heating with NH4FI and H2S04, which expels the Si02 in 
accordance with the following equation : 
4NH4FI+SiO2+2H2SO4=SiFI4+2(NH4)2SO4+2H2O. 
The loss in weight gives the amount of Si02; consult, 
however, Note 2 of A. 
AAA.—Graphite determination according to F. A. Cairns. 
Dissolve 5 grms. borings in dilute HCI, boil, filter, wash 
with hot water, then with KHO solution, then with boiling water, then with (a) alcohol, (b) ether and (c) hot water. 
Dry and transfer to flask and determine as in B. 
DETERMINATION OF TOTAL CARBON. 
79 
In this process the combined carbon goes off in volatile 
hydrocarbons, and graphite -|-Sio2 together with certain 
liquid hydrocarbons, remain. The Si02 is removed by the 
KHO, the hydrocarbons dissolve out in the alcohol and the 
ether, while the latter is removed at last by boiling water. 
B.—Determination of Total Carbon. 
A. H. Elliott’s modification of Roger’s Process. See 
Journal of Chemical Society, London, May, 1869; also 
Cairns’ article in Am. Chem., Vol, 11, p. 140. 
To 2.5 grms. of borings add 50 c.c. of a neutral solution 
of CuS04, containing one part of sulphate to 5 parts of 
water; heat gently for 10 minutes; the iron dissolves; 
copper is precipitated, and the silica, graphite, and com- 
bined carbon remain: 
Fe-f-Cu S 04= Cu-f-FeS 04. 
The cupric sulphate should be as neutral as possible, in 
order to avoid loss of combined carbon, in the form of 
volatile hydrocarbons, as shown in AA. 
Add 20 c.c. CuCl2 (1 part of chloride to 2 parts of water), 
with 50 c.c. strong HCI, and heat for some time nearly to 
boiling, until the copper dissolves : 
CuCl2-|-Cu=Cu2Cl2, 
Prepare an asbestus filter as follows: select a glass tube 
of about 3 to 4 cm. diameter, and 18 to 20 cm. in length. 
Draw out this tube to taper at one end, and place broken 
glass and asbestus, lightly packed, in the narrowed portion 
of the tube. (See Fres., § 218, I, 1, p. 759-) Filter the 
cuprous solution through the asbestus, wash thoroughly QUANTITATIVE ANALYSIS. 
with boiling water, and transfer contents of filter to a flask 
holding about 200 c.c. In making this transfer, the carbon, 
asbestus, and broken glass may be blown into the flask 
together, in order to use as little water as possible. Add 
to the contents of the flask about 3 grms. of Cr03, (or if 
this is not available, about 5 grms. K2Cr207), and arrange 
apparatus as in the determination of C02 by direct weight, 
Analysis No. 7, note 8, II (page 34). Avoid adding more 
water than absolutely necessary to transfer the carbon. 
Add 30 c.c. to 40 c.c. concentrated H2S04, little by little, 
shaking constantly, and closing cock of funnel-tube each 
time. Finally, heat gently to boiling, not allowing more 
than three bubbles of C02 gas to pass per second: 
3C-f-4CrO3+6H2SO4—3CO2-j-2Cr2(504)3-J-6H20. 
Boil one minute, attach guard tube of soda lime, and 
aspirate slowly, three bubbles per second. Weigh the 
soda-lime tube for amount of C02 absorbed, and calculate 
the amount of carbon. 
Note—The carbon separated from cast-iron by treatment 
with sulphate of copper contains H and O, and cannot 
therefore be determined by weighing directly. Schutzen- 
berger and Bourgeois assign to it the composition expressed 
by the formula C„3H2O, and consider it related to graphitic 
acid. Bulletin de la Societe Chimique de Paris, Vol. 23, 
No. 9. 
BB.—Other Methods for determining Total Carbon. 
A great number of methods have been devised for deter- 
mining total carbon, some of which we will briefly outline, 
remarking, however, that the foregoing is entirely satis- 
factory. DETERMINATION OF TOTAL CARBON. 
81 
i Method of Alvargonzalez. See Am. Chem., Vol, V., 
p. 437.—Place 10 grms. of borings in a beaker and treat 
with a solution of cupric sulphate (40 grms. CuS04 in 200 
200 v..c. H2O), stirring until the reaction ceases. Add di- 
lute HN03 gradually, and let stand until the copper has dis- 
solved. Dilute the solution and filter through one of Rath- 
ers naif filters (described in Chem. News, Jan. 30, 1874, 
p. 57), wash thoroughly, and dry on funnel at ioo° C. 
Detach ppt. from filter carefully, place in a weighed cru- 
cible (throw away filter), dry at ioo° C, and weigh. Ignite 
and weigh again; the difference between two weighings 
gives total carbon. 
This method is not free from objections, but will answer 
when great accuracy is not indispensable, and speedy results 
are desirable. 
2. Method employed by I. Lowthian Bell. See Chemical 
Phenomena of Iron Smelting, London, 1872.—Digest 3 grms. 
borings from 24 to 48 hours with a solution of CuS04 in 
excess, collect the spongy Cu-j-C-l-graphite on an asbestos 
filter, and burn the carbon in a stream of oxygen gas, as in 
the ultimate analysis of organic bodies collecting the C02 
in KHO solution, Cf. Analysis No. 30. 
3. Method of Regnault and Bromeis. See Crookes’ 
Select Methods, p. 74.—Heat borings in a combustion tube 
with a mixture of plumbic chromate and KCI03, collecting 
the C02 in KHO. 
4. Methods for the liberation of Combined Carbon are also 
numerous. 
(a) Boussingault triturates the iron in a porcelain mor- 
tar with 15 to 20 parts of HgCl2 and sufficient water to 
make a thin paste: 
Fe4-2HgCl2=FeCl2+Hg,Cla. 82 
QUANTITATIVE ANALYSIS. 
Then dilute with 200-250 c.c. HCI and warm for an hour; 
filter from the Si02-]-C, wash and dry. Transfer to a 
platinum boat, and heat in a current of pure H, volatilizing 
the Hg2Cl2. Weigh the C, heat again in a current of O, 
burning off the C, and weigh again. 
(b) Weyl dissolves the pig-iron under the influence of 
a galvanic current. Attach a weighed piece of cast-iron to 
the positive pole of a Bunsen cell, and suspend it in dilute 
HCI. The iron dissolves, H being given off at the negative 
pole, and the carbon is separated. 
Weyl has also devised another method based upon the 
following reaction: 
Fe.+KiCrA+7(HISO4)=FeI(SO4),+Cr2(SO4)J 
+7H.O+K,SO4. 
See Crookes’ Select Methods, p. 76. 
(c) McCreath’s Method. See Engineering and Mining 
Journal, March 17, 1877. The author uses double chloride 
of ammonium and copper to dissolve out the iron, while the 
precipitated copper dissolves in excess of this reagent; 
he then oxidizes the carbon by means of Cr03 in an appar- 
atus somewhat similar to Elliott’s, collecting the C02 in a 
Liebig potash-bulb. 
5. Eggertz Colorimetric Method. See Crookes’ Select 
Methods, pp. 81 to 84; also Britton’s paper in Journal of 
the Franklin Institute, May, 1870. 
C.—Other Methods for the Determination of Sulphur 
and Phosphorus. 
I. Eggertz’s Method. See Client. News. Vol. XVII, 
p. 207. DETERMINATION OF SULPHUR, ETC. 
A. Dissolve 10 grms. KCI03 in 200 c.c. H2O, place in a 
500 c.c. flask, add 5 grms. fine borings, boil and add 60 c.c. 
HCI, little by little, boiling until the Fe dissolves : 
4KCIO3+I2HCI=4KCI+3CIO2+9CI+6H2O, 
and 
2Fe+Clo2+Cl+4HCl=:Fe2Cl6+2H2o. 
Evaporate, dry on water-bath to insure oxidation of sul- 
phur, Thorough dryness is unnecessary, since Si02 does 
not interfere in acid solution with the precipitation of 
BaSQ4. Then add 10 c.c. HCI-l-30 c.c. H2O, and digest 
on water-bath until all the Fe2Cl6 is dissolved. Then add 
20 c.c. H2O, filter, and wash thoroughly. Add 2 c.c. of a 
saturated solution of BaCl2 (enough to precipitate the 
H2S04 from o. 1 grm. S); after cooling add 5 c.c. NH4HO, 
stir and let stand 24 hours. Filter, and wash by decanta- 
tion with cold water two or three times, and then tho- 
roughly with hot water. Dry, ignite, and weigh. If the 
precipitate shows traces of iron after ignition, purify by so- 
lution in H2S04. 
B. For the determination of phosphorus dissolve the 
pig-iron in the same manner, and dry at i4o° C ; some 
anhydrous Fe203 will remain with the Si02; add water, 
filter, fuse residue with a little KHS04, soften with H2S04, 
and dissolve in water. Filter from the Si02, and determine 
it as a check on the main analysis. Add filtrate to main 
one, and determine the P205 by means of ammonium molyb- 
date, as in Analysis No. 21. 
2. Method of Dr. T. M. Drown. See Am. Chem., Vol. 
IV, p. 423. 
Treat 5 grms. of borings in a flask with HCI, and pass 
the H2S and PH3 formed through a series of three bottles 
containing a solution of K,Mn2oß(i grm. to 200 c.c. H2O) 
Avoid a very rapid evolution of the gas; when this ceases, 84 
QUANTITATIVE ANALYSIS. 
aspirate for some time, and then pour the contents oi the 
bottle into a beaker, rinse with water, and add sufficient 
HCI to decompose the K2Mn208. Filter the colorless so- 
lution, add BaCl2, to throw down the H2S04, and proceed 
as usual. 
3. Method employed by J. Lowthian Bell. 
Dissolve in HCI as above, and pass the gases through a 
solution of potassic plumbate (lead nitrate super-saturated 
with KHO). Boil half an hour, or until the evolution of 
gas has ceased. Wash the PbS formed, oxidize it with 
HN03, and throw down the S as BaSQ4 by means of 
8a(N03)2. Let stand 24 hours, collect on a filter, dry, 
ignite, and weigh. This method is said to give higher 
percentages of S than that of Eggertz. Compare Fres., 
% 218, 3. 
4. Method of Arthur H. Elliott. See Am. Chem.y 
Vol. I, page 376. 
5, Method employed by Koninck and Dietz. See Pme- 
tical Manual of Chemical Analysis and Assaying applied 
to Iron. Translated by Robert Mallet. London, 1872. 
Dissolve 3 to 5 grms. borings in HCI in a flask connected 
with four bottles, the first a condenser, the three following 
containing solution of AgNOs(i part of nitrate to 20 parts 
of water). Boil, and when gas ceases to evolve, aspirate, 
Pour contents of flask on one filter, and wash the Ag2S. 
Wash out the flask and cleanse the ends of the tubes witn 
bromine water, and expel excess of Br by heat; the follow 
ing reaction ensues : 
Ag2S+BBr+4H20=H2S04+2Agßr+6Hßr. 
The phosphide is also converted into phosphoric aeio 
Filter from Agßr, and ppt. H2S04 with BaCl2 as usual. DETERMINATION OF IRON MANGANESE, ETC. 
85 
6. Method of Boussingault for determination of Phos- 
phorus. See Annales de Chimie et de Physique, June, 
1875, and abstract in American Chemist, Vol. VI, p. 275. 
7. For additional methods consult also papers by Alfred 
H. Allen, Chem. News, XXIX, p, 91, and paper by 
Hamilton, Chem. News, Vol. XXI, p. 147. Compare 
Crookes’ Select Methods, pp. 84-89. 
D.—Determination of Iron Manganese, etc. 
The iron may be determined by difference or by Margue- 
rite’s method, in which case dissolve 0.2 grms. of pig-iron 
in H2S04, and proceed as usual. It is advisable to use a 
rather dilute solution of K2Mn208 towards the close of the 
oxidation. 
For the determination of the bases of Groups 11, 111, 
and IV, dissolve 10 or 20 grms of pig-iron in HCI, remove 
the Si02 by drying thoroughly, and proceed as in Analysis 
No. 21. 
The manganese may be thrown down in the filtrate, from 
the basic acetate of iron by means of bromine, or in the 
absence of calcium, magnesium, etc., by hydrodisodic phos- 
phate. See Fres., § 109, 3, also § 218, 6. For other methods 
of estimating manganese see articles by Samuel Peters in 
Chem. News, Vol. XXXIII, p. 35, and by William Gal- 
braith, in Chem. News, Vol, XXXIII, p. 47. 
See also paper by Charles H. Piesse in Chem. News, 
Vol. XXIX., pp. 57 and no. 
For testimony as to the condition in which silicon exists 
in pig-iron, see paper by E. H. Morton, Chem. News, 
Vol. XXIX., p. 107. 86 
ANALYSES Nos. 23 AND 24. ARSENICAL NlCKEL ORE. 
May contain Si02, S, 
As, Sb, Pb, Cu, Fe, Al, Mn, Zn, Co, Ni, Cu, Mg, etc. 
To be determined: As, Ni, Co.—Pulverize very finely; heat 3 grms. (or 4, if a very poor ore) in a coveied 
casserole with fuming HNO, until the ore is completely dissolved, except a little silica. Expel excess of acid on 
a water-bath,.add 10 c.c. HC1, dilute to about 200 c.c., warm and filter. Consult article by Fresenius in Am. 
C/iem., Vol. IV, p. 289. 
Residue a. 
Filtrate a. 
SiOs PbS04. 
CaSOt, etc. 
Test with 
blowpipe for 
Co and Ni. If 
found, f u s e 
with KHS04. 
and add wa- 
Add a little Na2SO., and heat, pass H„S through the warm liquid until saturated. See Fres., § 125, 
1, and § 127, 4, a. Let stand some hours, throw on small filter, and wash with weak H,S water. 
Precipitate b. 
AStjSjj. 
If much free S is mixed 
with the precipitate, dry, 
and exhaust with CS2. 
Otherwise treat moist pre- 
cipitate, filter and all, in a 
porcelain casserole with 
fuming HN03; expel ex- 
cess of acid on water-bath, 
then dilute to about 150 
c.c., and throw down 
As„0- with “ magnesia 
mixture.” Fres., § 127, 
2, a. Let stand 12 hours 
1Solution b. 
Boil with a little KCIOs-f-5 c.c. cone. HC1, evaporate nearly to dryness, 
add water, warm, and add NILHO in excess. Wash well hot. 
ter solution 
to Filtrate a. 
Precipitate c. 
FeA 3H20. 
Dissolve in 
HC1 and re- 
precipitate 
with NH.HO. 
filter and add 
the filtrate to 
Filtrate c. 
Filtrate c. 
Combine with second filtrate from the iron and add 20 
c.c. NH4IIO. The solution should not measure more 
than 250 c.c. Introduce platinum electrodes and start 
the galvanic battery. (See Am. Chem., Vol. VI, 
page 213.) Run battery all night, but take care to 
maintain an excess of NH4HO. Wash the precipitated 
Co and Ni with water, alcohol, and weigh. To determine 
if precipitation is complete, test solution with NH4HS. 
