ITEM No. 17 FILE No. XXII—17 COPY No. NEW LIQUID INCENDIARY AGENT (C1F3), COMBINED INTELLIGENCE OBJECTIVES SUB-COMMITTEE INFORMATION ON A NEW LIQUID INCENDIARY AGENT ESSE 23 April, 1945, Reported by M.F. FOOLER, U.S. Civilian CWS, Eq.ETOUSA JOSEPH E. SWADEL, Lt .Col.,Medical Corps, Hq. BTOUSA 7 May, 1945. CIOS Black List Item - 17 Flame and Incendiaries COMBINED INTELLIGENCE OBJECTIVES SUB-COMMITTEE G-2 DIVISION, SHAEF (REAR) APO 413 TABLE OF CONTENTS Subject Page No, 1. Introduction... 3 2. Properties of 3 3. Preparation of CIF3 at Leverkusen 4 4. Industrial Development of GIF- 4 5. Effect of ClFj on Human Beings 5 6. Recommendations 5 7. Appendix I - Translation of Description of Fluorine Apparatus.... 7 8. Appendix II - Translation of Operating Instructions for Fluorine... 8 9. Appendix III - Translation of Operating Instructions for 11 PERSONNEL OF INSPECTION TEAM Mr, Francis J, Curtis. CWS,Hq,ETOUSA Cmdr, Charles L, McCarthy USNR Dr. Mayor F. Fogler CWS,Eq.ETOUSA Lt,Col,Joseph S, Smadel MC AUS Lt,Co1,KamiIton Southworth.......USPHS Dr. Ernest H. Volwiler CWS,Hq.ETOUSA CONFIDENTIAL CONFIDENTIAL INFORMATION ON A NEW LIQUID INCENDIARY AGENT 1. INTRODUCTION. a. The information contained in this report was obtained from Dr, L. Klebert, Director of Inorganic Department of the I.G, Farben- industrie plant at Leverkusen, Germany and Dr. Erich Noack, who is a member of Dr. Klebert’s department, during conversations on 23 and 25 April, 1945. b. Prior to 1937 a Dr. Kwasnik began an intensive study of fluorine compounds since the I.G, plant at Leverkusen was interested in obtaining a good fluorinating agent for the fluorination of hydrocarbons. Investigations were made of halogen trifluoride compounds which had been described previously in the literature. (Ruff and Krug; (Jber ein neues ohlorfluorid - CIF3, zt. Anorg. Chem.1930, 190. 270; Ruff; Neues aus der Chemie des Fluors, zt.f. Angew. Chem. 1933, 46, 739.) Iodine trifluorid© was prepared and tested for the fluorination of hydrocarbons with some success. As a matter of scientific interest, chlorine trifluoride was pre- pared and found unsatisfactory for the purpose just mentioned. The Inxr ganic Division had found no use for GIF, and had no interest in it until 1937 when the German Army Ordnance inspected the laboratory preparing the material. The Army subsequently asked for samples at intervals; the first sample was sent about four years ago, the last in 1944. During this period the laboratory prepared 3 to 5 tons of GIF™. It is believed that the German Army intended to use GIF, in shells against aircraft and tanks. The unique properties of the substance would be peculiarly suited against such machines since organic matter would be inmiediately ignited and glass or plastic windows would be permanently etched end rendered opaque. 2. PROPERTIES OF CIF a. The structure of the substance is not known. It is a liquid with a boiling point of 12 C, Iflhen stored in iron pressure cjrlinders, the material is stable and can be handled and shipped without difficulty. b. The substance combines with all organic and a number of inorganic compounds so vigorously that the heat generated will generally cause the material to burst into flame. Combustible organic compounds will then continue to burn in the normal manner. Non-combustible inorganic substances cease to flame as soon as the GIF* is dissipated. Glass, for example, would be badly etched and rendered opaque by contact with ClFg. Glass wool is said to burn with a flame in the presence of ClFg and the reaction with water is so vigorous as to give off incandescent gases. The reaction of C1B’3 with glass and water is illustrated as followst- SiOg + C1F3 SiF4 «- 02 +• Clg heat HgO *- C1F3 — HF + 0 + Cl2 i- heat 3. PREPARATION OF GIF- AT LEVERKUSEN. a. All the necessary apparatus for manufacturing on a laboratory scale was contained in a room with floor dimensions of about 8 x 16 ft. This small plant could make 3-g pounds of ClFj per hour. The process of manufacturing is as follows b. Fluorine is produced by electrolysis in a cell- made of metallic magnesium. Carbon anodes are used with the metallic vessel serving0as the cathode. The electrolyte, which is KHFn) is kept at 100°C and is not dissipated since liquid HF is continuously fed into the cell and broken down into Hg and Fg, A sketch of the cell end detailed description of its operation have been obtained for comparison with those employed industrially elsewhere. o. The gases from the fluorine cell are passed through a coil insnersed