Document 7Mqaj9aeanrZ234d317bzXBGB

REPORT NO. 2215 FINAL . REPORT ON AROCLOR DATA BOOK Job No, 171-451 File No. 141-27.1 AND THE INFORMATION ^TM*ECD HEREIN is the property of THE MONSANTO CHEMICAL COMPANY. RESEARCH DEPARTMENT'- PHOSPHATE DIVI3I0N Anniston, Alabama Report Submitted - April 27, 1948 Chemists: A.M. Ellenburg R.R. Knight Prepared by: R.R. Knight Eighteen copies were.made of this report and distributed as follows: No. 1. Research File , No. 2. R.L. Jenkins - C.B. Durgin No. 3. R.R. Colo - R.S. Weatherly No. 4. W.T. Durrett - F.P. LaBelle . No. 5. H.F. Weaver No. 6. C.A. Hochwalt No. 7. E.P. Rucker No. 8. Edgar E. Hardy No, 9. J.F. Reeves' No. 1C. J.F. Reeves . No. 11. A.M. Ellenburg No. 12. R.R. Kni^it No. 13. Paul Logue N * No. 14. P.O. Eenignus No. 15. No. 16. No. 17. No. 18. ; . . . This is copy No. /5* DSW 331770 STLCOPCB4078345 RESEARCH DEPARTL2NT - PilOTPH.TE 'DIVISION MONSANTO CHEMICAL COMPANY Anniston, Alabama AROC LOR DATA BOOK General information on properties of Aroclors, Aroolor process data, uses of Aroclors, and physiological effects of Aroclors. FOREWORD As a means of presenting the available data on Aroclors to the in terested personnel within the Monsanto organization, this looseleaf notebook is being compiled. Most of the data has x-esulted from work carried out within our own organization. Literature references, howtever, will be cited in all cases throughout the compilation in order to allow more detailed infor mation to bo obtained by the user. The following detailed outline ia for facilitating the location of. data in the book and to assist in properly inserting new data sheets. Each Aroolor is to be given a series number for location under the . general headings. This scheme at present is as followss Aroclor 1221 Aroclor 1232 Aroclor 1242 Aroclor 1248 . Aroclor 1254 Aroolor 1260 Aroclor 1262 Aroclor 1268 Aroclof 127Q Aroclor 1271 Other Diphenyl Aroclors 100 series 200 series 500 series 400 series 500 series 600 series 700 series 800 series 900 series 1000 series 1100 series Aroclor 4455 1500 series Other High Boiler Aroclors Aroclor 5442 Aroclor 5460 - Aroclor 5465 . Aroclor 5468 - 2100 series 2400 series 2500 series 2600 series 2700 series Aroclor 2565 - 3000 series Related Compounds - 4000 serie s DSW 331771 rnLSIJ!hcRT AND the 'NFORAmtion STAINED HEREIN is THE PROPERTY OF THE MONSANTO CHEMICAL COMPANY. STLCOPCB4078346 -2 - The page pertaining to the solubility of Aroclor 4465 in various solvents would be of this type "Llj - 1500",, In cases where the infor mation for all Aroclors can be compiled on one sheet, such as refrac tive indices, the page will be inserted under the general heading and will bear only.the number for the first Aroclor, for example, lAh - 100, I. GENERAL PROPERTIES OF AROCLOR 3 A. Physical Properties . (a) General Physical Constants . 1, Formula and molecular weight 2. Specifications for Manufacture (b) Density and Specific Gravity ` (c) Cubical Coefficients of Expansion (d) Vapor Pressure and Rate of Evaporation / (e) Specific Heat and Heat Capacity (f) Thermal Conductivity . (g) Viscosity (h) Refractive Index i . (i) Heats of Vaporization - Other Thermodynamic Properties (j) Solubilities (k) Flash and Flame Points _ (1) Miscellaneous B. Electrical Properties (a) Dielectric Constants (b) Power Factors (c) Dielectric Strength (d) Volume Resistivity (e) Dipole Moments . (f) Miscellaneous DSW 3317?2 STLCOPCB4078347 3 II,, METHODS OF MANUFACTURE Af Monsanto Process 1. Raw Materials 2. Chlorination 3. Distillation 4. Storage and Shipping . B. German Process C. Other Processes IIIo USES OF AR0CLCR3 * A. Electrical Field . 