QUANTITATIVE ANALYSIS. 87 
in the cold. Filter through 
a weighed filter, collect fil- 
trate and washings sep- 
arately. Measure filtrate 
and test washings. Dry 
precipitate at 105° to 1 io° 
C., and weigh, repeat to a 
constant weight. For 
every 16 c.c. of filtrate (not 
washings) add one mgm. 
to the weight of the pre- 
cipitate. See Fres§ 93, c. 
Test the pre- 
cipitate of iron 
for nickel. 
Filtrate d. 
Boil down to 
smaller bulk, 
and test with 
electricity as 
above. 
Precipitate d. 
Dissolve in warm HC1. partly neutral- 
ize with KHO, add a cone. sol. of KN03 
in excess, acidulate with acetic acid and 
let stand 34 hours. Filter and wash with 
a solution of neutral KC2H3O2 (10 per 
cent, sol.), and afterwards with alcohol. 
See Fres., § m, 4. 
Filtrate e. 
Concentrate, 
add KN02 and 
let stand. If 
pre c i p i t a t e 
forms add to 
precipitate e. 
Precipitate e. 
Dissolve in HC1, neu- 
tralize with NH4HO, and 
add 10c.c. more NH4HO. 
Throw down Co by the 
battery as before. Weigh. 
Weight of Co-f-Ni less 
weight of Co gives weight 
of Ni. 
Consult Revue Univer- 
selle des Mines, Vol. 32, 
P- 545- 
Notes.—By the addition of sodium sulphite to Filtrate a we reduce the nitric acid and prepare the solution for 
the action of H2S. The reaction is as follows : 
3Na0S0,+2HN0<!=3Na„S04+N„0,+H„0. and prevents the action shown in this equation: 
ioH;S+7HN0s=3NH4HS04+2NO+NH4NO3+S7+4H2O. 
Consult article by Parnell, in Chem. News, Vol. XXI, p. 133. On determination of cobalt a"d nickel consult 
article by E. Donath in Chem. Ne-ws. Vol. XLI, p. 13. 
ARSENICAL NICKEL ORE. 88 
QUANTITATIVE ANALYSIS. 
Consult Fres., Quant. Analysis, § 220 ; also article by F 
A. Cairns, Am. Chem., Vol. I, p. 82. 
Analysis No. 25.—Guano. 
To be determined: Si02, CaO, MgO, Fe203, P205, S03, 
H2O, NH3, total N, organic and volatile matter. 
A.—Determination of Moisture. 
Heat 1 grm. at ioo° C. until constant weight and loss= 
H.O[+(NH4).COJ. 
In cases where great accuracy is required, a correction 
for the (NH4)2CO3 counted as water must here be made. 
Heat the substance in a U tube in a water-bath and aspirate, 
collecting the (NH4)2CO3 in normal H2S04. Titrate with 
KHO as usual. Subtract (NH4)2CO3 found from HzO 
[-|-(NH4)2Co 3] determined by heating at ioo° C. as above. 
Determine loss by ignition in open crucible, and correct 
for H2O, (CO2) and (NH4)2CO3). 
B.—Organic and Volatile Matter. 
C.—Ammonia. 
Use Schlosings method, Fres., § 99, 3, b. Mix the guano 
with milk of lime and place under bell-jar over a dish of 
normal H2SQ4. A large surface of acid in proportion to 
the guano solution is desirable. Let stand, cold, 48 hours 
or more, and titrate with normal KHO as in acidimetry, 
(Cf. Analysis No. 11.) 
D.—Total Nitrogen. 
Use Varrentrapp and Will’s Method, as detailed in Fres., 
§ 185. Heat the guano in a combustion tube with sod? 
lime, converting it into NH3. Absorb the NH3 in a stand- 
ard solution of H2S04, aspirate and disconnect bulb. Add 
litmus and titrate with standard KHO. 
E-—Sulphuric Acid. 
Dissolve in hot HCI, filter and precipitate with BaCla, or' 
follow the Scheme F. GUANO 
89 
51.—Scheme for determination of Si02, A120, 
Fe203, CaO, MgO, 
and total P20„. 
Dissolve 5 grms. of guano 
in HNOs, evaporate to dryness, add HN03+H20, boil and filter. 
Residue a. 
Filtrate a. 
Si02 and 
silicates. 
Dilute filtrate and washings to 500 c-c., mix well, and divide into five unequal parts. 
Wash, dry, 
ignite, and 
weigh, o r 
fuse as in 
Analysis of 
dolomite. 
100 c. c. 
Reserve for 
accidents. 
100 c. c. 
Determine 
H2S04 with 
BaCl2 in the 
usual man- 
ner, if a du- 
plicate be 
desired. 
50 c. c. 
Determine 
the P2Os 
with a m- 
m 0 n i u m 
molybdate, 
as in Solu- 
tion g\ 
Analysis 
No. 21. 
50 c. c. 
Determine 
the P2Ob in 
duplicate. 
Cf. Note 
12 of Analy- 
sis No. 21. 
250 c.c. 
Add 1 grm. iron wire dissolved in HCI-f-HN03. 
Precipitate iron, etc., as basic acetates, as in 
Filtrate f Analysis No. 21. Wash the ppt., 
dissolve in HC1, dilute to 250 c. c., and divide 
into four unequal parts. 
50 c. c. 
Reserve for 
accidents. 
50 c. c. 
Determine 
total Fe by 
means of 
K2Mn208, 
and deduct 
20 per cent, 
fo r iron 
added. 
50 c. c. 
Determine 
the Fe in 
duplicate. 
For details 
see Analy- 
sis No. 3. 
100 c. c. 
Determine 
A1,03 as in 
Solution g2, 
Analysis 
No. 21, and 
in calculat- 
ing allow 
for the iron 
added. 90 
QUANTITATIVE ANALYSIS. 
Analysis No. 26.— Superphosphate of Lime. 
To be determined: Moisture, reduced (or reverted) 
P20s, soluble P20s and available P20s. 
A.—Determination of Moisture. 
Dry i grm. at ioo° and weigh—loss of weight=moisture. 
B.—Determination of Total P2Os, 
Weigh out 1 grm. accurately, mix with 2 grm. KN03 and 
4 grms. Na2COs, fuse in platinum crucible, dissolve in 
HN03, evaporate in a casserole to dryness (to dehydrate 
Si02-)-aq.), add water and filter. Wash thoroughly and 
dilute filtrate to 500 c.c.; take 50 c.c. of this solution 
(—O.l grm, of superphosphate) and determine P2Os with 
(NH4)2 Mo04 as usual. Consult Note 12, Analysis No. 21. 
C.—Determination of Insoluble P2Os. 
Digest 1 grm. with about 400 c.c. of water in 8 to 10 
different portions successively, rubbing the superphosphate 
with water in a porcelain mortar. Filter and treat residue 
(filter included) with about 50 c.c. solution of ammonium 
citrate containing 30 grm. of salt to 100 c.c. of water, and 
carefully neutralized if acid. Digest at about yo°C. for 40 
minutes or longer, filter and wash. Dry residue and fuse 
exactly as in B. Estimate the P20s in same manner using 
100 c.c. (=0.2 grm. of superphosphate) of the solution 
(500 c.c.) for each determination. 
D.—Determination of Reduced and Insoluble P2Os. 
Leach another sample (1 grm.) with water as in C 
(omitting the use of ammonium citrate), dry the residue 
and fuse as in B. Continue as in B, taking 150 c.c. of the 
solution for each determination. POTABLE WATER. 
91 
E.—Calculation. 
The reduced P205 is found by subtracting the P2Os in 
C from that in D. The soluble P2Os=B-D and the avail* 
.able P20s=B-C. 
Note.—Reduced or reverted P2Os forms thus: 
Ca3P208-j-CaH4P20B=2Ca2H2P208. 
Consult Balley's Handbuch, pages 802-806. 
Analysis No. 27.—Potable Water. 
To be detennined: K; Na; Mg; Ca; Cl; S03; Si02; 
organic and volatile matter, total 
solids; hardness (soap test) ; oxy- 
gen required to oxidize organic mat- 
ter (permanganate test). 
Quantity required, three to four gallons ; collect in clean 
demijohns. 
A.—Determination of Total Solids and Loss by Ignition. 
Measure out 250 c.c. of the water, evaporate to dryness 
on a water bath, in a weighed platinum dish of 100 c.c. ca- 
pacity. During the evaporation. cover the dish with a 
paper screen. Dry in an air bath I2o°-I3o° C. and 
weigh. Weight of residue gives “Total Solids.” Ignite 
gently over a Bunsen burner, moisten with a solution of 
C02 in distilled H2O, dry on water-bath, heat in air-bath 
I2o°-I3o° C. as before and weigh; difference between 
■second and first weights gives organic and volatile mat- 
ter, also called “ Loss by Ignition.” For further treatment 
■of residue see F. Compare Chapter II of Wanklyn’s 
■“ Water Analysis” 3rd edition, 1874. QUANTITATIVE ANALYSIS. 
B.—Determination of Si02, Fe203, A1203, CaO, HgO. 
Evaporate 4 to 6 litres of water (according to the 
proportion of total solids) to small bulk in porcelain 
dish. Add HCI, transfer to platinum dish, washing care- 
fully the porcelain dish, evaporate to dryness, filter from 
Si02 and follow scheme for Dolomite, Analysis No. 7, 
C.—Determination of H2S04. 
Take 1 litre (or less) of the water, boil down to 
200 c.c. with a few drops of HCI, and determine S04 
as BaS04 in the usual manner. If the water contains 
sufficient H2S04 (as sulphates) to give a feeble precip- 
itate with BaCl2 before concentration, one-half or one- 
quarter litre will suffice. 
Test the water with AgNOs for Cl, and if no cloud 
is formed evaporate 1 litre to small bulk; otherwise 25 
to 50 c.c. suffice. Add a slightly acid solution of AgN03, 
and proceed as usual. 
D.—Determination of 01. 
Second method. Determine the Cl volumetrically by 
a standard solution of AgN03, using potassium chromate 
as an indicator. See Fres. § 141,1, b, «. 
E.—Determination of Na and K. 
Evaporate 6 litres to dryness in a large porcelain dish, 
finishing on a water bath. Boil the residue with dis- 
tilled water several times, filter into a platinum dish 
and wash. Add Ba(HO), to filtrate. Evaporate to dryness, 
heat to low redness, let cool, take up with water, add 
(NH4)2COs and a little (NH4)C2O4, wash the precipitate, 
filter, add HCI to filtrate, evaporate to dryness, ignite 
and weigh. Dissolve in water and if not clear, filter, 
evaporate, dry, ignite cautiously, and weigh again. This POTABLE WATER. 
93 
residue of NaCl+KCl must be perfectly white and sol- 
uble without residue in water. Determine the Cl in the 
weighed NaCl-|-KCI and calculate the Na and K as in 
Fres. page 841. Compare Wanklyn, 3rd edition, page 63. 
F.—To check determination of Na and K. 
Moisten the weighed “ Total Solids ” of A with dilute 
H2S04, dry and ignite with a little powdered (NH4)2CO3 
to constant weight. By deducting from this weight, 
calculated fo7 one gallon, the combined weights of Si02, 
Fe203, A1203, CaO, MgO (the latter four reckoned as sul- 
phates), the weights of Na2S04 and K2S04 are obtained. 
GK—Dr. Clark’s Soap Test. 
Consult Sutton’s Volumetric Analysis, §83,10: or Wank- 
lyn's Water Analysis, 3rd edition, page 125. 
Principle.—Hard water, so called, destroys much soap 
before a lather is formed, owing to the formation of insol- 
uble salts, viz.: stearates, palmitates, and oleates of cal- 
cium and magnesium. 
Preparation of Soap Solutions.—Dissolve 10 grms. of 
good white Castile soap (which should contain about 
12 per cent, of water) in 1 litre of alcohol 90 to 95 
per cent. Let stand and siphon off from the residue. 
Label this solution “No. 1.” Take of solution No. 1, 
ico c.c.; of 56 per cent, alcohol, 65 c.c.; of distilled water, 
75 c.c., and mix. Label this soap solution “No 2.” 
Preparation of Standard Calcium Solution.—Dissolve 
1 grm. of precipitated CaC03 in HCI, evaporate until 
neutral, take up with water and dilute to 1000 c.c. 1 c.c. 
of this solution contains grm. 0.001 CaC03. 
Standardization of Soap Solution.—Fill a burette with 
soap solution No. 2. Place 10 c.c. of calcium solution 94 
QUANTITATIVE ANALYSIS. 
in a glass stoppered bottle. Add it to 100 c.c. of distilled 
water, run in soap solution from the burette and shake 
well, and continue adding soap solution until a lather 
is formed of sufficient consistence to remain for five 
minutes on the surface of the water. Read burette and 
calculate. Repeat. 
In certain cases allowance should be made for the 
amount of soap solution destroyed by water itself; 100 
c.c. destroys 0.8 c.c. soap solution. 
Performance of Analysis.—Same as above. Report mil* 
ligrammes per litre and grains per gallon of CaC03. 
Example.—ioc.c. of the standard solution of chloride of 
calcium required 23 c.c. of soap solution— 
But 10 c.c. of CaCl2 solution is equivalent to .01 grm. 
of CaC03, hence 
c.c. used) } .01 ) 
t i c.c. [ = V:a = .00043 grms 
23 ) ) grm. CaC03 ) 
And if 100 c.c. of water under examination require 
33 c.c. of CaCl2 solution, we have 33 X-00043 X 10 = grins, 
per litre of CaC03. This gives .1419; and .1419 X .058318 
gives grains per gallon. For the factor .058318 consult 
I, Calculation of Results. 
H. Permanganate Test for Organic Matter. 
Principle.—Permanganate of potassium in solution oxi- 
dizes putrescible organic matter. 
Preparaticn of solution of permanganate. - Dissolve 
0.320 grms. of permanganate in 1 litre of water. Dis- 
solve 0.7875 pure oxalic acid in 1 litre of water, weighing 
very accurately. Of this solution 1 c.c.=o.oooi grm. oxy POTABLE WATER. 
95 
gen. To standardize the permanganate, take 10 c.c. of 
oxalic acid solution; dilute to 100 c.c. with distilled water, 
add 5 c.c. dilute H2S04, heat nearly to boiling and run in 
from a burette the permanganate solution. 10 c.c. of 
oxalic acid will require 12 to 15 c.c. permanganate. Cal- 
culate value of 1 c.c. of latter in milligrammes of oxygen. 
Testing water.—Take 100 c.c. potable water add H2S04, 
add standardized permanganate, little by little in the 
cold, until the water retains a pink tinges after one-half 
hour’s standing. Report amount of oxygen required to 
oxidize organic matter. 
Example.—lo c.c. of standard solution of oxalic acid 
required 14 c.c. of solution of K2Mn208 
But 10 c.c. of H2C204 solution is equivalent to 0.001 
grms. of oxygen, hence 
c.c. used) ) I. mgm.) 