in dry ice (-80°C) to remove HF, The fluorine gas is then mixed with chlorine gas in proper proportions to have an excess of fluorine at all times. A blue flame results at the point of mixture. The gases are then passed through a U shaped tube which is heated to 280°C. The C1F3 thus obtained is condensed in a coil immersed in a -80°C bath and colt cted in iron cylinders. The cylinders are vented several times to allow HF, Gig and Fg to escape. The liquid C1F3 is stable in such iron cylinders for long periods of time. 4*. INDUSTRIAL DEVELOPMENT OF GIF,. a. No industrial development of ClFg was undertaken at Leverkusen. All information on this substance was given to the Laboratorium des Heereswaffen Amtea at Spandau, a suburb of Berlin; this is a laboratory of the Ordnance Department of the German Army. The Army name for the incendiary substance was "C-S" and the plant where it was subsequently manufactured was known as the "Seewerk”. b. The Army built a small pilot plant at Kuramersdorf which is an artillery proving ground about 50 kilometers south of Berlin, slightly west of Route 96 near a town named Speren- berg. This plant was of about the same size as the one at Leverkusen, and differed from it in no essential respect exoept that the fluoride cell was operated at a somewhat higher temperature* While it is not known when this plant was built, it was in operation in late 1943 when visited for a few hours by Dr* Erick N©ack and Dr, Kwasnik, both of I*G* Leverkusen* Dr* Kwasnik has recently moved to the I.G* plant at Bitterfeld; he is a specialist on fluorides and did mode of the development work on ClFj at Leverkusen* During its existence the pilot plant made several tons of ClFj. o* A production plant for GIF- of unknown capacity was built at Gottow which is part of the Kummersdorf proving ground. Drs. Kiebert and Noack do not know whether this plant was ever completed or, if completed, whether any GIF* was produced* They feel sure that GIF was never used by the German Army. V d. Dr, Kiebert was questioned regarding the availability of samples of GIF*. He said none was available and that the laboratory plant for GIF, at Leverkusen had not operated for almost a year* The plant could be reconditioned for the pro- duction of a few pounds of ClFg per hour within a month pro- vided that Dr* Kwasnik could be brought back from Bitterfeld to do the work* 5* EFFECT OF GIF, ON HUMAN BEINGS* a* No fatal accidents occurred during the work on GIF* at Leverkusen. However, experience was obtained with effect of the material on the skin. Contact was immediately followed by a flash flame which did not in itself cause an appreciable burn. However, the resultant formation of HF at the surface of the skin produced a chemical burn. These were treated by washing with buttermilk and bandaging. 6. REC0M&SENDATI0N5. On the basis of the above statements, it is recommended that *- a* Arrangements be made to produce samples of GIF5 at the earliest possible moment to determine if properties are as described above. b. Work on this substance be undertaken by G.W.S. o. The CIFg plants at Kummersdorf and Gottow be considered Black List targets and be investigated at the earliest opportunity. M.F. FOGLER, U*S.Civilian CWS,Hq. ETOUSA* JOSEPH E. SMADEL-j Lt*Col.,Medical Corps* Hq.ETOUSA APPENDIX I. TRANSLATION OF DESCRIPTION OP FLUORINE APPARATUS.- ’’’FLUORINE APPARATUS NO. 3 - for 2000 Amp. The cell vessel as well as the cover consists of Elektron. All the carbon anodes and the sheet nickel cathodes are connected in parallel and electrically insulated from the cell vessel and the cover respectively. To cool and homo- genize the electrolyte (especially during the introduction cf HF) { rgeneration, see Appendix Il),it is pumped through a lateral neutral compartment* containing a compressed air stirrer. A corresponding neutral compartment* on the other end of the cell contains a cooling coil (external cooling). The flowing electrolyte is led back from one end of the cell to the other through an Elektron tube beneath the cell. In this tube there is also a water cooled tube (internal cooling). The neutral compartment with the stirrer contains the BF inlet tube. The neutral compartment with the cooling coil contains a thermometer. In order to detect stoppages of the gas outlet tube, which may be caused by electrolyte dust, a slow stream of N« is led through the electrode compartment so that its flow may be observed in a bubble bottle. The usual diaphragms are omitted; the cell compart- ments are separated only in the portions wet by the melt. The electrolyte is a mixture of lQpt, KF to 2.5 pt. EF, The working temperature is 80-100 C. Because the man who did the experimental work is not available at present and because there are no written records, the above description may contain inaccuracies or small errors here and there. * Presumably electrically neutral - i.e. containing no electrode". APPENDIX II. TRANSLATION OF OPERATING INSTRUCTIONS FOR FLUORINE. 