1. Transformers 2.' Capacitors 3. Coating for '/ire 4. Other uses B. Varnishes C. Plasticizers D. Hydraulic Fluid 3. Fire Retardants F. Heating medium G. Miscellaneous . H. Suggestions for new Uses IV. PHYSIOLOGICAL EFFECTS . I. Skin Teats 2. Systematic Tests . . PATENTS USING AR0CL0R9 DSW 331773 STLCOPCB4078348 - 4- THIS REPORT AND THE INFORMATION CONTAINED HEREIN IS THE PROPERTY OF THE MONSANTO CHEMICAL COMPANY. The took Is subjeot to revision and changes as various data are located. Graphs and diagrams will be inserted when possible and new graphs drawn as information is compiled. No indices of sections is planned at this time, but later re visions may include such pages if the volume of information warrants it. Contributions of new and supplementary data are earnestly so licited. Any discrepancies in the existing data or advice as to a better means of presenting the information will be greatfully acknow. lodged. Address all correspondence to the group leader in charge of the research on Aroclors at Phosphate Division - Research Department, Anniston, Alabama. R. R. Knight ra 12/2/47 A. H. Ellenburg DSW 331774 STLCOPCB4078349 CU.4 - STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON, ALABAMA Page No. ------ PRODUCT: GRADE: Aroelor 1221 CODE NO.: 1040-825-75-09 ItegalarAUTHORIZED: DATE Decenber 4, 1948 PROD. DEPT. NO.: ___ _______________ ___________ SUPERSEDES: HOT-Tontstlvo F ,A*B* APPROVED BY (Initials) 12-17-46 12-10-46 12-19-4G 12-19-46________ Control Specification Consumer Specification Orudis Arcelor 1121 * 3p. Or. at $5C, Acidity, rag, JlaOIt/gm* Aroclor 1221: Color Acidity, mg. NaC&l/gm, 3p* Or* ot 65/15,5*0* Chlorine content Viscosity at 100F, - 1.150-1*160 <C0,5 40 APT1A mas* 0.01 mas* 1,145-1,155 20,5-21.5/ 3G-41 303 NOTES: Copied by re 4/8/48 dSNN 33A775 STLCOPCB4078350 C 411 S4 STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON, ALABAMA Page No. PRODUCT: GRADE: Aroolos 1232 CODE NO.* 1040-830--75-09 DATE Deoenber 4, 1946 XtCfila*;AUTHORIZED:____________________________________ ____ PROD. DEPT. NO.: SUPERSEDES: KwMfentatlvn } A.M.E. f IT *A ,0, APPROVED BY (Initials) 13-17-46 12-18-46 12-19-46 13-19-46 Control Specification Consumer Specification Ggu&e Arcelor 1132: &21. aii 65/25,5C Acidity, ra^s NaOH/gsi, Arcelor 1252: Col os* Aoidlty, ns, NaGH/f^a. 3p* Gr,, at 65/13,5*0, Chlorine ecmtent Tiseosity at 100*F, 1.240-1.245 -C.0,5 50 A.FHA max. ,0a nax. 1,235-1,240 31.5-33.5 46-49 303 - NOTES: Oopis.fi by re 4/6/48 OSNN^716 STLCOPCB4078351 STANDARD SPECIFICATION OF MONSANTO CHEMICAL COMPANY Product; Chlorinated Dlphonyl, flistilled Code Noa 1040-540-75-09 Grade: Aroclor 1242 _________ Date Authorized June 21, 1940 Supersedes Specification Dated July 3S 1934 Tolerable Limits Typical Value Sp.-Gr. at 65/15.5*0. Color, N.P.A. Acidity, Mgra RaOH/grri, Viscosity at 54.4C. 1.338 to 1.348 0.5 Maximum .01 Maximum 47 to 50 Seconds Saybolt Universal Approved by Approved by A. B. Gerber Chief Cfliomist Ethy. A. OeNealt Jr. Works Manager Approved by Robert S Weatherly Sales manager Authorized by J. N. Carothsrs Chemical Director Copied by rs 4/8/48 DSW 331777 STLCOPCB4078352 STANDARD specification OF MONSANTO CHEMICAL COMPANY Product: Chlorinated Diphenyl, distilled i. Grade: Aroclor 1248 Code No, 1040-260-75-09 . .... ... Date Authorized June 21 ,, 1940 Supersedes Specification Dated July 5B 1954 , Tolerable Limits Typical Value . Sp. Gr. at 65/15.5*0. Color,, N.P.A. Acidity, MgmNaC3^/gm Viscosity at 54.4C. 1.404 to 1.414 0.5 Maximum ,01 Maximum 69 to 76 Seconds Saybolt Universal Aroclor 1362 Sp. Gr. at 90/15.5*>C. Color^ N*P*A# .. Acidity, Mgs NaOH/gn. Viscosity at 98.9C. 1.572-1.583 1.0 Maximum .01 Maximum ' 88-100 SCJS Code No. 1040->310-75-09 Approved by A. B. Gerber ~ '" Chief Chemist Approved by Edw. A . O'Nealt Jr. ger Approved by Robert 3. Weatherly______ _ ` ' " ' SaleManager Authorized by J. N,, Carothers______ " --* -* ' che.'7iical Director Copied by rs 4/8/48 DSW 331778 STLCOPCB4078353 9 STANDARD 3PECIFIC-TIQN f CDF MONSANTO CHEMICAL COMPANY ' ' Product: Aroolor 12S4 Grade: Dielectric Code No. 1040-80-75-09 _ Date Authorized 10/5/41 Supersedes: 6/21/40 Color, AIHA Seale Condition Specific Gravity at 65/15,5*C Acidity, M@n. NaOH/gm. Inorganic Chlorides, ppm. Saybolt Viscosity at 98.9*C, sec. Dielectric Constant at 100*C Resistivity at 100*C, ohm-cm. 500 volts Refractive Index at 25 C Distilling Range, Observed, 10# Observed, 50# _ Observed, 90# Pour Point Water, ppm. ' Evaporation, 6 Hrs. at 100 C Corrosion