} : i. c.c. }■= \ :a .0713 mgms. 
14- J J oxygen J 
And if 100 c.c. of water under examination required 
0.8 c.c. of K2Mn2Os, we have 0.8X.0713X 10 = mgms. per 
litre of oxygen required to oxidize organic matter. This 
gives .5704 milligrammes and .5704 X.058318 gives grains 
of oxygen per gallon. See I, Calculation of Results. 
I.—-Calculation of Results. 
To convert grms. in a litre into grains in a gallon, multi- 
ply the number of milligrammes of each constituent by 
0.058318; or use Dr. Waller’s Table, published in Am. 
Chem., Vol. V, p. 278. Report results in two ways; the 
grains per gallon of uncombined constituents, viz., Si02, 
Fe203, A1203, CaO, MgO, Na20, K2O, Cl, S03, together 
with “ Loss by Ignition ” and “ Total Solids; ” and secondly QUANTITATIVE ANALYSIS. 
report the grains per gallon of the bases combined with 
acids in accordance with the following scheme. 
Combine K as K2 S04 
excess of K “ KCI 
“ “ “ Cl “ Na Cl 
“ “ “ Na “ Na2S04 
“ “ “ Cl “ Mg Cl2 
“ “ “ S04 “ Ca S04 
“ “ “ Ca “ Ca C03 
“ “ “ Mg “ Mg COa. 
The sum of the combined salts -j- “ Loss by Ignition ” 
should equal the “Total Solids” very nearly. 
Example, showing method of calculation.—A sample of 
potable water yielded on analysis the following results: 
Cl .215 grains per gallon. 
Na .291 
S03 .340 
CaO .804 “ “ “ 
etc. etc. 
Begin by calculating the amount of Na required to 
saturate the Cl found, thus: 
(1) Cl :Na = J Amount 1 J Amount of Na 
[of Cl found./ * [needed for the Cl. - 
.35-5 :23 = 0.215 : w 
w 0.139 grains, 
hence 0.215 -f- 0.139 = 0.354 grains NaCl. 
But the water contains .291 grains Na, hence we have 
.291 .139 = .152 grains Na left over to combine with 
S03. POTABLE WATER. 
97 
0152 grains Na corresponds however to 0.204 grains 
Na20 making then a proportion similar to (1) we have 
(2) Na20 : S03 = Amount Amount of SOs 
- of NazO ■ : - needed 
remaining, j for the Na20. 1 
62 :80 = 0.204 : x 
x = 0.263 grains, 
hence 0.204 -f- 0.263 0.467 grains Na2S04. 
x = 0.263 grains. 
But the water contains 0.340 grains S03 hence we have 
0.340 0.263 = 0.077 grains S03 left over to combine 
with CaO. 
Accordingly we have the proportion 
(3) f S03: CaO = f Amount of SOs 1 f Amount of CaO 1 
| remaining. \' \ needed for the S03. [ 
80 : 56= 0.077 : y j 
y 0.0539 grains CaO, 
hence 0.077 -}- 0.0539 = 0.130 grains CaS04. 
Proceeding in like manner the CaO remaining is regarded 
as combined with C02. 
0.804 —0.0539 0.7501 grains CaO ; and since. 
(4) f CaO : CaC03 = 0.7501 : z 
[ whence z = 1.34 grains CaC03. j 
Collecting the results of the calculation we have (thus 
far) the following figures for the constituents combined: 
NaCl = 0.354 grains per gallon. 
Na2S04 = 0.467 “ “ “ 
CaS04 = 0.130 “ “ “ 
CaC03 = 1.34 “ “ * 
etc., etc. 98 
The following will serve as a further example of the 
manner of reporting similar analyses. 
QUANTITATIVE ANALYSIS 
Analysis of Croton Water by Dr. C. F. Chandler. 
Grains per gallon. 
Soda 0.326 
Potassa 0.097 
Lime 0.988 
Magnesia 0.524 
Chlorine ....... 0.243 
Sulphuric acid ...... 0.322 
Silica 0.621 
Alumina and oxide of iron trace 
Carbonic acid (calculated) . . . 2.604 
Water in bicarbonates (calculated) . . 0.532 
Organic and volatile matter . . . 0.670 
6.927 
Less oxygen equivalent to the chlorine . .054 
Total . . . 6.873 
These acids and bases are probably combined as follows; 
Grains per gallon. 
Chloride of sodium 0.402 
Sulphate of potassa o. 179 
Sulphate of soda 0.260 
Sulphate of lime 0.158 
Bicarbonate of lime ..... 2.670 
Bicarbonate of magnesia .... 1.913 
Silica ....... 0.621 
Alumina and oxide of iron trace 
Organic matter 0.670 
6.873 Analyses No. 28 and No. 29. Specific Gravities of 
Solids and Liquids. 
SPECIFIC GRAVITIES OF SOLIDS AND LIQUIDS. 
A—Sp. gr. of a solid by direct weight. 
Weight of solid in the air = w 
“ “ “ “ water =w1 
w 
Sp. gr. = 
w w1 
B.—Sp. gr. of a solid by the flask. 
Weight of solid = w 
“ “ flask -f- water =w1 
“ “ “ “ “ solid =w” 
w 
Sp. gr. = 
(w -f- w1) wll 
O,—Sp. gr. of a body soluble in water. 
Weight of body in air = w 
“ “ “ “ oil =w1 
Sp. gr. of oil = a 
“ “ “ water = i 
The liquid displaced being 
w w1 = wll 
then 
a: i = w" : w”1 
w 
Sp. gr. = 
wlll 
D.—Sp. gr. of a body lighter than water and insoluble 
in it, e.g., Cork. 
Weight of cork in air = w 
“ “ lead “ water = w1 
“ “ “ and cork in water =w" QUANTITATIVE ANALYSIS. 
Sp-Sr= w,_^'+w 
E. Sp. gr. of a Body lighter than Water and soluble in it. 
Weight of body in air = w 
“ “ “ “ naphtha =w' 
w—w' = w" 
Sp. gr. of naphtha = A 
“ “ “ water = i 
A : w"= i : w'" 
0 w 
bp. gr. = 
° w'" 
P. Determination of the Proportion of two Metals in an 
Alloy. 
Sp. gr. of the alloy = S 
Weight of the alloy = A 
Sp. gr. of one of the metals = s' 
Sp. gr. of the second metal = s" 
Weight of one metal = w' 
Weight of the second metal = w" 
w' = A Ls'—s">s' 
(s'—s")S 
w" = A—w' 
For proofs of this formula, see Gallozvay s First Step in 
Chemistry, p. 74. 
G. Sp. gr. of a liquid by the flask 
Weight of flask = F 
“ “ “ and water = w 
“ “ “ liquid =w/ ORGANIC ANALYSIS. 
W7—F 
Sp. err. 
1 & w—b 
H. Sp. gr. of a Liquid by weighing a Substance in it. 
Weight of substance = w 
“ “ “ in liquid w7 
Sp. gr. of the substance = A 
w : (w—w') = A : sp. gr. 
c f w—w') A 
or Sp. gr. = i L— 
w 
Analysis No. 30, 31, and 32. Organic Analysis. 
Introductory Notes. The analysis of organic bodies 
comprises two branches ; Proximate Analysis which deals 
with the separation of proximate principles of organic bodies 
without altering them, and Ultimate Analysis, by which 
the nature and quantity of the elements composing the 
organic bodies are determined. 
No systematic course of proximate analysis is possible 
in the present state of the science; animal chemistry is in 
this respect more advanced than vegetable ; for a course of 
zoo-chemical analysis see article by Gornp-Besanez in the 
Neues Handworterbuch der Chemie, I, 551, and compare 
Watt's Dictionary, I, 249. See also Heintz Lehrbuch der 
Zoochemie and Lehmans Physiological Chemistry. For 
general principles of proximate organic analysis, consult 
Dr. Albert B. Prescott's “ Outlines of Proximate Organic 
Analysis,” a most useful manual, and the only one of its 
kind. For special methods of analyzing organic bodies, 
especially of commercial articles, consult “ Balley s Hand- 
buch der Technisch-chemischen Untersuchungen,” of which 
the second edition by Emil Kopp is most valuable. 102 
QUANTITATIVE ANALYSIS. 
The method of conducting an ultimate analysis is suffi- 
ciently detailed in Fresenius’ System, § 171-189, yet the 
following summary may be of service in calling attention 
to the chief points. 
A. Determination of C, H, and O, in Sugar. 
Select a very pure well crystallized sample of sugar, rock- 
candy will do, but small crystals from a vacuum pan are 
better. Dry at ioo° C, in powder. 
Provide the following articles : 
(1) The dried substance in a tared watch glass. 
(2) Combustion tube of hard glass drawn out as shown 
in Fres. § 174, cleaned and carefully dried. 
(3) Liebig potash bulb filled with a KHO solution of 
Sp. gr. 1,27, or a U-tube filled with soda-lime. 
(4) Chloride of Calcium tube ; that of the form described 
by Thorpe in his Quant. Chem. Analysis page 347, fig. 80 is 
advantageous. 
(5) Small U-tube containing potash-pumice in one limb 
and CaCl2 in the other. 
(6) Rubber tubing. 
(7) Fine wire for binding the tubing. 
(8) Good corks, free from holes, rolled and pressed. 
(9) Cupric oxide, granulated preferred, chemically pure, 
freshly ignited to remove organic matter and moisture, and 
contained in a corked holder. 
(10) A platinum boat to contain the substance, or if 
another process be followed, a mixing wire. 
(11) Combustion furnace. 
(12) If oxygen is to be employed, a cylinder of this gas 
and a system of drying U-tubes must be provided. ORGANIC ANALYSIS, 
103 
(13) Sundry articles, such as glazed paper, agate mortar, 
towel, asbestus, a ramrod for cleaning combustion tube. etc. 
Process of the Combustion. 
(a) Weigh the substance (sugar) and preserve in a des- 
iccator until ready for use ; weigh also the KHO bulb to- 
gether with the U-tube (5), CaCl2 tube. 
{b) Dry the combustion tube and fill with cupric oxide ; 
the substance may be inserted on a platinum boat if the 
combustion is to be conducted with oxygen, otherwise it 
must be intimately mixed with some powdered CuO in 
the agate mortar and transferred by the glazed paper to 
the combustion tube. Stir also with the iron mixer. Avoid 
introducing moisture. 
(<:) Connect the apparatus, arranging it as shown in the 
cut on page 433 of Fresenius' System. Test the joints by 
heating the air in that bulb of the KHO apparatus which 
is between the solution and the combustion tube ; drive 
out a few bubbles of air and let cool, if an unequal level 
of the solution is maintained, the joints are tight. 
(1d) Conduct the ignition, heating gradually, and begin- 
ning at the end next to the CaCl2 tube ; do not apply heat 
to the substance until several inches of CuO are red hot. 
Pass oxygen gas through the tube if that method is em- 
ployed. Fres. § 178. The combustion of sugar may be 
completed in about half an hour, other substances require 
more time, especially those rich in Carbon. 
(e) Aspirate air, or pass oxygen through the apparatus 
slowly. 
(f) Disconnect the weighed tubes, cool and weigh. P'rom 
the C02 and the H2O found, calculate the C and the H 
respectively. The Ois found by difference. 104 
QUANTITATIVE ANALYSIS. 
Theoretical Composition of Cane Sugar. 
Ci 2 144 . . . . 42.11 
Ha 22 ... . 6.43 
On 176 ... . 51.46 
342 100.00 
In the case of nitrogenous bodies introduce copper turn- 
ings or a spiral of sheet copper in the end of the combus- 
tion tube next to the absorption tubes ; the metallic copper 
at a red heat reduces any nitric oxide which may form, and 
the inert nitrogen passes through the absorption tubes 
without increasing their weight. See Fres. § 183.2. 
The difficulty of effecting a complete oxidation of the 
carbon in organic substances increases, other things being 
equal, with the percentage of carbon contained in the sub- 
stance ; the richer the substance in carbon, the smaller the 
amount should be taken for combustion. Moreover, it is 
desirable to graduate the quantity used, to prevent the for- 
mation of too large a quantity of carbonic anhydride to 
admit of complete absorption by the potash solution ; hence 
the following Table, used in Prof. A. W. Hoffman’s Labo- 
ratory, University of Berlin, is of service in determining 
the amount of substance which may be conveniently em- 
ployed. 
Table showing amount of Substances to be used in 
Ultimate Analysis. 
Of substances containing 80 percent carbon take o.2oogrms. 
“ “ 75 “ “ “ 0.225 “ 
“ “ 70 “ “ “ 0.250 “ 
“ “ 65 “ “ “ 0.275 “ 
“ “ 60 “ “ “ 0.300 “ 
niC hr* a a a 
s:> °-32 5 DETERMINATION OF NITROGEN. 
105 
Of substances containing 50 percent carbon take 0.350 grms. 
u u 45 u U u 0.375 U 
u u 40 u u u “ 
u u 25 11 11 u 0.425 “ 
u u 20 “ u u 0.450 u 
Cl u 25 u u u 0.475 “ 
“ 11 20 11 u “ 0.500 “ 
CJ. Determination of Nitrogen in Potassium Ferrocy- 
anide by Conversion into Ammonia. 
Method of Varrentrapp & Will. See Fres. § 185. 
Purify about 50 grms. of the commercial salt by recrys- 
tallization ; dry the crystals on filter paper and preserve in 
a desiccator. The crystallized salt contains 3 molecules 
of water. 
Principle: When organic substances are heated with 
hydroxides of the alkaline metals the carbon is oxidized by 
the oxygen of the hydroxide, and hydrogen is set free ; if, 
however, nitrogen is present it combines with the nascent 
hydrogen, forming ammonia. (For an exception, see D.) 
By conducting the operation in such a way as to complete 
the reaction, and collecting all the ammonia by absorption 
in acid of known strength, the amount of nitrogen is 
easily calculated. 
Requisites: The apparatus needed is, in general, the 
same as that used in determination of C and of H, but 
a somewhat shorter tube (40 cm.) may be used ; the am- 
monia is absorbed by normal sulphuric acid placed in pear- 
shaped bulbs of the form shown in Fig. 92, or Fig. 94, 
pages 443 and 445 of Fres. System. The substance used 
to oxidize the carbon is soda-lime, at present a commercial QUANTITATIVE ANALYSIS. 
article ; it should be heated in a porcelain dish to expel 
water and ammonia before using. 
Operation: Fill the combustion tube about one-third full 
of warm soda-lime and let it cool ; then mix this in an 
agate mortar with 0.2 to 0.4 grms. of the dry ferrocyanide 
of potassium, and introduce the mixture again into the 
tube ; rinse the mortar with a little soda-lime, and then 
fill the tube with the same nearly to the open end. Insert 
a small plug of asbestos loosely, attach the absorption bulb 
containing the sulphuric acid by a well-fitting cork, and 
place the tube in the combustion furnace. Begin to heat 
the tube at the end nearest the cork, and proceed gradu- 
ally towards the other end. 
