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. ,-* -- W[ ...v ^ ^ , :,". `Sr -'. r cC..: vO,<*s**>r: > ~ v- '-*?> ^^Wsgfe'Si '^3c&?r* ^ .- . fe#^- -^Si:* * Vk'fel?" **? '"* ~ -vi. rs*-* _ ' /3^ ^ Louis Research Report No. 2420 PINAL REPORT ON ASSISTANCE TO SALES AND DEVELOPMENT DEPARTMENTS ON AROCLORS, BIPHENYL AND RELATED PRODUCTS - 1954 y' STLCOPCB4096008 MONSANTO CHEMICAL COMPANY ORGANIC CHEMICALS DIVISION St. Louis Research Department St. Louis Research Report No. 2420 PINAL REPORT ON ASSISTANCE TO SALES AND DEVELOPMENT DEPARTMENTS ON AROCLORS, BIPHENYL AND RELATED PRODUCTS - 1954 JOB NO. 2-02-750.01-2681 January 8, i960 Written by: A.M. Ellenburg Work done by: A.M. Ellenburg DSW 621978 STLCOPCB4096009 DISTRIBUTION FOR REPORT NO. 2420 1. File 2. A. M. Ellenburg 3- J. H. Lum - F. B. Zienty - fils 4. Duplicate file 5. Central Technical Files - C.C. 6. P. G. Benignus ~ General Offices - B-2-S 7- MCL - England 8. MCL - England Extra 10. Extra This report contains confidential information which is the property of the Monsanto Chemical Company which shall be disclosed only to duly authorized persons. The recipient is held accountable for the filing and safe custody of this report which must be returned on demand. . DSW 621979 STLCOPCB4096010 INTRODUCTION During 1954 many requests for physical properties and other data on the Aroclor series of compounds were received through our Sales Department. The information reported here has been used by Sales to assist in the marketing of Aroclors, biphenyl and related products. SUMMARY The requests by individual companies will be fully discussed in the experimental section of this report. CONCLUSIONS Any conclusions are expressed in the various projects written about in the report proper. RECOMMENDATIONS It is recommended that engineering assistance be obtained by the Sales Department to allow a more u::rcugh exploitation of the use of Aroclor 1248 in heat transfer applications. REFERENCES . St. Louis Research Report No. 1306 - Aroclor 1248 as a Heat Transfer Medium - August 26, 1965, A.M. Ellenburg, Job No. 2-02-750.01-2957. EXPERIMENTAL WORK ' A statement of the request and the work done to obtain the information will be reported fully for each company in separate sections of this part of the report. A. Electrical Utilities Company, LaSalle, Illinois manufactures capacitors using Aroclor 1242, Aroclor 1254 and Pyranol l48l (mixture of Aroclor 1254 and trichlorobenzene) as the impregnant. Coefficients of expansion for these products was requested over the temperature range of 25 to 70C. Using the pycnometer method, three density determinations were / made at 25 and 70C. for Pyranol 1481. Pyranol 1481 Density at 25/25C. Density at 70/70C. Coeffici?nt cc/cc/C. Coefficient of Expansion Determinations No. 1 No. 2 No. 3 1.5188 1.4697 C.000742 1.5193 1.4706 0.000736 1.5185 1.4703 0.000729 DSW 621980 STLCOPCB4096011 2. The calculations were made using the formula, d _ = d /T + &< (70-25J7, where^C is the coefficient of expanilon. 70 The Aroclor booklet lists the coefficients for Aroclors 1242 and 1254 in the 25 to 65C. range. Data sent to Electrical Utilities were as follows: Coefficient of Expansion cc/cc/C. cc/cc/F. Aroclor 1242 (25 to 65C. Aroclor 1254 (25 to 65C. Pyranol 1481 (25 to 70C.. 0.00068 0.00066 0.000735 0.00038 0.000367 0.000408 Phosphate Division NB No. 99761. B. Samples of chlorinated biphenyl were obtained from Italian and French producers for comparison to our Aroclor 1254. The Italian samples were from the Societa Elettrica ed Elettrochimica del Caffaro of Milan and their sample is called Fenclor 54. The quality of this sample is much improved over previous samples evaluated in 1952. Prodelac of Paris, France produces Pyralene 1476 which is a high quality material. Small quantities of these samples were received, so only a limited analysis could be made for comparison. Property Corrosion Test-210C., Loss of Aluminum Acidity, mg. KOH/gm. Inorganic Chlorides, Color, APHA 6 hrs. ppm. Aroclor 1254 Lot 1932 None 0.001 0.05 50 Fenclor 54 Pyralene 1476 None 0.001 0.15 50 None 0.001 0.05 30 Dielectric Constant 60 cycles, 100C. 4.33 4.28 4.33 Power Factor 60 cycles, 100C. 4.1# 4.5# 3.4# Resistivity, 100C. 500 volts DC, ohm-cm 1200 x 109 1420 x 109 4800 x 109 The limited comparison shows that these two foreign producers are supplying chlorinated biphenyl to their customers that is equivalent to our Aroclor 1254. This situation, of course, affects our ability to sell Aroclor in these foreign markets. Phosphate Division NB No. 99766-99767-99768. DSW 621981 STLCOPCB4096012 3- C. A Wagner Electric Company 7500 KVA transformer at Monsanto No. 4 substation