Test-Change in weight Acidity _ after test In6rganic~cElorides - _ after test Condition after test Color after test rs 5/11/48 100 Max. Clear 1.495-1.505 .01 0.10 Max. 44.5-47.5 4.15-4.35 Above 500 X lOy 1.6370-1.6590 350-555C 355-362C 362-375*0 8 to 12 35 Max. . #0.4# 00 0.01 0.10 Max. Clear 150 Max. DSW 331779 STLCOPCB4078354 i STANDARD SPECIFICATION OF MONSANTO CHEMICAL COMPANY Product: Axoclor 1260 Ore do: Dielectric Code No# 1040-290-75--09 ____________ Date Authorised 11/18/41 ' Supersedes: ,1/50/56 Color, AFHA. scale , Condition Specific Gravity at 90/15.5*C Acidity, Mgm. NaOH/gm. . Inorganic Ohlorides* ppm. . Saybolt Viscosity at 98.9C, sec. Dielectric Constant at 100C Resistivity at 100G, oha^-cm. at 500 volts Refractive Index at 35*C Distilling Rang, Observed, 10# 1 Observed, 50# Observed, 90# Pair Point Water, ppu. Evaporation, 6 Era. at 100C Corrosion Test-Change in weight Acidity after test Inorganio Chlorides______ after test Cond itlon _ after test Color after test 100 Max. Clear ' 1.550-1.560 .01 0,10 Max. 79-80 S.6-5.8 Above 500 X 10^ 1,6455-1.6465 370-377*0 377-385*0 385-400*0 26-34 35 Max. 00..20## 0.01 0.10 Max. Clear 150 Max. rs 5/11/48 DSW 331780 \ STLCOPCB4078355 i to m 1crC> oo SPECIFICATIONS FOR SOLID DISTILLED AROCLQR2 Copied by 4/8/48 H o 00 O PM O tIt--ooIl a 0s tiCnoj,- to 0013 O i8to I CM .ar-H< ' 3 u> 1 &03 Ti? O P( a p rH *rl O rH 4 t> H 4^3 3 fe S p. Is aa oto> a ot> rH aa m ft 0S\N 33178A STLCOPCB4078356 d] An 84 STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON, ALABAMA Page No. PROHI ifTt GRADE: Aroolosr 4463 (Regular) CODE NO.: 1040*430^73-09 DATE AUTHORIZED: October 4, 1044 PROD. DEPT. NO.: R #1 W } APPROVED BY ^Initials'! 9-B0^4 II.F.i.j $-39-44 SUPERSEDES: June S,, 1944 P.L. J IVW.f 7.A.B* 10-S -44- 10-3-44 30-4*44 Control Specification Consumer Specification Appearance s Colors $0P*A,$ Point Aoid Number (} Crystslllnlfey clear, 11'"it yellow, brittle resin 3,0 rsax* 60 - 66C. 0 - ,0SS NO, STOSBo * Raising color limit to 20 maximum is recommendd because inspection records <sbow that all lots produced In 1944 itavfi had a color of 1,,5 ` NOTES: Copied, by re 4/8/48 DSW 331782 STLCOPCB4078357 STANDARD SPECIFICATION ' CD? MONSANTO CHEMICAL COMPANY r V Produet; Chlorinated High Boiler Code Noa 1040-480-75-09 Grade: Aroolor 5460 _____________ Date Authorized May 10, 1940 Supersedes Specification Dated December 25, 1932 Tolerable Limits Typical Value Appearance Color, N.P.A. Crystallinity Test Softening Point, ASTM Acid Number Mgm. NaOH/@m. Chlorine Clear, light yellow, brittle resin 2,0 maximum To pass test 100 - 105.5C. 0 - .05 59.0-80.6# Approved by A. B, Gerber " Chief Chemist Approved by Edw. Ac. O'Neal, Jra Works Manager Copied by rs 4/8/48 Approved by Robert S. Weatherly, 5/6/40 " " : "" Sales mnager Authorized by J. N. Carothers, 5/10/40 Chemical blreetoF DSW 331783 STLCOPCB4078358 Monsanto Chemical Company Anniston, Alabama Aroelor Test Methods and Designations Sped if ic Gravity of Aroolora Total Chlorine in Aroclors ksoftening Point of Solid Aroclors Determination of Iron in Aroolor Flash and Flame Points Viscosity Liquid Aroclors Distillation Range of Aroclors Evaporation Test of Liquid Aroclors Refraotive Index of Liquid Aroclors Resistivity of Liquid Aroclors Dielectric Constant of Liquid Aroclors Acid Number of Liquid Aroelor Color of Aroolor - NPA Scale Color of Aroolor - APHA. Scale Acid Number of Solid Aroclors Pour Point of liquid Aroclors Inorganic Chlorides in Aroclors Water Content of Liquid Aroclors 14-10-48 14-13-48 14-17-48 14-21-48 14-24-48 14-29-48 14-31-48 14-32-48 14-34-48 14-35-48 14-36-48 14-42-48 14-43-48 14-44-48 14-46-48 14-47-48 14-48-48 14-53-48 DSW 331784 STLCOPCB4078359 Monsanto Chemical Company Aimiston Method No,, 14-10-48 Specific Gravity of Aroelors The temperature at which the gravities of liquid Aroelors are taken varies with the viscosity of the liquid. Note the temperature at which the gravity is to be taken for the Aroolor under test and heat the sample to 10C. above that temperature. Pour the hot sample into the steam or