The gas evolved should bubble quietly through the ab- 
sorption tube, and when it ceases to pass break the tail- 
piece of the combustion tube, and aspirate gently through 
the whole apparatus. 
Detach the absorption tube, empty its contents into a 
beaker, rinse well, add a little litmus, or cochineal solu- 
tion, and determine, by means of normal KHO, the 
amount of acid remaining unneutralized by the ammonia. 
For details of this process see Analysis No. 12, 
Theoretical Composition of Potassium Ferrocyanide: 
Q iy.i 
N6 19.9 
Fe 13.3 
K4 37.0 
3H20 12.7 
100.0 DETERMINATION OF NITROGEN. 
Dumas' method modified by Melsens, Cf. Fres. § 184. 
See also Watts’ Dictionary, I. 242. 
D. Determination of N from the Volume. 
When nitrogen exists in an organic substance in the form 
of an oxide, e.g. nitro-benzol C 6H5 (NQ2), Varrentrapp & 
Will’s method cannot be employed because the oxides of 
nitrogen are not completely converted into ammonia on 
heating with soda lime. Dumas’ method consists in heat- 
ing the substance with oxide of copper, and measuring the 
nitrogen evolved by collecting over mercury. The process 
originally devised by Dumas necessitated the use of an air- 
pump to exhaust the combustion tube, but this may be 
obviated by following Melsens, who introduces hydro- 
sodium carbonate into the tube which gives up carbonic 
anhydride on heating, and drives out the nitrogen before it. 
For Melsen’s process provide the following articles : 
(r) A combustion tube 70 cm. long. 
(2) Mercury trough. 
(3) Graduated cylinder, 
(4) Copper oxide. 
(5) Solution of potassium hydrate. 
(6) Hydrosodium carbonate. 
(7) Connecting tube. 
(8) Corks, asbestos, rubber tubing, etc. 
(9) Combustion furnace. 
In filling the combustion tube observe the following 
order: Insert, first, 15 cm. of hydrosodium carbonate, then 
5 cm. of copper oxide, then 15 cm. of copper oxide mixed 
with the substance to be analyzed, next add about 28 cm. 
of copper oxide, insert a copper spiral 5 cm. long, and 
lastly a plug of asbestos in the remaining 2 cm. Insert 
cork with connecting tube, and arrange apparatus as shown 
in Fig. 93, page 635, of Fres. System. QUANTITATIVE ANALYSIS. 
Conduct the operation as follows : Heat a portion of the 
NaHCOs until all the air is expelled ; test with a solution 
of KHOinan inverted test-tube; then heat CuO to red- 
ness, arrange the graduated cylinder containing KHO solu- 
tion over mercury, and heat the mixed CuO and substance 
until gas ceases to come off; lastly, expel the nitrogen in 
the combustion tube by again heating the NaHC03, some 
of which must have been left undecomposed. (Oxalic acid 
may be substituted for the HNaC03. See Thorpe, page 
332.) Transfer the graduated cylinder to a vessel of 
water, hold it so that the level of the water within the 
cylinder and without is equal, then read off the volume of 
the gas in cubic centimeters, and simultaneously the tem- 
perature of the water and the height of the barometer. 
Calculation of Results. To obtain the weight of nitro- 
gen from its volume employ the following formula : 
Let V = Volume of N observed, expressed in cubic centi- 
meters. 
And t°= Temperature of the gas. 
“ B = Height of the barometer expressed in millimeters. 
“ f= Tension of aqueous vapor at the temperature t°, 
expressed in mm. of mercury. 
Then if W = weight of nitrogen we have : 
i B —f 
W = .0012566 V - —- 
i-f-00367t° 760 
The constant 0.0012566 is the weight in grammes of 
Ic.c.ofN at o° C and 760 mm. The constant 0.00367 is 
the coefficient of expansion of gas. 
Example : In an analysis of Butvramide 
C 4H70) 
H V N, the following data were obtained : 
Hj ANALYSIS OF URINE. 
0-315 grms. of substance gave 43.9 c. c. Nat /°=l7°3 C 
and B = 753.2 mm. 
First look out in a table the value of fat i7°-3. {Fres.y 
page 837, Table.) We find (calculating for the tenths of a 
degree)/= 14.7. 
Now V = 43.9 c. c. 
B f =753.2 mm. 14.7=738.5 mm. 
And 1 + ,00367 X t° = 1.0635. 
Substituting in equation : 
j jg £ 
W = .0012566 V —7 —o —?— we have : 
J 1+.003671 760 
~7 .0012566X43.9X 738.5 _T 
W = -—— - = 0.0504 grms. N. 
1.0635 x 760 d 
* ,0.0504X100 , . 
And —0315 = I°‘°° Per cent nitr°gen* 
Theoretical Composition of Duty ramide 
c4 
55-2 
h9 .... 
10.3 
0 
18.4 
N 
100.0 
For brief methods of analysis consult Dr. George B. 
Fowler’s “ Urine Analysis,” Thudicum’s “ Manual of Chem- 
ical Physiology,” pages 178-192, and Sutton’s “ Systematic 
Handbook of Volumetric Analysis,” part vi. § 78. For 
figures of sedimentary deposits examine Ultzmann & Hof- 
mann’s “Atlas der Physiologischen und Pathologischen 
Harnsedimente.” (44 plates.) 
Analysis No. 33, Urine. 
The following works may also be studied: Legg’s 
‘ Guide to the Examination of Urine,” Attfield’s “ Chem- QUANTITATIVE ANALYSIS. 
istry,” F. Hoppe-Seyler’s “ Handbuch der Physiol, and 
Pathol. Chem. Analyse,” Neubauer & Vogel’s “ Anleitung 
zur Qualitative und Quantitative Analyse des Hams,” 
Gorup Besanez’ “ Lehrbuch der Physiologischen Chemie,” 
pages 576-580, Ultzmann & Hofmann’s “Anleitung zur 
Untersuchung des Hams.” 
Constituents of Urine. 
Urine, the secretion of the kidneys, in a healthy individ- 
ual, is a clear, yellowish, fluorescent liquid of a peculiar 
odor, saline taste, with a mean sp. gr. 1.020. The follow- 
ing are its normal constituents : 
1. Water. H2O. 
2. Inorganic Salts. —K, Na, NH, Ca, Mg, combined with 
HCI, H3P04. H2S04, C02, (HNO3,) and Si02. 
3. Nitrogenous crystalline bodies.— Urea, uric acid, hip- 
puric acid, creatine, creatinine, xanthine, (ammonia,) 
cystine. 
4. Non-nitrogenous organic bodies. Sugar, lactic, succinic, 
oxalic, formic, malic, and phenylic acids, all in small 
quantities. 
5. Pigments.— Urochrome, urohaematin. 
6. Albumenoid matters. 
y. Matters derived directly from the food. 
Besides these, urine may contain, under varying cir- 
cumstances, as in disease, a large number of 
8. Abnormal constituents.— Blood, pus, mucus, albumen, 
fibrin, casein, fats, cholesterin, leucine, tyrosine, allan- 
toin, taurine, biliary pigments, indigo-blue, melanin, 
glucose, inosite, acetone, butyric acid, benzoic acid, 
oxaluric acid, taurocholic acid, glycocholic acid, and 
many others. (See Watts’ Dictionary, vol. v. p. 962.) ANALYSIS OF URINE. 
These substances do not occur simultaneously in all 
urine, and many of them but rarely. Only those com- 
monly determined are considered in the Scheme 
(page 112). 
Chemical Composition of Urine. (Dalton.) 
Healthy. — Numbers Approximate. 
Water 
938.00 
Urea 
30.00 
Creatine 
1.25 
Creatinine 
1.50 
Urate of soda ) 
“ potassia >- . . 
1.80 
“ ammonia ) 
Coloring matter and mucus 
.30 
Bi-pbosphate of soda 
Phosphate of soda 
“ potassa 
12.45 
“ magnesia 
“ lime 
Chlorides of sodium and potassium . . . 
7.80 
Sulphates of soda and potassa 
6.90 
1000.00 
Morbid urine may contain, also: 
Albumen, (Bright’s disease.) 
Sugar, (Diabetes.) 
Bile, 
Excess of Urea, 
Oxalate of calcium. 112 
QUANTITATIVE ANALYSIS. 
Action of Reagents on Urine. 
Boiling acid urine effects no change. 
Boiling alkaline urine makes it turbid if rich in earthy 
phosphates. 
HNOgOr HCI darkens the color, and throws down uric acid 
on standing. 
KHO or NH4HO throws down earthy phosphates. 
BaCl2 or PbA, in acidified urine, yield a white ppt. of sul- 
phates. 
AgN03 white ppt. of chlorides, also coloring matter and 
some organic substances. 
Murexid Test. Collect some of the uric acid thrown 
down by HCI, remove supernatant liquid, add cone. 
and evaporate to dryness. When cold add a drop of NHr 
HO. A purplish-crimson color shows formation of mur- 
exid (QH N606). 
Reactions of Urea. —Hg (N03)2 throws down a gelati- 
nous white ppt. containing COH4N2 .2HgO. 
Boiling with KHO converted into NHJfO ; test with 
Nessler reagent. 
HNOg, nitrate of urea precipitates. 
NaCIO or NaßrO decomposes urea with evolution of N.. 
Scheme for Analysis of Urine. 
1. Physical Characters. 
(a) Odor. Certain peculiarities in odor indicate either 
nature of food or symptoms of disease. 
(b) Consistence.—Viscous or fluid. 
(c) Color.—When healthy, urine is amber-colored ; when 
bilious, brown or greenish. 
(d) Specific Gravity. —By the urinoraeter, 1015 to 1025 
is marked H. S., signifying Healthy State. 40 c. makes a 
difference of about i° in the reading. ANALYSIS OF URINE. 
2. Test with Litmus Paper, and note whether acid or 
alkaline. 
3. Pour a sample into a stop-cock funnel, and let stand 
12 hours. If a deposit forms, filter, and examine the filtrate 
and sediment separately. Filtered urine leaves a scum of 
mucus. (For sediments, see Schemes, page 117 and 118.) 
4. Determine Total Solids. Evaporate 4t06 c. c., 
weighed, to dryness in a weighed dish. Dry at 115 c. (In- 
accurate). 
5. Ash. Evaporate 100 c. c. urine and ignite residue. 
6. Determination of Urea, CH4N20. 
A. Liebigs Method. 
Principle: Mercuric nitrate added to a solution of urea 
gives a white, gelatinous ppt. containing I molecule urea, 
and 2HgO. (Absence of NaCl necessary.) 
Requirements: 
(a) Standard solution Hg (N03)2. 
(b) Baryta solution. 
(e) Carbonate of soda test paper. 
(a) Standard solution of mercuric nitrate. Dissolve 
72 grms. pure dry HgO in strong HN03, (50 grms.,) 
evaporate until syrupy, and dilute to 1 litre. If a yellow 
ppt. is produced by dilution, too little acid is present. It 
must be evaporated down, fresh acid added, and again di- 
luted. Ic.c. = 0.01 grm. urea. To test the strength of 
the mercuric nitrate dissolve 2 grms. cryst. urea in 100 c. c. 
water. Ic. c. mercuric solution should equal 0.01 grm. urea. 
(b) Solution of Ba(No3)2+BaH2o2. Mix 1 part cold 
saturated solution 8a(N03)2 with 2 parts cold saturated 
solution BaH202, and add 3 parts distilled water. 
(e) Soda test paper. Dip a sheet white filter paper into 
cone. sol. Na2(C03) and dry. 114 
QUANTITATIVE ANALYSIS. 
Process: Collect the urine passed during 24 hours, and 
measure carefully. Place 20 c. c. in a small beaker, add 
20 c. c. barium solution, filter from the sulphates and phos- 
phates. Of the filtrate 20 c. c. (containing 10 c. c. urine) 
are measured off, a drop of AgNOa added to precipitate 
excess of chlorides, and then standard solution of mercuric 
nitrate is added until a drop of the mixed solutions gives a 
yellow stain (of mercuric hydrate) on the test paper. 
Byasson adds some of a solution of KHO (25 grms. to 1 litre 
water) from time to time to partly neutralize the acid set 
free. The solution must not be rendered alkaline. 
Calculation: Amount urine passed in 24 hours = A ; 
c. c. mercuric solution used = C ; each c. c. being equal 
A x C 
to 0.01 grm. urea ; then = grms. urea passed in 24 
hours. 
Caiition: The urine must be free from phosphoric and 
hippuric acids. Consult Caldwell’s “Agricultural Analy- 
sis,” page 220. Urine must contain 2 per cent. urea. Cf. 
Watts’ Diet, vol, v. p. 967. 
B. Davey s Method of Estimating Urea. 
Pour a small quantity of urine into a graduated glass 
tube one-third full of mercury. Fill the tube with a solu- 
tion of sodic hypochlorite, close tube, and invert quickly 
over a saturated solution of NaCl. Let stand several hours 
while the following reaction ensues : 
CH,N2O4-3(NaCIO)=CO2+2H2O + 3NaCI+N2 
Read off the quantity of N. 1.549 cubic inches of Nat 
6o° Fah. and 30" bar. = i grain urea. 
Method inaccurate since ammonia, uric acid, &c., are 
likewise decomposed. ANALYSIS OF URINE. 
C. Heintz and Ragsky s Method. 
First determine ammonia by precipitation with PtCl4. 
Heat 2 to 5 c. c. with equal vol. H2S04 in a covered cap- 
sule to iBo°-200°. Cool, dilute with water, filter, and de- 
termine NH3 formed by PtCl4. Calculate both amounts for 
100 c. c., and take the difference ; this multiplied by 0.13423 
gives per cent, of urea. 
Results very accurate. 
D.—Apjohns Method. 
See “American Chemist,” V. 431. 
Provide the following apparatus : 
(1) A glass tube 30 cm. long, subdivided into 30 equal 
parts, whose aggregate volume is 55 c. c. The end of the 
tube is drawn out like a Mohr’s burette. 
(2) A wide-mouthed gas bottle of 60 c. c. capacity. 
(3) A test tube of 10 c. c. capacity, and long enough to 
be slightly inclined when introduced into the gas bottle. 
The principle of the process is based upon the following 
equation : 
2(CON2H4)+3(CaBr2O2)=3CaBr2-f 2CO2+N4 
To make the hypobromite solution take loogrms. NaHO, 
250 c. c. H2O, and add 25 c. c. bromine ; agitate and set 
aside for use. 
Process : Into a glass cylinder containing water the tube 
(1) is depressed till the zero mark and surface of water 
coincide. 15 c. c. hypobromite solution (100 grms. NaHO, 
250 c. c. H2O, 25 c. c. Br) are placed in (2) and the test- 
tube containing the urine is introduced carefully to avoid 
spilling its contents. The flask is closed by a perforated 116 
QUANTITATIVE ANALYSIS. 
stopper which is connected by tubing with the measuring 
tube. The urine is now mixed with the hypobromite, and 
the disengaged nitrogen is driven into the measuring tube. 