in the J.F.Q. Plant was down for inspection. This unit stepped 66,000 volts down to 3300 volts. Samples were taken from the transformer and from the switch gear box for examination. Pyranol 1467 Transformer Switch gear Condition Resistivity, 100C. Power Factor, 1 kc, 100C Water, ppm. Dielectric Strength, KV Acidity, mg. KOH/gm. Fe, ppm. Clear 282 x 10 9 0.47% 25 45 Black 0.02 x 10y >60$ 20 29 0.16 35 No doubt the iron in the switch gear Pyranol was the result of arcing and subsequent rusting of the steel. Mineral oil was used to replace the Pyranol in the switch gear box. The transformer sample was in excellent condition and required no treatment. Phosphate Division NB No. 99778 D. Sangamo Electric Company, Marion, Illinois began studies on the use of Aroclor 1242 for capacitor impregnation. Difficulty was encountered in upgrading a drum of Aroclor 1242, Lot TC-3986. Samples were sent to St. Louis for tests. After checking the resistivity of the material as received, 1000 grams of the Aroclor 1242 was stirred with 0.1$ earth for 2-1/2 hours at 70-100C. A second batch was treated Similarly with 0.5$ earth. The attapulgus earth was filtered out and the resistivity of the filtered Aroclor was checked. _ Sample Resistivity at 100C. Original Aroclor 1242 Original Aroclor 1242 N Treated Aroclor 1242 (0.1$ earth Treated Aroclor 1242 (0.5$ earth 96 x 109 ohm-cm. 165 x 109 4100 x log 18,800 x 10y . Samples of our earth and our cell cleaning methods were sent to Sangamo for their use in solving the problem. Phosphate Division NB No. 99784. DSW 621982 STLCOPCB4096013 4. E. Electrical Utilities Company of LaSalle, Illinois requested the vapor pressure of Pyranol 1481 in the temperature range of 0-50C. Since no measurements had been made of the desired property, calcula tions were made from the vapor pressures of the components, 75$ Aroclor 1254 and 25$ trichlorobenzene by weight. Vapor pressure for 1,2,4-trichlorobenzene was taken from Chemical Engineering, Vol. 6l, April, 1954, p. 154. The formula for the vapor pressure of Aroclor 1254 is: log P =- 3780 + 8.62 T(K) Pyranol 1481 Temperature Partial Pressure TCB Partial Pressure Aroclor 1254 Total Pressure Pyranol l48l 112 C. 50 40 30 20 10 0 13-12 mm. 76 .34 .23 .114 .057 .027 .039 mm. .00051 .00022 .000086 .000032 .000011 .0000036 13.16 mm. 76 34 .23 .114 057 .027 Partial pressures were obtained by multiplying the vapor pressure of the components by the mole fraction present, 38$ mole fraction TCB and 62$ mole fraction Aroclor 1254. It is evident that the trichlorobenzene contributes most of the vapor pressure of Pyranol 1481 in the temperature range of 0 to 50C. F. As a result of a flash fire in the exhaust scrubber of an air compressor using Aroclor 1254, Mr. R.B. Sykes of Pan-Am Southern Corporation Destrelan, Louisiana informed us that Aroclor 1254, Lot 105* had a flash point. The reserve sample of Lot 105 and a returned sample from Pan-Am both confirmed the presence of a flash point of 360F. for our non-flammable Aroclor 1254. Infrared studies, distillation and odor tests all confirmed the fact that about three percent biphenyl had contaminated this lot of Aroclor. From Anniston, it was learned that this Aroclor had been pumped into a storage tank which had previously contained biphenyl. Apparently all of the biphenyl had not been cleaned out completely. As a step to prevent the passing of Aroclor by our labora tory, flash point determinations are now made on each lot of Aroclors 1242 and 1254 produced. - Phosphate Division NB NO. 99794. DSW 621983 STLCOPCB4096014 D- G. General Electric Company of Hudson Falls, New York has been using a mixture of Aroclor 5460 and Aroclor 1260 (1:2) as a potting compound. Up to now, G.E. has been making their own mixture and have rejected several lots of Aroclor 5460 because of solid matter which contains iron, non-magnetic dust and fibrous material. No doubt some of the contaminants come from the fiber drums used for packaging Aroclor 5460. A practical solution to the problem is to mix the Aroclors at Anniston, then filter the mixture. A laboratory mix of this new Pyranol 1492 was made, heated to 200C. with 0.1$ attapulgus earth and altered. The resistivity was increased from 25 x 10 ohm-cm. to a high value of 50,000 x 10^ ohm-cm. at 100C. by the filtering treatment. G.E. was sent a sample of the proposed mixture for acceptance tests. , Specifications were set and plant production of this Pyranol 1492 was begun. Composition by weight Aroclor 5460 Aroclor 1260 Properties Color Flow Point (Ball and Ring) Dielectric Strength Condition Resistivity, 100C. 33-3$ 66.7$ Pale Yellow 45-50C. 50 KV min. Clear 500 x 10 