hot water jacketed hydrometer Jar provided for this test. Stir well with an accurate thermomet&r and adjust the temperature to the desired point by controlling the steam or hot water feed to the jacket. Continue stirring until the temperature remains constant for half a minute. Allow the-hydrometer to sink into the liquid t then read the hydrometer scale at the point of the lower meniscus and record with the temperature. Report the specific gravity to the nearest 0.001 unit. r DSW 331785 STLCOPCB4078360 ' Monsanto Chemical Company Anniston Method Ho* 14-13-48 SUBJECT: . Total Chlorine in Aroclars ____________ _ METHOD: Volhard Titration following Peroxide Fusion Chlorine in Aroolors may he determined by fusion of the sample v/ith sodium peroxide in a Burgess-Parr fusion cup, extracting the fusion with water, acidifying the vater extract with nitric acid, and ore- cipitatlng the ohlorine by addition of an excess of silver nitrate. After filtration, the excess of silver nitrate is determined by ti tration against potassium thiocyanate, using ferric ammonium sulfate as Indicator. - Apparatus . The fusion cup used is the Burgess-Parr Sulfur Bomb No. 3 for flame ignition. A lead gasket is used. For ignition, the bomb is sus pended through a 1-3/16" round hole in a 1/8" transits plate. This allows the fusion cup to extend through the plate for about 5/8 inch. -Ignition is effected by strongly heating the bottom of the fusion cup with the full flame of a Meker burner for two minutes. The bomb, gaskets, and the sodium peroxide ere obtained from the Parr Instrument Company, Moline, Illinois. Charge for Fusion The fusion mixture is made up of about 15 grams (one metal scoop) of sodium peroxide and 0.5 grans of finely powdered cane sugar. The reagents should be free from chlorine, or a blank run and corrected accordingly. The fusion mixture is well mixed by placing the ingre- dlenta in a small glass stoppered bottle and. shaking vigorously. A measuring spoon for the sugar is convenient. . SOLID AR0CL0R3: The non-crystalline type are weighed in the form of small pellets. These are preoared by heating the Aroclor until a con sistency is reached as will permit dropping it from a glass stirring rod onto a tinned surface (a can top), e&ch drop forming a pellet. V/hen cool these pellets can be removed from the surface by inserting > a spatula under them. .4 "Tams are used. The pellets are brushed into the bottom of the fusion cup and the fusion mixture placed on top of them. After tightening the lid, the charge is ready for fusion,, The crystalline type Aroclors are xveighed in the powdered form. j4 grams being used. They are charged in the sane manner as the non crystalline type. .< DSW 331786 STLCOPCB4078361 Total Chlorine in Aroclors -2- LI<5?ID AROCLORS: .20 to .30 grams are weighed by drowning from a stirring rod onto a piece of thin hemispherically shaped glass, or 1/2 gelatin capsul (Gelatin Capsules No. 00, "United Drug Company, Boston - St. Louis), which has been, just previously tared, and which remains on the balance. It is necessary to beat the more viscous Aroclors to "dropping" consistency. The piece of glass then easily slides off the balance pan into the fusion cup. Confer with the fusion mixture. The following quantities of sample, sugar, and AgN03 are used for the respective chlorine contents: Cl Content Weight of Sample Amount sugar AgN0? 0# - 30% 30% - 45% 45% - 58% 50/ - 66% 66% - 70% 0.3 grams 0.3 grama 0.3 grams 0.3 grams 0.3 grams t 0.3 g. 0.3 g. 0.3 g. " 03 go 0.3 g. ' 50 ml. . 50 ml. 50 ml* 75 ml. 100 ml. Procedure Place the fusion cup, which contains the prepared sample and fusion mixture, in the transite ignition plate and apply the full flame of the Meker burner to the bottom of the fusion cup for 2 minutes. (CAUTION: Do not stand too near the fusion during ignition. The use of a safety shield is recommended.) Then remove the flame and cool under the tap. 7vhen cool remove screw cep. Thoroughly rinse the cup cover with water, collecting the rinsings in a dean. 400 ml. beaker. . Then place the fusion cup on its side in the beaker and cover with a watch glass. 