The tube is now levelled to relieve hydrostatic pressure, 
and the volume of nitrogen read off. Since 55 c. c. equal 
0.15 grm. of urea, a single division corresponds to 
=0.005 grm* urea. 
(0.15 grm. urea gives 55 c. c. nitrogen at 6o° Fah. and 
30° bar.) 
7. Determination of Actual Ammonia. Takecoc.c. 
filtered urine and treat by Schlosing’s method. 
The NH3 is expelled by milk of lime, and absorbed by 
standard acid, in the cold under a bell jar. For details see 
Fres. § 99, 3b. (Human urine contains 0.078 to 0.143 per 
cent.) 
8. Determination of Albumen, Measure urine 
passed in 24 hours. Drop 50 c. c., one c. c. at a time, 
into 1 ounce boiling distilled water in a porcelain dish. 
If the urine was alkaline add a drop of acetic acid, avoid 
excess. Allow the coagulated albumen to settle, filter 
through a weighed filter, and wash well. Dry at ioo° C, 
and weigh. 
9. Determination of Sugar. Dilute urine 5 or 10 
times, and apply Fehling’s solution as in grape sugar. See 
Analysis No. 35, Raw Sugar. 
10. Determination of Phosphoric Acid. To 50 c. c. 
filtered urine add 5 c. c. sodic acetate and titrate with 
uranic acetate. For details see Sutton’s “ Volumetric 
Analysis.” 
11. Determination of Uric Acid.—To 200 c. c. 
urine add 10 c. c. HCI, stand 48 hours in a cool place, DETERMINATION OF URINE. 
filter on a very small weighed filter. Wash-water should 
not exceed 30 c. c. If more is necessary add 0.045 mgm. 
uric acid for each c. c. additional. (Albumen must first be 
removed by coagulation.) Dry at ioo°c. and weigh. 
12. Tests for Bile. 
(1) Place a little urine on a white plate, add HN03. A 
peculiar play of colors —green, yellow, violet, &c. —occurs 
if coloring matter of bile is present. 
(2) Agitate concentrated urine with boiling ether. If 
Bile is present the ether solution will be greenish-yellow. 
(3) Add baric acetate to urine, treat the ppt with alco- 
hol, decompose it with HCI, and evaporate the liquid to 
■dryness. Water will dissolve out in the residue coloring 
matter of the bile. 
(4) Pettenkofer s Test.—Mix fluid with one-half vol. H2S04, 
avoiding rise of temperature ; add a little powdered cane 
sugar ; mix and add more H2S04. Liberation of cholalic 
acid produces a purplish-red coloration ; this gives a pecul- 
iar absorption spectrum. See Thudichura’s “ Manual.” 
Scheme for analysis of Urinary Sediments. (Attfield.) 
Warm the sediment with the supernatant urine, and filter. 
INSOLUBLE. 
Phosphates, oxalate of calcium and uric acid. 
Warm with acetic acid, and filter. 
SOLUBLE. 
Urates of Ca, Na, 
and NH4, — 
chiefly of Na. 
They are re-depos- 
ited as the liquid 
cools, and if suffi- 
cient in quantity 
may be exam- 
ined for uric 
acid and bases 
by usual tests. 
INSOLUBLE. 
Oxalate of calcium and uric acid. 
Warm with HC1, and filter. 
SOLUBLE. 
Phosphates. 
Add NH4HO, 
and exam- 
ine ppt. 
for P0O5, 
CaO and 
MgO. 
INSOLUBLE. 
Uric acid. Apply 
murexid test. 
SOLUBLE. 
Oxalate of cal- 
cium. May 
be pptd. by 
NH4HO. 
Note. — Urates are often of a pink or red color, owing to the pig- 
ment purpurine. This is soluble in alcohol. QUANTITATIVE ANALYSIS. 
Scheme for Determination of Urinary Sediments by Chemi-« 
cal Tests. (Attfield.) 
The sediment is white; warm 
with the supernatant urine 
and filter. 
and and amorphous 
crystalline easily soluble 
uric acid, on heating 
urates. 
The sediment is colored 
Solution 
contains 
urates. 
Residue 
Treat with ammonia. 
and 
amorphous, 
slowlv solu- 
ble on heat- 
ing. Urates 
colored by 
purpurine. 
Solution | Residue 
contains [Treat with 
cystine. / acetic acid. 
Residue Solution. 
oxalate and Add NH4 
oxalurate HO white 
of calcium, ppt. of 
earthy 
phos- 
phates. 
Analysis No. 34. Milk. 
Wash quartz sand thoroughly with HCI and water, and 
ignite. Put about one-quarter inch of this sand in a plati- 
num pan, weigh, and pour on 3 to 5 grms milk. Dry at ioo° 
C. to constant weight. 
A. Determination of Water. 
Break up the cake from residue A and wash the butter 
out with ether into a weighed beaker, evaporate the ether 
and weigh the butter. 
B Determination of Butter. 
C. Determination of Sugar. 
Collect the residue from B on a dried and weighed filter, 
dry it at ioo° C, boil it four or five times with fresh por- 
tions (150 c.c. each) of 80 per cent, alcohol, and dry the 
insoluble residue at ioo° C. and weigh on a tared filter. 
The loss of weight gives the sugar approximately. Or 
determine sugar as under grape sugar, Analysis No. 35. DETERMINATION OF SUGAR. 
A convenient apparatus for the extraction of sugar is 
described by Prof. S. W. Johnson, in Am. J. of Sci. (3) xiii, 
page 196(1877). 
D. Determination of total Non-volatile Matter. 
Evaporate 10 to 20 grms. milk to dryness, with the 
addition of a little acetic acid, and ignite the residue in a 
muffle furnace, at the lowest possible temperature. 
Subtract the sum of the butter, sugar, and ash from the 
total dry substance, and the remainder is chiefly casein. 
E. Determination of Protein Compounds. 
For other methods, see “A Method for the Analysis of 
Milk,” by E. H. von Baumhauer, Am. Chem., Vol. VII., 191. 
Analysis No. 35. Raw Sugar. 
CiaH^Ou 
A. Determination of Moisture. 
Heat a weighed amount of sugar at 1 io° until it no 
longer loses in weight. Loss = moisture. 
E.— Determination of Ash. 
Weigh off ten grms. in a platinum dish. Either burn the 
sugar direct, or add a few drops of cone. H2S04 and heat 
very cautiously in a gas muffle. Weigh the ash. 
The two methods do not give results at all concordant; 
the latter is the French method, and the results are called 
“ the salts,” after subtracting one-ninth, but this is seldom 
correct, though the ash burns very white. 
C.— Determination of Grape Sugar. 
c 6h12o0, h2o 
(1) Qualitative reactions. Glucose is colored dark- 120 
QUANTITATIVE ANALYSIS. 
brown when heated with a strong solution of sodic hy- 
drate. It dissolves in cold cone. H2S04 without being 
blackened. [Cane sugar blackens.] 
If a cone, solution of glucose is mixed with cobaltic 
nitrate, and a small quantity of fused NaHO, the solution 
remains clear on being boiled ; if very concentrated it de- 
posits a light-brown ppt. 
[Cane sugar solutions similarly treated give a violet ppt., 
which turns green on standing]. 
BaH202 added to an alcoholic solution of glucose forms 
a white ppt. 
If a little caustic soda is added to a solution of glucose, 
and then drop by drop a dilute solution of CuS04, a deep- 
blue liquid forms ; after some time in the cold, but imme- 
diately if heated, a yellowish or red ppt. of hydrated cuprous 
oxide is deposited. yinKoTtf °f glucose may be easily de- 
tected ; T,ooiooo still gives a red tint to the solution. 
Cupric acetate is similarly reduced. Potassio-tartrate of 
copper acts likewise. 
(2) Quantitative estimation. 1 eq. glucose will reduce 
10 eq. of cupric oxide to cuprous oxide. 
Preparation of Fehlings Solution. 
Dissolve exactly 34.639 grms. pure dry CuS04 in about 
200 c. c. water. In another vessel dissolve 173 grms. C. P. 
Rochelle salts (C4H4K NaOg-j-qPCO) in 480 c. c. pure sodi- 
um hydrate solution having a sp. gr. 1.14. 
Mix the solutions and dilute to exactly 1000 c. c. 10 c. c. 
of this solution contains 0.34639 grms. CuSO4 and corre- 
sponds to 0.050 grms. anhydrous glucose. Keep in the 
dark. On boiling with four vols. of water, it should give 
no precipitate. DETERMINATION OF GRAPE SUGAR. 
121 
The solution of glucose should not contain more than 
| per cent, glucose ; if stronger, dilute. 
Performance of Analysis: 
Run exactly 10 c. c. of the copper solution into a small 
flask, add 40 c. c. water, (or a dilute solution of NaHO,) 
heat to boiling and run into the solution the liquid con- 
taining the glucose, slowly and gradually, from an accurate 
burette. Continue until the last shade of bluish green 
disappears, and a small portion of liquid filtered, gives no 
reaction with H2S, nor with HC2H302 and K4Fe2Cy6- 
Calcidation. Since we took 10 c. c., Fehling’s solution, 
corresponding to 0.050 grms. anhydrous glucose, we read off 
the number of c. c. of glucose solution taken ; this shows us 
how much of the substance contains 50 grms. grape sugar. 
Example. Used 9. 5 c. c. solution containing glucose : 
9-5 : -05 = 100, : 
If solution was diluted, then xXd=p&r cent, glucose. 
This method may be applied to cane sugar, by first con- 
verting it into grape sugar by boiling one to two hours 
with dilute H2SG4 (1 part acid 5 parts water). This is not 
very accurate, owing to formation of caramel. Milk sugar 
reduces Fehling’s solution direct, but in another propor- 
tion, 100 glucose = 134 milk sugar. 
Weigh out ;r grms* of sugar or syrup, add water so that 
the whole will form about 80 c. c. Dissolve and add for 
D. Determination of Crystalizable Cane Sugar. 
* The value of x depends upon the instrument employed. Instruc- 
tions usually accompany a saccharimeter. 122 
QUANTITATIVE ANALYSIS. 
syrup 5 to 10 c. c. basic acetate of lead ; for raw sugar less ; 
for pure sugar, none. Dilute to 100 c. c. ; pour into a 
beaker, and add pulverized bone-black, and filter ; do not 
wash. Fill the tube of a Soleil or Dubosq Saccharimeter 
with this solution, perfectly full, insert the tube, and 
observe the transition tint. For details, see Atkinson’s 
translation of Ganot’s Physics, § 613. Cf. Fownes’ Chem- 
istry, p. 84, and Watts’ Diet, hi. 673-5. 
Analysis of a sample of Raw Sugar. 
Water, 
2.07 
Ash, .... 
. . . 1.58 
Grape Sugar, 
1.82 
Cane Sugar, . 
. 86.00 
Analysis No. 37. Petroleum. 
For information as to the composition and refining of 
petroleum, the products which it yields by distillation, and 
the methods of testing kerosene, see Dr. C. F. Chandler’s 
“ Report on Petroleum Oil ” in the “ American Chemist,” 
Vol. 11. pp. 409, 446, and Vol. 111. pp. 20 and 41. 
A.—Distillation of Petroleum. 
The method of examining crude petroleum for determi- 
nation of its commercial value, is not that of fractional 
distillation in its true, scientific sense, but consists in a 
process of distillation which separates the liquid into a 
certain number of aliquot parts, having determinable den- 
sities, and flashing points ; and the value of the sample 
depends upon the proportion of the light and heavy pro- 
ducts. 
The process of distillation is conducted as follows. Se- 
lect a tubulated retort of strong glass, free from flaws, and DISTILLATION OF PETROLEUM. 
123 
of about 500 c. c. capacity ; connect this with a Liebig’s 
condenser, and arrange for distilling in the usual manner. 
Through the tubulus of the retort insert a thermometer. 
Provide ten glass cylinders of 50 to 75 c. c. in capacity, 
and mark each with a file, so as to show the volume occu- 
pied by 25 c. c. of liquid. These cylinders are to serve as 
recipients of the distillate. 
Pour 250 c. c. crude petroleum into the retort, and apply 
heat very gently at first, increasing gradually, and finally 
heating until the residue in the retort is coked. Collect 
25 c. c. of the distillate in the first cylinder, and note the 
temperature indicated by the thermometer in the retort; 
collect the second 25 c. c. in another recipient, note also 
temperature, and continue in this manner, changing the 
recipient for every 25 c. c. until the whole liquid has dis- 
tilled over. 
Determine the sp. gr. of each distillate by floating in it 
a small Baume Hydrometer, note the color of each sam- 
ple, and determine its flashing point by means of Taglia- 
bue’s “ Open Tester,” a figure and description of which are 
found on page 41, Vol. 111. of the “ American Chemist.” 
B. Examination of the Distillates. 
To test the flashing point, proceed as follows ; pour a 
small quantity of the sample to be examined into the open 
cup, which is surrounded by a vessel of water. Light the 
lamp beneath and apply heat very gradually ; the tempera- 
ture should not rise faster than two degrees a minute. 
The thermometer bulb should dip beneath the surface of 
the oil. From time to time test the inflammable vapors 
which arise from the surface of the oil, using a small flame, 
flitting it quickly across the surface, and noting simultane- 
ously the height of the thermometer at the moment of 
ignition. Record results with each distillate. 124 
QUANTITATIVE ANALYSIS. 
Example. The following report of an actual distilla- 
tion shows how the results may be reported. This distilla- 
tion was accompanied with the phenomena technically 
called “cracking,” by which the heavier hydrocarbons split 
up into lighter ones. 
No of r | Temperature Sp. Gr. Flashing Point, 
fraction. olor‘ Fahr. BeaumG Fahr. 
2. “ 224 -298 60 48 
i. Colorless, i 42c-224° 64 20° 
3. Light yellow, 298 -404 55 102 
4. “ 404 -458 51 H7 
5- “ 458 -532 45 208 
6. Yellow, 532 - ? 42 254 
7 Dark yellow, 40 204 
8. Deeper “ 42 114 
9. Green, 44 82 
10. Black. 
The tenth product was coke left in the retort. 
Fig. 6 shows the disposition of apparatus at the commencement of the distillation; so soon 
as the lighter products have passed over, the bulb tube a c must be removed and connection 
made with the condenser by a short bent tube. APPENDIX. 
TABLE I. 
THE ELEMENTS, THEIR SYMBOLS, AND ATOMIC 
WEIGHTS, 
Name. 
Symbol. 
Atomic 
Weight. 
Name. 
Symbol. 
Atomic 
Weight. 
Aluminium . . . 
A1 
27.O 
Molybdenum . . 
Mo 
96. 
Antimony 
Sb 
120. 
Nickel .... 
Ni 
58.8 
Arsenic .... 
As 
75- 
Nitrogen .... 
N 
14. 
Barium .... 
Ba 
137 
Osmium .... 
Os 
195.2 
Bismuth .... 
Bi 
207.5 
Oxygen .... 
O 
l6. 
Boron 
B 
11. 
Palladium . 
Pd 
106.6 
Bromine .... 
Br 
80. 
Phosphorus . . 