ohm-cm., min. Reference Test Methods Sampling Dielectric Strength Resistivity Flow Point ASTM D901 ASTM D924 G.E. Method E4D2-S1 ASTM E28 St. Louis Research NB No. A-57^54. H. Physical Constants of Aroclor 1248 were assembled and graphs were made of several properties over the range of 0 to 600F. These data are specifically for the Aroclor 1248 - Heat Engineering Data Book, which Monsanto is publishing to assist in the design of Aroclor heaters for heat transfer medium. These plots are attached to this report. I. Allis-Chalmers Manufacturing Company of Milwaukee, Wisconsin submitted samples of Aroclor 1242 which they had extracted from Westinghouse and General Electric capacitors. DSW 621984 STLCOPCB4096015 0. The request was made for assistance In determining what produced the yellow color In the Westinghouse sample. Since It is known that Westinghouse uses anthraquinone in capacitor fluid, an ultraviolet absorption spectrum was used to detect the presence of about 0.2$ anthraquinone In the Westinghouse sample. None was found In the General Electric material. Dr. Keller reports that a simple test for anthraquinone was also devised. A small amount of sample is mixed in a test tube with an equal amount of concentrated H2S04 by stirring vigorously with a stirring rod. A positive test at the 0.1 to 1$ level is the formation of a bright yellow H2S04 phase which when standing becomes orange at the interface. A negative test is indicated by a colorless H2S04 phase. The sensitivity of the test method has not been established. The test is not necessarily specific for anthraquinone and it Is conclusive only in the case of a negative test. , DISCUSSION In addition to the laboratory work presented, several visits were made with Mr. P.G. Benignus to firms Interested in the use of Aroclors for various applications. . Cleaver Brooks Company, Milwaukee, Wisconsin was visited In connection with the use of Aroclor 1248 in their heater for barges handling asphalt and bituminous materials. International Boiler Works Company, East Strondsburg, Pennsylvania was visited In connection with the use of the Lamont forced circulation heater for Aroclor 1248 in heat transfer applications. Electrical Utilities Company, LaSalle, Illinois; Gudeman Electric Company, Chicago, Illinois; General Electric Company, Hudson Falls, New York; Sangamo Electric Company, Marion, Illinois and Allis-Chalmers Manufacturing Company, Milwaukee, Wisconsin were visited in the interest of the use of Aroclor 1242 for capacitor manufacture. It was about this time that the entire industry was switching from Aroclor 1254 to the more fluid Aroclor 1242 for lower temperature use. National Cash Register Company of Dayton, Ohio was getting into large scale production on their carbonless reproducing paper. A visit to their plant was made to discuss the handling of tankcar quantities of Aroclor 1242. Several other firms sent representatives to St. Louis to discuss Aroclor applications mainly In the design of plants to use Aroclors for capacitor impregnation. Mr. Robert T. Sutherland of Starring and Company, Inc. (now Ventures, Inc.), Bridgeport, Connecticut discussed their plant for capacitors. Since 1954, the plant was built and Is now In production of capacitors. DSW 621985 STLCOPCB4096016 Mr. Jack Devine and Mr. F. W. Robinson of Deleo Products Division of General Motors Corporation, Dayton, Ohio made two visits to 3t. louis to discuss Aroclor capacitor plant design. So far, their plans have not materialized to build a plant. Mr. M. Meyer of the Wells Manufacturing Company, Foud du Lac, Wisconsin was interested in the use of Aroclor 1254 for ignition capacitors for Ford automobiles. Advice was requested several times during the startup of their operation, but it has been producing excellent capacitors. The Research Group has been glad to cooperate with the Sales Department, especially Mr. P.G. Benignus in promoting a greater and more varied use of the Aroelors. A. M. Ellenburg . de 5-2-60 A" APPENDIX Graph 1 - Density of Aroclor 1248 Graph 2 - Specific Heat of Aroclor 1248 Graph 5 - Comparison of Specific Heat of Thermal Fluids Graph 4 - Viscosity of Aroclor 1248, absolute Graph 5 - Viscosity of Arcelor 1248, Saybclt Universal Seconds DSW 621986 STLCOPCB4096017 LOG G GO DSW 621987 STLCOPCB4096018 SPECIFIC HEAT B T U /lb 8 ./ F _Uj -iOa a ss 0z x*av:* ho2 2 x 200 500 400 TEMPERATURE 8F. 500 /*/ DSW 621988 STLCOPCB4096019 SraC TFlC HEAT B T U /g a llo n / F STLCOPCB4096020 STLCOPCB4096021 VISCOSITY. SAYBOLT UNIVERSAL SECONDS , ft ft Js at s al tf ST ` #' a m a tr- at -i" VISCOSITY. SAYBOLT UNIVERSAL SECONDS' STLCOPCB4096022 - *> -. . >Y> V"' r ^:-. : STLCOPCB4096023