50 - 75 ml. will be in the beaker from rinsing the cap, and this is sufficient to decompose thg charge. Remove the cup and rinse well. ".Tien decomposition is complete, rinse off cover-glass and add pure HN03, with stirring, until acid is present in excess to the extent of about 10 ml. (About 50 ml. of acid are required.) Add exactly 50, 75, or 100 ml. of standard silver nitrate solution from a pipet (depending upon chlorine present) and stir to effect coagulation of silver nitrate precipitate. Filter with suction through an asbestos pad on a 1-1/2" perforated porcelain plate and wash beaker and filter 4 times with small portions of cold water. Allow the filter to drain com pletely between washings. Transfer the filtrate back into the 400 ml. beaker and rinse the flask twice, adding the rinsings to the beaker. Add 5 ml. of ferric iron indicator to the solution and titrate with standard KCN3 solution until a distinct pink tint is just obtained. DSW 331787 STLCOPCB4078362 Total Chlorine in Aroclors > -3- Calculation of Chlorine Content Subtract the volume of KCNS required from the volume of KCNS required to titrate the amount of standard AgNOs solution used. This will give the volume of KCNS equivalent to the chlorine in the sample. Multiply the volume so obtained by the chlorine value of each ml. of KCNS and divide by the weight of sample taken. For example: If 50 ml. of silver nitrate solution is equivalent to 61.4 ml. of KCNS solution and the value of 1 ml. of KCNS solution is .003770 gram Cl; then if it is found that 0.3 rram of sample shows a KCH3 titration of 10.4 ml. the percent , of ohlarine is: (61.4 - 10.4) X .003770 X 100 , 64.09# Cl 3 . ' In case the fusion mixture or other reagents contain ohlorine, the amount must be determined and deducted from the chlorine found. Solutions Required . Standard AgNQg Solution: Dissolve 22 grains of silver nitrate in each liter of viater. Protect the solution from light. Standard K'GNS solution: Dissolve 10 '-rams of KCNS in 1 liter of water. Ferric Iron Indicator: Use a saturated solution of ferric ansnonium alum, about 50 g. per 100 ml. of water. Pure Nitric Aoid: Stock acid suffices provided it is colorless. It can be boiled in a beaker until colorless if necessary using 600 ml. HN03 and 300 ml. of HgO. , Standardization of solutions 7eigh 0.3 and 0.15 gram portions of pure dry NaCl into separate 600 ml. beakers. Add 250 ml. of distilled water to each and 10 ml. of pure 50# nitric acid. Vihen solution is complete, add 50 ml. of standard AgNOa solution from pipet. Stir well and filter tjjbrough an asbestos mat on a perforated porcelain plate, using suction. Nash filter and transfer the filtrate back to the beaker in the same manner as when working with a sample. Titrate the filtrates with standard KCNS solu tion, using ferric iron indicator. The value of 50 ml. of A$I03 solution in terms of KCNS solution is ' found by subtracting the ml. of KCNS solution in titrating the 0.3 gram of NaCl from twice the number of ml. of KCNS solution used in titrating the 0.15 gram of NaCl. i DSW 331788 STLCOPCB4078363 Total Chlorine in Aroclors -4- Thie value is checked by titrating 50 ml, of A^T03 solution added to 400 ml. of water and 10 ml. of pure 50# HNOa with KCNs solution. This titration should agree very closely (i 0.1 ml.) with the value found from the titration of NaCl. The titration must he made slowly to avoid drainage error. ' . Since pure NaCl oontains 60.66# 01 by theory, the value of the KCNS in terms of ohlorine may be found by dividing the weight of chlorine in the NaCl taken by the ml. of KCN3 equivalent to the silver nitrate required. . Example: < Two 0.3 gram portions of NaCl show KCNS titrations of 13.11 and 13.13 ml. Two 0.15 gram portions of NaCl show KCNS titrations of 37.28 and 37.24 ml. The KCNS equivalent to 50 ml. of AgNOs is then (37.28 37.24) - 13.12 or 61.4 ml. By titration of 50 ml. of AgN03 against KCNS solution, it is found that 61.36 ml. are required. This agrees within .04 