P 
31 • 
Cadmium .... 
Cd 
112. 
Platinum .... 
Pt 
194-5 
Caesium .... 
Cs 
133- 
Potassium . . . 
K 
39-1 
Calcium .... 
Ca 
40. 
Rhodium , . . 
Rh 
104.4. 
Carbon .... 
C 
12. 
Rubidium . . 
Rb 
85.4 
Cerium .... 
Ce 
141. 
Ruthenium . 
Ru 
103.5 
Chlorine .... 
Cl 
35-5 
Samarium . . . 
Sa 
(?) 
Chromium . . . 
Cr 
52.5 
Scandium . . . 
Sc 
44. 
Cobalt 
Co 
59- 
Selenium.... 
Se 
79-4- 
Columbium . . . 
Nb 
94. 
Silicon . ’ . . . 
Si 
28. 
Copper .... 
Cu 
63-4 
Silver 
Ag 
108. 
Didymium . . . 
D 
146. 
Sodium .... 
Na 
23- 
Erbium .... 
E 
166. 
Strontium . . . 
Sr 
87.6 
Fluorine .... 
F 
19. 
Sulphur .... 
S 
32. 
Gallium .... 
Ga 
70. 
Tantalum . . . 
Ta 
182. 
Glucinum .... 
Be 
9- 
Tellurium . . . 
Te 
128. 
Gold 
Au 
196.5 
Terbium .... 
Tb 
(?) 
Hydrogen . . . 
H 
1. 
Thallium. 
Tl 
204. 
Indium .... 
In 
II3-4 
Thorium .... 
Th 
232. 
Iodine 
I 
127. 
Tin 
Sn 
118. 
Iridium .... 
Ir 
192.5 
Titanium 
Ti 
50. 
Iron 
Fe 
56. 
Tungsten . . . 
W 
184. 
Lanthanum . . . 
La 
138.5 
Uranium. . . . 
U 
240. 
Lead 
Pb 
206.5 
Ytterbium . . . 
Yb 
173- 
Lithium .... 
Li 
7- 
Yttrium .... 
Y 
90. 
Magnesium . 
Mg 
24. 
Zinc 
Zn 
65.2 
Manganese . 
Mn 
55- 
Zirconium . . 
Zr 
89.6 
Mercury .... 
H g 
200. 
125 126 
APPENDIX. 
TABLE 11. 
PRECIPITATING VALUE OF COMMON REAGENTS. 
Solutions of reagents being prepared of the strength recommended 
by Fresenius (see Fres. Qual. Anal, § 17 to § 85, b, Johnson’s edition 
•f 1875), the amount of a reagent required for precipitation may be 
calculated from the following table: 
One cubic centimetre of Will precipitate 
Dilute sulphuric acid 0.231 grm. Ba. 
Barium chloride 0.032 “ S03. 
Hydrodisodic phosphate .... 0.011 “ MgO. 
Magnesia mixture 0.024 “ P205 
Ammonium molybdate . . ... . 0.001 “ P205. 
Ammonium oxalate 0.016 “ CaO. 
Argentic nitrate 0.010 “ Cl. 
TABLE 111. 
DIAMETER OF FILTERS AND WEIGHTS OF FILTER 
ASHES; SWEDISH PAPER. 
Weight of Ash. 
Filter No. Diameter. Acid. Alkaline. 
i . . . 70 mm. 0.0004 grin. 0.0014 
2 . . . 104 “ 0.0007 “ 0.0027 
3 • • • 122 “ 0.0011 “ 0.0043 
4 ... 147 “ 0.0016 “ 0.0062 APPENDIX. 
127 
TRINITY COLLEGE. 
Hartford, iSB - 
Report of 
Analysis of 
Determination of 
Grammes taken ; 
Method of Analysis. 
Actual Calculated Theoretical 
Precipitates. Weights. Constituents. Weights. Percentages. Percentages. 
Special Remarks. 
[This is a reduced fac-simile of the reporting blank, measuring 8 by 10 inches, de- 
scribed on page 17.] 128 
APPENDIX. 
OFFICIAL METHODS OF ANALYSIS 
■OF THE ASSOCIATION OF OFFICIAL AGRICULTURAL CHEMISTS FOR 
iSSy-’SS. 
METHODS FOR DETERMINING PHOSPHORIC ACID 
AND MOISTURE. 
(i) Preparation of Sample.—The sample should be well intermixed 
and properly prepared, so that separate portions shall accurately 
represent the substance under examination, without loss or gain of 
moisture. 
(2) Determination of Moisture.—(a) In potash salts, nitrate of 
soda, and sulphate of ammonia heat 1 to 5 grams at 130° C. till the 
weight is constant, and reckon water from the loss. (b) In all other 
fertilizers heat 2 grams, or if the sample is too coarse to secure 
uniform lots of 2 grams each, 5 grams for five hours at 100° in a 
steam bath. 
(3) Water-soluble Phosphoric Acid.—Bring 2 grams on a filter, 
add a little water, let it run out before adding more water, and repeat 
this treatment cautiously until no phosphate is likely to precipitate in 
the filter. If the washings show turbidity after passing the filter 
clear up with acid. When the substance is nearly washed in this 
manner it is transferred to a mortar and rubbed with a rubber-tipped 
pestle to a homogeneous paste (but not further pulverized), then 
returned to the filter and washed with water untd the filtrate meas- 
ures not less than 250 cc. Mix the washings. Take an aliquot 
(usually corresponding to £ or | gram of the substance) and deter- 
mine phosphoric acid, as under total phosphoric acid. 
(4) Citrate-insoluble Phosphoric Acid.—Wash the residue of the 
treatment with water into a 200 cc. flask with 100 cc. of strictly 
neutral ammonium citrate solution of 1.09 density, prepared as here- 
after directed. Cork the flask securely and place it in a water bath, 
the water of which stands at 65° C. (The water bath should be of 
such a size that the introduction of the cold flask or flasks shall not 
cause a reduction of the temperature of the bath of more than 2° C.) 
Raising the temperature as rapidly as practicable to 65° C., which is subsequently maintained, digest with frequent shakings for thirty 
minutes from the instant of insertion, filter the warm solution quickly 
(best with filter-pumpj, and wash with water of ordinary temperature. 
Transfer the filter and its contents to a capsule, ignite until the 
organic matter is destroyed, treat with 10 to 15 cc. of concentrated 
hydrochloric or nitric acid, digest over a low flame until the phos- 
phate is dissolved, dilute to 200 cc., mix, pass through a dry filter, 
take an aliquot and determine phosphoric acid as under total. 
APPENDIX. 
In case a determination of citrate-insoluble phosphoric acid is re- 
quired in non-acidulated goods, it is to be made by treating 2 grams 
of the phosphatic material, without previous washing with water, 
precisely in the way above described, except that in case the sub- 
stance contains much animal matter (bone, fish, etc.) the residue 
insoluble in ammonium citrate is to be treated by one of the pro 
cesses described below. 
(5) Total Phosphoric Acid.—Weigh 2 grams and treat by one of 
the following methods : (1) Evaporation with 5 cc. magnesium 
nitrate, ignition, and solution in acid. (2) Solution in 30 cc. concen- 
trated nitric acid with a small quantity of hydrochloric acid. (3) Add 
30 cc. concentrated hydrochloric acid, heat, and add cautiously and 
in small quantities at a time about 0.5 gram of finely pulverized 
potassium chlorate. 
Boil gently until all phosphates are dissolved and all organic matter 
destroyed ; dilute to 200 cc.; mix and pass through a dry filter ; take 
50 cc. of filtrate ; neutralize with ammonia (in case hydrochloric acid 
has been used as a solvent add about 15 grams dry ammonium 
nitrate or its equivalent). To the hot solutions for every decigram 
of P205 that is present, add 50 cc. of molybdic solution. Digest at 
about 65° C. for one hour, filter, and wash with ammonium nitrate 
solution. (Test the filtrate by renewed digestion and addition of 
more molybdic solution.) Dissolve the precipitate on the filter with 
ammonia and hot water and wash into a beaker to a bulk of not 
more than 100 cc. Nearly neutralize with hydrochloric acid, cool, 
and add magnesia mixture from a burette ; add slowly (one drop per 
second), stirring vigorously. After fifteen minutes add 30 cc. of 
ammonia solution of density 0.96. Let stand several hours (two 
hours is usually enough). Filter, wash with dilute ammonia, ignite 
intensely for ten minutes, and weigh. 
(6) Citrate-soluble phosphoric acid. The sum of the water-soluble 
and citric insoluble subtracted from the total gives the citrate-soluble. 130 
APPENDIX. 
PREPARATION OF REAGENTS. 
(1) To Prepare Ammonium Citrate Solution.—Mix 370 grams of 
commercial citric acid with 1,500 cc. of water ; nearly neutralize with 
crushed commercial carbonate of ammonia ; heat to expel the car- 
bonic acid ; cool; add ammonia until exactly neutral (testing by 
saturated alcoholic solution of coralline) and bring to volume of two 
liters. Test the specific gravity, which should be 1.09 at 20° C., 
before using. 
(2) To Prepare Molybdic Solution.—Dissolve 100 grams of molyb- 
dic acid in 400 grams or 417 cc. of ammonia of specific gravity 0.96, 
and pour the solution thus obtained into ideograms or 1,250 cc. of 
nitric acid of specific gravity 1.20. Keep the mixture in a warm place 
for several days, or until a portion heated to 40° C. deposits no yellow 
precipitate of ammonium phospho-molybdate. Decant the solution 
from any sediment, and preserve in glass-stoppered vessels. 
(3) To Prepare Ammonium Nitrate Solution.—Dissolve 200 grams 
of commercial ammonium nitrate in water and bring to a volume of 
two liters. 
(4) To Prepare Magnesia Mixture.—Dissolve 22 grams of recently 
ignited calcined magnesia in dilute hydrochloric acid, avoiding excess 
of the latter. Add a little calcined magnesia in excess, and boil a 
few minutes to precipitate iron, alumina, and phosphoric acid, filter, 
add 280 grams of ammonium chloride, 700 cc. of ammonia of specific 
gravity 0,96, and water enough to make the volume of two liters. 
Instead of the solution of 22 grams of calcined magnesia no grams 
of crystallized magnesium chloride (MgCl2, 6H20) may be used. 
(5) Dilute Ammonia for Washing.—One volume ammonia of 
specific gravity 0.96 mixed with three volumes of water, or usually 
one volume of concentrated ammonia with six volumes of water. 
(6) Nitrate of Magnesia.—Dissolve 320 grams of calcined mag- 
nesia in nitric acid, avoiding an excess of the latter ; then add a little 
calcined magnesia in excess, boil ; filter from excess of magnesia, 
ferric oxide, etc., and bring to volume of two liters. 
METHODS OF DETERMINING POTASH. 
METHOD OF UNDO AS MODIFIED BY GLADDING. 
(1) Superphosphates.—Boil 10 grams of the fertilizer with 300 cc. 
of water for ten minutes. Cool the solution ; add ammonia in slight excess, thus precipitating all phosphate of lime, oxide of iron, and 
alumina, etc., make up to 500 cc., mix thoroughly and filter through 
a dry filter ; take 50 cc. corresponding to 1 gram, evaporate nearly 
to dryness, add 1 cc. of dilute H2SO4 (l to 1), and evaporate to dry- 
ness and ignite to whiteness. As all the potash is in form of sul- 
phate, no loss need he apprehended by volatilization of potash, and a 
full red heat must be used until the residue is perfectly white. This 
residue is dissolved in hot water plus a few drops of HCI ; 5 cc. of a 
solution of pure NaCl (containing 20 grams NaCl to the liter) and an 
excess of platinum solution (4 cc.) are now added, and the whole 
evaporated as usual. The precipitate is washed thoroughly with 
alcohol by decantation and on filter, as usual. The washing should 
be continued even after the filtrate is colorless. Ten cc. of the 
NH4CI solution prepared as above are now run through the filter. 
These 10 cc. will contain the bulk of the impurities, and are thrown 
away. A fresh portion of 10 cc. NH4CI is now run through the 
filter several times (five or six). The filter is then washed thoroughly 
wdth pure alcohol, dried, and weighed as usual. The platinum solu- 
tion used contains 1 gram metallic platinum in every 10 cc. 
APPENDIX. 
(2) Muriates of Potash.—ln the analysis of these salts an aliquot 
portion, containing .500 gram is evaporated with 10 cc. platinum 
solution plus a few drops of HCI, and washed as before. 
(3) Sulphate of Potash, Kainite, &■*c.—ln the analysis of these salts 
an aliquot portion containing .500 gram is taken, .250 gram of NaCl 
added, plus a few drops of HCI, and the whole evaporated with 15 
cc. platinum solution. In this case special care must be taken, in the 
washing with alcohol, to remove all the double chloride of platinum 
and sodium. The washing should be continued for some time after 
the filtrate is colorless. Twenty-five cubic centimeters of the NH4CI 
solution are employed, instead of 10 cc., and the 25 cc. poured 
through at least six times to remove all sulphates and chlorides. 
Wash finally with alcohol, dry and weigh as usual. 
To prepare the washing solution of NH4CI, place in a bottle 500 
cc. H2O, ioo grams of NH4CI; shake till disolved. Now pulverize 
5 or to grams of K2PtClc, put in the bottle, and shake at intervals for 
six or eight hours ; let settle over night ; then filter off liquid into a 
second bottle. The first bottle is then ready for a preparation of a 
fresh supply when needed. APPENDIX. 
ALTERNATE METHOD. 
Pulverize the fertilizer (200 or 300 grams) in a mortar ; take 10 
grams, boil for ten minutes with 200 cc. water, and after cooling, and 
without filtering, make up to 1,000 cc., and filter through a dry paper. 
In this method, in case the potash is contained in organic compounds, 
like tobacco stems, cottonseed hulls, &c., the substance is to be 
saturated with strong sulphuric acid and ignited in a muffle to de- 
stroy organic matter. If the sample have 10 to 15 per cent K2O 
(kainite), take 50 cc. of the filtrate ;if from 2to 3 per cent K2O (ordi- 
nary potash fertilizers), take too cc. of the filtrate. In each case 
make the volume up to 150 cc., heat to ioo°, and add, drop by drop, 
with constant stirring, slight excess of barium chloride ; without 
filtering, in the same manner, add barium hydrate in slight excess 
Heat, filter, and wash until precipitate is free of chlorides. Add to 
filtrate 1 cc. strong ammonium hydrate, and then a saturated solution 
of ammonium carbonate until excess of barium is precipitated. Heat. 
Add now, in fine powder, 0.5 gram pure oxalic acid or 0.75 gram 
ammonium oxalate. Filter, wash free of chlorides, evaporate filtrate 
to dryness in a platinum dish, and, holding dish with crucible tongs, 
ignite carefully over the free flame below red heat until all volatile 
matter is driven off. 