'FLUORINE PREPARATION (OPERATING INSTRUCTIONS) Very Confidential O rt 1. -Temperature control. Keep the electrolyte at 70-75 C, 2. Observe whether the stirrer is working satisfactorily. 3. • Control the level of the melt at 4 cm below the cover. 4. Put the bubble bottle (a high pressure glass vessel filled with K.SO.) under nitrogen pressure. Notice whether there is any stoppage of the pipes. 5. Turn on the direct current machines in the order given by the numbers on the switches. 6. Turn on the current gradually. If the cell operation is not smooth load it with a maximum of 500 amps, and hunt for the source of trouble (level of electrolyte too low, stoppage of the pipes, partially opened valves). 7. Ydien the cell is loaded with 500 to 800 amps, start the internal cooling (outlet temperature 34 to 38°C), with higher loading using external cooling also* 8. The cell is shut down in the reverse order: external cooling off, internal cooling off, current off, bubble bottles turned off, direct current machine shut down* S. The regeneration of the melt is carried out as follows: The HF cans are heated to 40°C thereby the vapor pressure of HF becomes high enough to cause liquid HF to flow into the melt until the HF content of the melt has reached its original value. This can be done nfcile the cell is in operation. A control analysis of the composition of the melt (Titration vdth N/l NaOH and phenolphthalein) is necessary only at intervals of 6 months. (Composition KF 2.4, BF 2.6). APPENDIX II. (Continued) 10* If, for any reason, the melt freezes in the circulating pipe (for example when the current fails), instead of cooling water steam is passed through the internal cooling coil until the electrolyte is again liquid and is pumped through the stirrer. 11, The plate built into the circulating pipe, (thermal expansion equalizing plate), must be continuously heated with gas as it will otherwise swell up with the freezing melt and crack. 12, Yiihen the Works alarm sounds (high siren), the cell must be shut down.** * - . •. ■ • - . APPENDIX III. TRANSLATION OF OPERATING INSTRUCTIONS FOR ClFr "PREPARATION OF C.T.F.(C1F3). (DISRATING INSTRUCTIONS). Strictly Confidential The cooling coil (for removal of KF from F), the condens- ing coil (for C.T.F.) and the storage flasks for C.T.F. were cooled with dry ice. The reaction oven is heated to 280°C and flushed with P. As soon as fluorine can be detected in the cutlet tube, the flow of chlorine is started and regulated as followss- 58 liters Cl per hour with 650 Amp load on F cell gg ii nc n n it it it it it it 134 11 « " " " 1500 " " " " " It II II It II 2000 11 " ” 11 M The maintenance of constant temperature in the reaction chamber follows automatically. Yftiile the cell is in operation, the liquid C.T.F. must be tested every 15 minutes by looking through the peep-hole to see that it is colorless and flowing off quietly. If the flow of C.T.F. is boo slow, there is a deficiency of chlorine; if it is yellow instead of colorless there is either too much chlorine or a leak in the fluorine pipe. As soon as one storage vessel is full, the valves on the condensing coil (for C.T.F.) are reset so that liquid C.T.F. flows into the second storage vessel. The most important thing to do during the preparation of C.T.F, is to watch the apparatus to prevent stoppage of the pipes (formation of If a stoppage occurs, all the liquid C.T.F. that has collected in the cooling coil and pipes must be completely vaporized before repairs can be undertaken. If liquid C.T.F. leaks out, it is covered with a generous quantity of dry ice and the C.T.F. and allowed to vaporize off in a hood. As soon as a steel bottle is filled with C.T.F., it is closed with a degreased Hofer valve and allowed to come to room temperature* A 10 atm pressure gauge is then attached to this valve and a second valve added after the gauge# The excess pressure is then carefully removed by venting Clp^C.K.F.) until the pressure has dropped to 1*2 atm. The steel flasks are then ready for shipment# Leverkusen, 26 September, 1944# (signed) Kwesnik.11