ml. of the value obtained from the NaCl titrations. The chlorine value of the KCNS is then, .6066 X .3 divided by 61.4 13.12 or -.003770 grams Cl per ml. of KCNS. The chlorine value may also be calculated from the titration of 0.15 gram of NaCl. 0.6066 X .15 divided by 61.4 - 37.26 gives .003770 grams Cl, per ml. of KCNS. Precautions 1. The fusion materials have explosive properties if handled improperly; consequently care must be taken to use safe proportions, to secure a good mixture free of large lumps, and to oroperly 3eat the Oover of the fusion cup. The fusion mixture must he kept away from water or moist air, either of which may ignite the charge. The fusion mixture should not be ground to reduce lumps. 2. The method as described is not applicable to volatile organic com pounds unless precautions are taken to avoid loss of sample during weighing. Effect of Variables 1. On account of the high chlorine content of many of the Aroclors and the small amount of sample taken, great accuracy is required in weighing, transfer, and mixing of the sample. The pipet and buret for measuring the standard solutions must be very clean to avoid drainage errora. DSW 331789 STLCOPCB4078364 Total Chlorine in Aroclors -5- 2, Fusions which show black oarbon depo sites on the oover and side of tho fusion oup may or may not give the full chlorine content. If a carbon deposit is found, a second fusion should be made using a smaller sample or reducing the amount of sugar in the charge or both, . 3, Tho temperature at which the standard solutions are standardized . should be noted. In case room temperatures vary from thi3 tem perature, appropriate volume corrections should be made. 4, The fusion mixture materials should be essentially free of chlorine. Tie chlorine content may be determined by making a blank fusion, that.Is, without addition of sample, and titrating in the usual- way. Five ml. of AgN05 may be added instead of 50 ml. portions of AgN05 solution in like volumes of solution and nitric acid. References , Beamish: Determination of Organic Halogens, Ind. Eng, Chora., Anal. Ed., jS 352 (1934). FAB:cm 1--29--45 Copied by rs 4/20/48 DSW 331790 STLCOPCB4078365 Monsanto Chemical Company Anniston Method No. 14-1Tr-A8'^C*][ - SUBJECT: Softening Point of Solid Aroclors METHOD Ball and Ring _________________ Z) This method is a modification of the A.S.T.M, standard method of test for softening point of bituminous materials, serial designation: . E 28~9Wf The-method differs from the etandurd-ngthod--tn-thet--the rings are larger tharL.a two ring support is also U3ed in order that two tests may be made simultaneously. Apparatus Tinhe apparatus consists orf tnhe fallowing: (a) Two tapered brass rings, 5/8" inside dia. at bottom, JK inside diameter at top and 1/4" deep: thickness of '.vail b))''<aKTwo steel balls, 3/8n diameter weighing 3.45 to 3.55 grams eacn.* (c) A 800 ml. Griffin low form beaker, (d) A ring support for the two rings having a brass plate exactly one inch be low the plate supporting the ring, (e) A-800C. A.j.T.K--Ion diattlla-y tlon thermornctqr~gH7dtta. CL. f\STCy Lhw-- /P1PtsCYA jrvwjlJL** . &* Preparation of the Sample / The sample shall be melted and stirred t3\oroughly, avoiding overheating or incorporating air bubbles in the mass and then poured into the ring so as to leave a slight excess on cooling. Since the Aroclors 9hrink considerably on cooling, the ring should be well filled, nearly to over flowing. A little of the excess should be drawn over the top of the ring at several points so as to prevent the cooled Aroclar from dropping out of the ring. .In the same way, the second ring is filled with a standard Aroclor of known'softening point. The standard Aroclor should have a softening within at least 10 to 15*of the Aroclor being tested. The rings while being filled should rest on a clean can lid or on a brass plate which has been amalgamated to prevent the Aroclor from ad hering to it. The Aroclor in the rings should be fully cooled and hardened before proceding with the test. Procedure Add cool solution (employ water for softening point between 0-80*C, glycerin for betoeen 80-200*C., mineral oil for above 200*0.) to the beaker until the surface of the solution is 2" above the plate holding the rings when the ring support is suspended in the beaker. Place the rings containing the Aroclar to be tested and the standard Aroclor on the ring support. Place a ball on the center of the upper surface of the Aroclor in each ring. Suspend the thermometer so that the bottom of the bulb is level with thebottora of the ringj and just midway be tween the two rings. 