The residue is now digested with hot water, filtered through a 
small filter, and washed with successive small portions of water until 
the filtrate amounts to 30 cc. or more. To this filtrate, after adding 
two drops of strong hydrochloric acid, is added, in a porcelain dish, 5 
to 10 cc. of a solution of 10 grams of platinic chloride in xoo cc. of 
water. The mixture is now evaporated on the water-bath to a thick 
syrup, or further treated with strong alcohol washed by decantation, 
collected in a Gooch crucible or other form of filter, washed with 
strong alcohol, afterwards with 5 cc. ether, dried for thirty minutes 
at too’ C., and weighed. 
It is desirable, if there is an appearance of white foreign matter in 
the double salt, that it should be washed, according to the previous 
method, with 10 cc. of the half-concentrated solution of NH4CI, which 
has been saturated by shaking with K2PtCl6, as recommended by 
Gladding. 
The use of the factor 0.3056 for converting K-iPtCF to KCI and 
0.19308 for converting to K2O is continued. APPENDIX. 
133 
METHOD FOR THE DETERMINATION OF NITROGEN. 
The Absolute or Cupric Oxide Method. 
The apparatus and reagents needed are as follows : 
APPARATUS. 
Combustion Tube of best hard Bohemian glass, about 26 inches long 
and one-half inch internal diameter. 
Azotometer of at least 100 cubic centimeters capacity, accurately 
calibrated. 
Sprengel Mercury Air Pump. 
Small Paper Scoop, easily made from stiff writing-paper. 
REAGENTS. 
Cupric Oxide (coarse).—Wire form ; to be ignited and cooled 
before using. 
Fine Cupric Oxide.—Prepared by pounding ordinary cupric oxide 
in mortar. 
Metallic Copper.—Granulated copper or fine copper gauze reduced 
and cooled in steam of hydrogen. 
Caustic Potash Solution.—Dissolve commercial stick potash in 
less than its weight of water so that crystals are deposited on cooling. 
When absorption of carbonic acid ceases to be prompt solution must 
be discarded. 
Sodium Bicarbonate.—Free from organic matter. 
loading tube. 
Of ordinary commercial fertilizers take 1 to 2 grams for analysis. 
In the case of highly nitrogenous substances the amount to be taken 
must be regulated by the amount of nitrogen estimated to be pres- 
ent. Fill tube as follows : (1) About 2 inches of coarse cupric oxide. 
(2) Place on the small paper scoop enough of the fine cupric oxide to 
fill, after having been mixed with the substance to be analyzed, about 
4 inches of the tube ; pour on this the substance, rinsing watch glass 
with a little of the fine oxide and mix thoroughly with spatula ; pour 
into tube, rinsing the scoop with a little fine oxide. (3) About 12 
inches of coarse cupric oxide. (4) About 3 inches of metallic copper. 134 
APPENDIX. 
(5) About 2| inches of coarse cupric oxide (anterior layer). (6) Small 
plug of asbestos. (7) Eight-tenths to 1 gram of sodium bicarbonate. 
(8) Large, loose plug of asbestos ; place tube in furnace, leaving 
about one inch of it projecting; connect with pump by rubber stopper 
smeared with glycerine, taking care to make connection perfectly 
tight. 
OPERATION. 
Exhaust air from tube by means of pump. When a vacuum has 
been obtained, allow flow of mercury to continue, light gas under 
that part of tube containing metallic copper, anterior layer of cupric 
oxide (see sth above) and bicarbonate of soda. As soon as vacuum 
is destroyed and apparatus filled with carbonic acid gas, shut off the 
flow of mercury, and at once introduce the delivery tube of the pump 
into the receiving arm of the azotometer and just below the surface of 
the mercury seal of the azotometer, so that the escaping bubbles will 
pass into the air and not into the azotometer, thus avoiding the use- 
less saturation of the caustic potash solution. 
When the flow of carbonic acid has very nearly or completely 
ceased, pass the delivery tube down into the receiving arm, so that 
the bubbles will escape into the azotometer. Light the jets under 
the 12-inch layer of oxide, heat gently for a few moments to drive out 
any moisture that may be present, and bring to red heat. Heat 
gradually mixture of substance and oxide, lighting one jet at a time. 
Avoid too rapid evolution of bubbles, which should be allowed to 
escape at rate of about one per second or a little faster. 
When the jets under mixture have all been turned on, light jets 
under layer of oxide at end of tube. When evolution of gas has 
ceased turn out all the lights except those under the metallic copper 
and anterior layer of oxide, and allow to cool for a few moments. 
Exhaust with pump and remove azotometer before flow of mercury 
is stopped. Break connection of tube with pump, stop flow of mer- 
cury, and extinguish lights. Allow azotometer to stand at least an 
hour or cool with stream of water until permanent volume and tem- 
perature are reached. 
Adjust accurately the level of the KOH solution in bulb to that in 
azotometer, note volume of gas, temperature, and height of barom- 
eter ; make calculations as usual. The labor of calculation may 
be much diminished by the use of the tables prepared by Messrs. APPENDIX. 
Battle and Dancy, of the North Carolina Experiment Station 
(Raleigh, N. C). 
The above details are, with some modifications, those given in 
the report of the Connecticut Station for 1879 (P- 124). which may 
be consulted for details of apparatus, should such details be desired. 
Determination by the Method of Kjeldahl. 
(1) Hydrochloric acid whose absolute strength has been determined, 
(.a) by precipitating with silver nitrate and weighing the silver chlo- 
ride, (b) by sodium carbonate, as described in Fresenius’s Quantita- 
tive Analysis, second American edition, page 680, and (c) by deter- 
mining the amount neutralized by the distillate from a weighed 
quantity of pure ammonium chloride boiled with an excess of sodium 
hydrate. 
REAGENTS AND APPARATUS. 
(2) Standard ammonia whose strength, relative to the acid, has 
been accurately determined. 
(3) “C. P.” sulphuric acid, specific gravity 1.83, free from 
nitrates and also from ammonium sulphate, which is sometimes 
added in the process of manufacture to destroy oxides of nitrogen. 
(4) Mercuric oxide, HgO, prepared in the wet way. That pre- 
pared from mercury nitrate cannot safely be used. 
(5) Potassium permanganate tolerably finely pulverized. 
(6) Granulated zinc. 
(7) A solution of 40 grams of commercial potassium sulphide in 
one liter of water. 
(8) A saturated solution of sodium hydrate free from nitrates, 
which are sometimes added in the process of manufacture to destroy 
organic matter and improve the color of the product. That of the 
Greenbank Alkali Company is of good quality. 
(9) Solution of cochineal prepared according to Fresenius’s 
Quantitative Analysis, second American edition, page 679. 
(10) Burettes should be calibrated in all cases by the user. 
(n) Digestion flasks of hard, moderately thick, well-annealed glass. 
These flasks are about 9 inches long, with a round, pear-shaped 
bottom, having a maximum diameter of 2l inches, and tapering out 
gradually in a long neck, which is three-fourths of an inch in diam- APPENDIX. 
eter at the narrowest part, and flared a little at the edge. The 
total capacity is 225 to 250 cc. 
(12) Distillation flasks of ordinary shape, 550 cc. capacity, and 
fitted with a rubber stopper and a bulb tube above to prevent the 
possibility of sodium hydrate being carried over mechanically during 
distillation. This is adjusted to the tube of the condenser by a rub- 
ber tube. 
(13) A condenser. Several forms have been described, no one of 
which is equally convenient for all laboratories. The essential thing 
is that the tube which carries the steam to be condensed shall be of 
block tin. All kinds of glass are decomposed by steam and ammonia 
vapor, and will give up alkali enough to impair accuracy. (See Kreus- 
sler and Henzold, Ber. d. chem.Ges., XVII., 34.) The condenser in 
use in the laboratory of the Connecticut Experiment Station, devised by 
Professor Johnson, consists of a copper tank supported by a wooden 
frame, so that its bottom is 11 inches above the work-bench on which 
it stands. This tank is 16 inches high, 32 inches long, and 3 inches 
wide from front to back, widening above to 6 inches. It is provided 
with a water-supply tube which goes to the bottom, and a larger 
overflow pipe above. The block tin condensing tubes, whose exter- 
nal diameter is f of an inch, seven in number, enter the tank through 
holes in the front side of it near the top, above the level of the over- 
flow, and pass down perpendicularly through the tank and out 
through rubber stoppers, tightly fitted into holes in the bottom. They 
project about i-J- inches below the bottom of the tank, and are con- 
nected by short rubber tubes with glass bulb tubes of the usual shape, 
which dip into glass precipitating beakers. These beakers are 
6£ inches high, 3 inches in diameter below, somewhat narrower 
above, and of about 500 cc. capacity. The titration can be made 
directly in them. The seven distillation flasks are supported on a 
sheet-iron shelf attached to the wooden frame that supports the tank 
in front of the latter. Where each flask is to stand a circular hole 
is cut, with three projecting lips, which support the wire gauze under 
the flask, and three other lips which hold the flask in place and pre- 
vent its moving laterally out of place while distillation is going on. 
Below this sheet-iron shelf is a metal tube carrying seven Bunsen 
burners, each with a stop-cock like those of a gas-combustion fur- 
nace. These burners are of larger diameter at the top, which pre- 
vents smoking when covered with fine gauze to prevent the flame 
from striking back. APPENDIX. 
137 
(14) The stand for holding the digestion flasks consists of a pan of 
sheet-iron 29 inches long by 8 inches wide, on the front of which is 
fastened a shelf of sheet-iron as long as the pan, 5 inches wide and 
4 inches high. In this are cut six holes if inches in diameter. At 
the back of the pan is a stout wire running lengthwise of the stand, 8 
inches high, with a bend or depression opposite each hole in the 
shelf. The digestion flask rests with its lower part over a hole in 
the shelf and its neck in one of the depressions in the wire frame- 
which holds it securely in position. Heat is supplied by low Bunsen 
burners below the shelf. With a little care the naked flame can be 
applied directly to the flask without danger. 
One gram of the substance to be analyzed is brought into a diges- 
tion flask with approximately 0.7 gram of mercuric oxide and 20 
cc. of sulphuric acid. The flask is placed on the frame above de- 
scribed in an inclined position and heated below the boiling point of 
the acid for from sto 15 minutes, or until frothing has ceased. The 
heat is then raised till the acid boils briskly. No further attention 
is required till the contents of the flask have become a clear liquid, 
which is colorless or at least has only a very pale straw color. The 
flask is then removed from the frame, held upright, and, while still 
hot, potassium permanganate is dropped in carefully and in small 
quantity at a time till after shaking the liquid remains of a green or 
purple color. After cooling, the contents of the flask are transferred 
to the distilling flask with water, and to this 25 cc. of potassium 
sulphide solution are added, 50 cc. of the soda solution, or sufficient 
to make the reaction strongly alkaline, and a few pieces of granu- 
lated zinc. The flask is at once connected with the condenser and 
the contents of the flask are distilled till all ammonia has passed 
over into the standard acid contained in the precipitating flask pre- 
viously described and the concentrated solution can no longer be 
safely boiled. This operation usually requires from 20 to 40 minutes. 
The distillate is then titrated with standard ammonia. 
THE DETERMINATION. 
The use of mercuric oxide in this operation greatly shortens the 
time necessary for digestion, which is rarely over an hour and a half 
in the case of substances most difficult to oxidize and is more com- 
monly less than an hour. In most cases the use of potassium per- 
manganate is quite unnecessary, but it is believed that in excep- tional cases it is required for complete oxidation, and in view of the 
uncertainty it is always used. Potassium sulphide removes all mer- 
cury from solution and so prevents the formation of mercuro- 
ammonium compounds which are not completely decomposed by 
soda solution. The addition of zinc gives rise to an evolution of 
hydrogen and prevents violent bumping. Previous to use, the 
reagents should be tested by a blank experiment with sugar, which: 
will partially reduce any nitrates that are present which might other- 
wise escape notice. 
APPENDIX. 
The following modification must be used for the determination of 
nitrogen in substances which contain nitrates when it is desired to 
use this method : 
Determination of Nitrogen, Including the Nitrogen of 
Nitrates, by a Modified Method of Kjeldahl.* 
Bring from 07. to 1.4 grams of the substance to be analyzed into a 
Kjeldahl digesting flask, add to this 30 cc. of sulphuric acid contain- 
ing 2 grams of salicylic acid, and shake thoroughly. Then add 
gradually three grams of zinc-dust, shaking the contents of the 
flask at the same time. Finally, add two or three drops of platinic 
chloride solution and place the flask on the stand for holding the 
digestion flasks, where it is heated over a low flame until all danger 
from frothing has passed. The heat is then raised until the acid 
boils briskly, and the boiling; continued until white fumes no longer 
pour out of the flask. This requires about five or ten minutes. Add 
now approximately o. 7 gram mercuric oxide and continue the boil- 
ing until the liquid in the flask is colorless, or nearly so. (In case 
the contents of the flask are likely to become solid before this point 
is reached add 10 cc. more of sulphuric acid.) Complete this oxida- 
tion with a little permanganate of potash in the usual way, and 
proceed with the distillation as described in the method above. 
Determination by the Ruffle Method. 
preparation of reagents. 
(1) A standard solutioti of sulphuric acid, half normal, or 19.968 
grams SO3 per liter. 
(2) A standard solution of potassium hydrate, half normal, or 
27.99! grams KOH per liter. 
♦Described by Prof. M. A. Scovell. APPENDIX. 
139 
(3) An alcoholic solution of cochineal. 
(4) Hyposulphite mixture.—Prepared by mixing equal parts by 
-weight of soda-lime and finely powdered crystallized sodium 
hyposulphite. 
(5) Sugar and sulphur mixture.—This is prepared by mixing 
•equal parts by weight of finely powered granulated sugar and flowers 
of sulphur. 
(6) Ordinary granulated soda-lime. 
(1) Combustion tubes of hard Bohemian glass, 20 inches long and 
i inch internal diameter, drawn to a point. 
APPARATUS. 
(2) Three-bulb, 6-inch U tubes, with glass stop-cock. 
(3) Aspirator. 
PREPARATION. 
(1) Clean and fill the U tube with 10 cubic centimeters of standard 
acid. 
(2) Fit cork and glass connecting tube. Fill the tube as follows : 
<x) A loosely fitting plug of asbestos, previously ignited, and then 
Ito li inches of the hyposulphite mixture. (2) The weighed portion 
of the substance to be analyzed is intimately mixed with from 5 to 10 
grams of the sugar and sulphur mixture. (3) Pour on a piece of 
glazed paper, or porcelain mortar, a sufficient quantity of the hyposul- 
phite mixture to fill about 10 inches of the tube ; then add the sub- 
stance to be analyzed, as previously prepared ; mix carefully and 
pour into the tube ; shake down the contents of the tube ; rinse off 
the paper or mortar with a small quantity of the hyposulphite mix- 
ture and pour into the tube ; then fill up with soda-lime to within 
2 inches of the end of the tube. (4) Place another plug of ignited 
asbestos at the end of the tube, and close with a cork. (5) Hold the 
tube in a horizontal position, and tap on the table until there is a gas 
channel all along the top of the tube. Make connection with the 
U tube containing the acid, aspirate, and see that the apparatus is 
tight. 