4 ^AdU^/^C^ jJL., j i~D DSW 331791 STLCOPCB4078366 Softening Point of Solid Aroclara - 2 - ,v tr- Plaoe beaker and apparatus on a ft-** jTinfl hot TV^ftp and heat/\at such a rote that the temperature is raised 5*>C 7 each minute. 'T/L- .'A- O ^ , *7'"^ ~ZTl~J J > rf .' ' j)j j /1 fevjrairl&ui'e/ reciordeli0 by't he^t^ierraomSter^a't or ,--1 i- U r / touches the bottom plate is reported os the softening point,. The heat- hrrftring Is continued until both Aroelors have dropned to the bottom rlate. ' ^o corrections are made for emergent stem. Hotes 1. The standard Aroclor is run along with the sample under test in order to compensate for Tariations in.rate of heating, dilution of glycerin, and thermometer variations. r 2. The softening point of the standard sample is determined by making several determinations using fresh glycerin and carefully checking the rise in temperature of the glycerin so that it is as near as possible to 5C. per minute. ) \ 3. The glycerin may be used repeatedly for the tests after removal of the Aroclor. 4. Benzol is used for cleaning the rings and balls. 5. '.atsr can be used instead of glycerin for softening points up to 90 C . Of 0^ 6 For softening points above 16&*, well boiled glycerin should be used. The usual glycerin is not satisfactory above 125 to 130C, it bolls with loss of water while the temperature remains practi cally constant. It is well to have a supply of high-boiling glycerin on hand to be used only for softening points above 90\^. 7, Air bubbles on the rings and balls during the test should be avoided as far as possible, 8. The rate of rise of temperature of the glycerin shall be uniform for each minute after the first 3 minutes of heating and not averaged over the period of the test. FAB; or 1-&L- Copied'iby rs 4/20/48 0 kJ*-' DSW 331792 STLCOPCB4078367 Monsanto Chemical Company Anniston Method No, 14-21-45 SUBJECT: Determination of Iron in Aroelors Iron In Aroelors may be determined by extracting a benzol solution of the Aroclor with dilute hydrochloric acid until further extractions show no appreciable iron content. The iron in the combined extracts is then determined by diohromate titration, . Procedure Transfer 5 - 10 grama of sample to a clean separatory funnel of about 150 ml. capacity. Add about 50 ml. of benzol and shake until the sample is in solution. . .Then solution is complete, add 10 ml. of 1:1 iron-free HC1 and shake for about 2 minutes. let stand until separation of the two layers is complete, then draw off and preserve the acid extract.. Add another 10 ml. of 1:1 HC1 and shake again. Dravj off the acid layer and combine with the first extract. Continue until HC1 layer is clear. Determine the iron by usual dichromate titration method. FAB:cm 1-51-45 Copied by rs 4/21/48 DSW 331793 STLCOPCB4078368 t Monsanto Chemical Company Anniston Method Ho. 14-24-48 gPBJECT; Flash and Flame Points METHOD: Cleveland Open Cup The flash and flame points of Aroclor shall be determined in the Cleveland Open Cup Tester, following the procedure described in ASTtH D 92-33. Apparatus , . . The cup shall be supported by a metal plate 1/4" {.635 cm) in thick ness and 6 inches (15.24 cm) in width. The plate shall be of brass, cast iron, wrought iron, or steel. In the center of the Plate there . shall be a plane depression 1/32" (.079 cm) in depth, and of just sufficient diameter to fit cup. There shall be a circular opening 2 3/16" (5.50 cm), in diameter, cut thru the plate, centering with the center of the above mentioned