The Combustion.—Place the prepared combustion tube in the 
furnace, letting the open end project a little so as not to burn the 
cork. Commence by heating the soda-lime portion until it is brought 
to a full red heat. Then turn up slowly jet after jet towards the 
••outer end of the tube, so that the bubbles come off two or three a APPENDIX. 
second. When the whole tube is red hot and the evolution of the gas 
has ceased and the liquid in the U tube begins to recede toward the 
furnace, attach the aspirator to the other limb of the U tube, break 
off the end of the tube, and draw a current of air through for a few 
minutes. Detach the U tube and wash the contents into a beaker 
or porcelain basin, add a few drops of the cochineal solution, and 
titrate. 
Select a tube of hard glass 14 to 16 inches long, draw one end of it 
to a tine point, and to the other end fit a cork, through which is passed 
a tube bent at right angles, the other end of which passes through a 
cork closing tightly one arm of a 6-inch three-bulbed U tube with 
glass stop-cock. Into the combustion tube first slip a loosely fitting 
plug of asbestos previously ignited, and then i£ to 2 inches of soda- 
lime. Weigh out from 0.7 to 2.8 grams of the substance to be 
analyzed, and mix it on a piece of glazed paper or porcelain mor- 
tar with some finely pulverized soda-lime, and introduce the mix- 
ture into the combustion tube. The paper or mortar is then rinsed 
out with a small quantity of soda-lime and poured into the tube. 
The tube is then filled up to within 1 to 2 inches of the open end 
with granulated soda-lime, then with a plug of ignited asbestos. 
A free passage is formed for the evolved gases by holding the 
tube in a horizontal position and tapping gently on the table. In- 
troduce the prepared combustion tube into the furnace, letting the 
open end project a little so as not to burn the cork, supporting 
the U tube by a clamp. The tube is then gradually heated, com- 
mencing at the fore part, nearest the cork, and progressing slowly 
towards the tail. The combustion should be conducted so as to 
obtain a steady and uninterrupted flow of gas. When properly 
carried out, the acid in the U tube is never colored. When the 
acid begins to recede attach the aspirator to the other limb of 
the U tube, and start it slowly, then break off the point of the 
combustion tube and draw a current of air through the apparatus 
for a few minutes, in order to sweep all the ammonia into the acid. 
Determination by the Soda-Lime Method. 
Detach the U tube and wash the contents into a beaker or 
porcelain basin, add a few drops of an alcoholic solution of cochi- 
neal, and titrate. 
The standard acid and alkali to be the same as that used in 
the Ruffle method. INDEX 
Acidimetry, 45. 
Albumen, determination of, in urine, 116. 
Alkalies, determination of, in potable water, 
92. 
Calorific power of coal, 39. 
Cane sugar, analysis of, 101. 
in feldspar, estimation of, 56. 
Alkalimetry, 42. 
determination of, 121. 
Carbon, estimation of, in coal, 39. 
total, determination of, in pig-iron, 79. 
ultimate determination of, in sugar, 102. 
Alloys, determination of two metals in, 100. 
Alum, ammonia-iron, analysis of, 20. 
Alumina, iron ana phosphoric acid, 75. 
Alvargonzalez, determination of total car- 
Carbonic anhydride, determination by direct 
weight, 34. 
determination by loss, 33. 
bon, 81. 
Chandler’s analysis of Croton Water, 98. 
Chloride of lime, valuation of, 49. 
Ammonia-iron-alum, analysis of, 20. 
Ammonia, determination of, in guano, BS. 
Ammoniomagnesic phosphate, properties 
of, 19. 
Chlorimetry, 47. 
Chlorine, determination of, 13. 
Ammonium, gravimetric determination of, 20. 
phospho-molybdate, properties of, 70. 
determination of, in potable water, 92. 
Chromic iron ore, analysis of, 54. 
Clark’s soap test for potable water, 93. 
Coal, proximate analysis of, 36. 
Cobalt, determination of, in nickel ore, 86. 
Combustions, process of conducting, 103. 
Copper, electrolytic estimation of, 35, 39. 
Analysis, organic, 101. 
Analyses, calculations of, 15. 
reporting of, 17. 
Antimony, determination of, 51. 
Apjohn’s method of estimating urea, 115. 
Arsenical nickel ore, analysis of, 86. 
estimation of, in a silver coin, 29. 
pyrites, analysis of, 39. 
Ash, estimation of, in coal, 37. 
Davey’s method of estimating urea, 114. 
Distillation of petroleum, 122. 
Baric chloride, analysis of, 13. 
Barium, determination of, 14. 
sulphate, properties of, 18. 
Dolomite, analysis of, 30. 
Drown’s determination of sulphur in pig- 
iron, 83. 
Bell’s determination of total carbon in pig- 
iron, 81. 
Eggertz’ determination of graphite in pig- 
iron, 77. 
Bile, tests for, in urine, 117. 
determination of sulphur and phosphorus 
in pig-iron, 82. 
Bleaching powder, constitution of, 47. 
reactions of, 48. 
valuation of, 49. 
Elliott’s determination of total carbon in 
pig-iron, 79. 
Bronze, analysis of, 35. 
Butter, determination of, in milk, 118. 
Fehling’s solution, preparation of, 120. 
Feldspar, analysis of, 56. 
Butyramide, estimation of nitrogen in, 107. 
Ferrocyanide of potassium, determination of 
nitrogen in, 105. 
Cairns’determination of graphite in pig-iron, 
78. 
Flight’s method of separating iron, alumina, 
and phosphoric acid, 75. 
Calcium, determination of, 31. 
Calculation of results of analyses, 15. 
Fusion of an iron ore, 66. 
141 142 
INDEX, 
Glucose, estimation of, ug. 
Pearl-ash, valuation of, 45. 
Grape sugar, determination of, 119. 
Graphite, determination of, in pig-iron, 76. 
Guano, analysis of, 88. 
Penot’s method for valuation of chloride of 
lime, 49. 
Heintz and Ragsky’s method of estimating 
Permanganate of potassium, standardization 
of, 25. 
Hematite, analysis of, 62. 
urea, 115. 
Petroleum, distillation of, 122. 
Phosphoric acid, determination of, 28. 
determination of, in guano, 89. 
determination of, by molybdenum, 69. 
Flight’s method of separation from iron, 
Hydrochloric acid, valuation of, 46. 
Hydrodisodic phosphate, analysis of, 27. 
Hydrogen, determination of, in sugar, 102. 
75- 
insoluble, determination of, in superphos- 
phates, 90. 
Iron and titanium, determination of, 74. 
basic acetate of, 53, 68. 
reduced, determination of, in superphos- 
phates, go. 
determination of, in ammonia-iron-alum, 
21. 
determination of, in a titaniferous ore, 68, 
7*- 
Phosphorus, determination of, in pig iron, 
76, 82. 
determination of, by precipitation, 22. 
determination of, in hematite, 62. 
ore, titaniferous, analysis of, 63. 
Pig-iron, analysis of, 76. 
Potassium chloride, analysis of, 26. 
ferrocyanide, determination of nitrogen in, 
105. 
slag, analysis of, 60. 
volumetric determination of, 22, 71. 
gravimetric estimation of, 26. 
permanganate, solution of, 22. 
Koninck and Dietz’ determination of sulphur 
in pig-iron, 84. 
Pyrolusite, analysis of, 56. 
Lead, estimation of, in a silver coin, 29. 
Liebig’s method of estimating urea, 113. 
Liquids, specific gravity of, 99. 
Raw sugar, analyses of, 119. 
Reporting analyses, 17. 
Reverted phosphoric acid, determination of, 
gt. 
Litmus solution, preparation of, 42. 
Salammoniac, action of nitric acid on, 32. 
Schlosing’s determination of ammonia, 88. 
Silica, determination of, in soluble silicates, 
59- 
Magnesic sulphate, analysis of, xB. 
Magnesium, separation from calcium, 30. 
Manganese, estimation of, 56. 
Gibbs’ method of estimation, 70. 
Marguerite’s method for determination of 
iron, 22. 
determination of, in slag, 61. 
separation of, from titanium, 64. 
Silicates, analysis of soluble, 59. 
Silver coin, analysis of, 29. 
Melsens’ determination of nitrogen, 107. 
Milk, analysis of, 118. 
Slag, analysis of iron, 60. 
Moisture, determination of, in coal, 36. 
Molybdenum, use of, in estimation of phos- 
Soap test for potable water, 93. 
Soda ash, valuation of. 44. 
Sodium, determination of, 27. 
phoric acid, 69. 
Specific gravities of solids and liquids, 99. 
Standard solutions, 42. 
Nickel ore, arsenical, analysis of, 86. 
Nitrogen, determination of, by Varrentrapp 
and Will’s method, 105. 
Sugar, determination of ash in raw sugar, 
119. 
Melsens’ determination of, 107. 
Normal solutions, 41. 
determination of, in milk, 118. 
ultimate analysis of, 101. 
Sulphur, determination of, in pig-iron, 82. 
estimation of, in coal, 37. 
Organic analysis, 101. 
matter in potable water, 94. 
Sulphuric acid, gravimetric determination 
of, 18. INDEX 
H3 
Sulphuric acid in potable water, determina- 
tion of, ga. 
Varrentrapp and Will’s estimation of nitro- 
gen, 105. 
Superphosphate of lime, analysis of, go. 
Testing petroleum, 122. 
Vinegar, analysis of, 46. 
Volatile matter, estimation of, in coal, 37. 
Volumetric analysis, general notes on, 40. 
Tin, determination of, in type metal, 51. 
determination of, in bronze, 35. 
estimation of nitrogen, 107. 
Titaniferous iron ore, analysis of, 63. 
Titanium, estimation of, in iron ore, 74. 
Titration, residual method of, 45. 
Water analysis, calculation of results, 95. 
determination of, by direct weight, 28. 
determination of, by ignition, 13, 28. 
determination of, in milk, 118. 
Type metal, analysis of, 31. 
Urea, determination ofj Liebig’s method, 113. 
Apjohn’s method, 115. 
Davey’s method, 114. 
Weyl’s determination of total carbon in pig- 
iron, 82. 
potable, analysis of, 91. 
Urinary sediments, scheme for analysis of, 
117- 
Zinc, determination of, in bronze, 36. 
ore, analysis of, 53. 
Urine, analysis of, 109. 
composition of, in. 
APPENDIX 
Agricultural chemists, official methods of 
analysis, 128. 
Phosphoric acid, official method of determina- 
tion, 128 
Atomic weights of elements, table I. 125. 
Filters, diameters and weight of ashes, 126. 
Cladding’s methods of determining potash, 130. 
Kjeldahl’s method of determining nitrogen, 135 
Moisture, official methods of determination, 128. 
Nitrogen, official methods of determination, 133. 
Official methods of agricultural chemists, 128. 
Potash, official method of determination, 130. 
Reagents, precipitating value of, 126. 
Report blank, 127. 
Ruffle method of determining nitrogen, 138. 
Soda-lime method of determining nitrogen, 140. 
Zettnow’s scheme for qualitative analysis, fold 
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" Elements of Analytics. achanics Bvo, 300 
MATERIALS OF ENGINEERING. 
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ployed in Construction 16mo, 3 00 
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Johnson’s Materials of Construction Large Bvo, 6 00 
Keep’s Cast Iron Bvo, S 50 
Lanza’s Applied Mechanics Bvo, 7 56 
Martens’s Handbook on Testing Materials. (Henning.).2 v., Bvo, 7 50 
Merrill’s Stones for Building and Decoration Bvo, 6 00 
Merriman’s Text-book on the Mechanics of Materials Bvo, 4 0© 
Merriman’s Strength of Materials 12rao, 1 00 
Metcalf’s Steel. A Manual for Steel-users 12mo, 2 00 
Patton’s Practical Treatise on Foundations Bvo, 5 00 
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Elements of Analytical Mechanics Bvo, 3 00 
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Butts’s Civil Engineer’s Field-book 16mo, morocco, 2 50 
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“ “ Engineering ” and Electric Traction Pocket-book. 
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Dredge’s History of the Pennsylvania Railroad: (1879.) .Paper, 500 
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Fisher’s Table of Cubic Yards Cardboard, 26 
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Howard’s Transition Curve Field-book 16mo, morocco, 1 50 
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Molitor and Beard’s Manual for Resident Engineers. 16mo, 1 00 
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Jones’s Machine Design: 
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MacCord’s Elements of Descriptive Geometry Bvo, 3 00 
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chine Design Bvo, 3 00 
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Mather’s Dynamometers, and the Measurement of Power. .12mo, 3 00 
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Carpenter’s Experimental Engineering Bvo, 6 00 
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Clerk’s Gas and Oil Engine Small Bvo, 4 00 
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Jones’s Machine Design: 
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11 MacCord’s Kinematics; or, Practical Mechanism Bvo, 6 00 
Mechanical Drawing 4to, 4 00 
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mann—Klein.) 8 vo, 5 00 
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Wolff’s Windmill as a Prime Mover Bvo, 3 00 
Wood’s Turbines Bvo, 250 
Bovey’s Strength of Materials and Theory of Structures. .Bvo, 7 60 
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Ford’s Boiler Making for Boiler Makers 18mo, 1 00 
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Goss’s Locomotive Sparks Bvo, 2 00 
Hall’s Car Lubrication 12mo, 1 00 
Holly’s Art of Saw Filing 18mo, 75 
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Jones’s Machine Design: 
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Kerr’s Power and Power Transmission Bvo, 2 00 
Lanza’s Applied Mechanics Bvo, 7 60 
MacCord’s Kinematics; or, Practical Mechanism Bvo, 5 00 
Velocity Diagrams. Bvo, I 50 
Merriman’s Text-book on the Mechanics of Materials Bvo, 4 00 
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Reagan’s Locomotive Mechanism and Engineering 12mo, 2 00 
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Richards’s Compressed Air 12mo, 1 50 
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14 MINERALOGY. 
Barringer’s Description of Minerals of Commercial Value. 
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Brush’s Manual of Determinative Mineralogy. (Penfield.) .Bvo, 400 
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Williams’s Manual of Lithology .Bvo, 3 00 
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Boyd’s Resources of Southwest Virginia Bvo, 3 00 
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Steel’s Treatise on the Diseases of the Dog Bvo, 3 50 
Totten’s Important Question in Metrology Bvo, 2 60 
The World’s Columbian Exposition of 1893 4to, 1 00 
Worcester and Atkinson. Small Hospitals, Establishment and 
Maintenance, and Suggestions for Hospital Architecture, 
with Plans for a Small Hospital 12mo, 1 26 
HEBREW AND CHALDEE TEXT-BOOKS. 
Green’s Grammar of the Hebrew Language Bvo, 8 00 
“ Elementary Hebrew Grammar 12mo, 126 
“ Hebrew Chrestomathy Bvo, 200 
Geeenius’s Hebrew and Chaldee Lexicon to the Old Testament 
Scriptures. (Tregelles.) Small 4to, half morocco, 600 
Letteris’s Hebrew Bible Bvo, 2 26 
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