depression. The plate shall be covered with a sheet of hard asbestos board 1/4" in thickness, and of the same shape as the metal plate. There shall be cut in the center of the as bestos board a circular bole just fitting the cup. Heat may be supr>lied from any convenient source. The use of a gas burner, electric heater, or alcohol lamp is permitted, but under no circumstances are products of com bustion or free flame allo^jed to come up around the cup. The source of heat shall be centered under the opening in the plate and shall be of a. type that will not produce local superheating. If a flame heater is used, it may be protected from drafts or excessive radiation by any suitable type of shield, that does not project above the level of the upper surface of the asbestos board. The thermometer shall conform to the requirements of thermometer No. 8. ('See A3TL5 table of thermometers). Procedure The thermometer shall be suspended or held in a vertical position by any suitable device, the bottom of the bulb shall be l/4 in. (.635 cm) fro,m . the bottom of the oup, and above a point half way between the center and back of the cup. The cup shall be filled with oil to be tested in such a manner that the top of the meniscus is exactly at the filling line at room temperature. The surface of the oil shall be free from bubbles. There shall be no oil above the filling line or outside of apparatus. The test flame shall be approximately 5/32" (.397 cm) in diameter. The teat flame shall be applied as the temperature read on the thermo meter reaches each successive 5F mark. The flame shall pass in a straight line, (or on the circumference of a circle having a radius of at least 6 inches.) across the center of the cup and at right angles to the diameter passing, thru the thermometer. The test flame shall, .while passing across the surface of the oil, be in the plane of the upper edge of the cup. The time for the passage of the test flame across the cup shall be approxi mately 1 second. DSW 331794 STLCOPCB4078369 Flash and Flame Points -2 - The oil shall be heated at a rate not exceeding' 30*F per minute tem perature rise till a point.is reached approximately 100F below the probable flash point of the oil. Thereafter the rate of heating shall be decreased and for at least the last 50F before the flash point is reached the rate shall be not less than 9F. or more than 11*F per minute. . \ ' The flash point shall be taken as the temperature read on the therrao- meter when a flash appears at any point on the surface of the oil. The true flash must not be confused with a' bluish halo which sometimes surrounds the test flame. After determining the flash point, the heating shall be continued at the specified rate of 9*F to 11 *F per minute* and application of the tost flame shall be made at the specified intervals until the oil ignites and con tinues to burn for a period of at least five seconds. The method of t application of the flame shall be the same as for flash point. The tem- ' perature read at the time of the flame application, which causes burning for a period of five seconds or more, shall be recorded as the flam - point. The flash point and flame point tests shall be made in a room or com partment free from air drafts. The operator shall avoid breathing over the surface of the oil. It is desirable that the room or compart ment may be darkened sufficient^ so that the flash may be readily dis cernible. . Mote ' , Aroolors 1248, 1254, 1260, and higher chlorinated Aroclors do not have a distinet flash or flame point below their boiling temperatures. FAB:cm 1-26-45 Copied by rs 4/21/48 DSW 331795 STLCOPCB4078370 MONSANTO CHEMICAL COMPANY Anniston, Alabama Analytical Laboratory Anniston Method Number 14-4-62 Test Ifethod: Viscosity -- Saybolt Universal Reference: Ifethod No. 11,433-52 VGK GM 25 1. Take a scrupulously clean, dry 60 ml. viscosity receiving flask from the oven and allow it to oool to room temperature while the viscosimeter is being cleaned. (Use only receiving flasks which have been standardized and found to be vdthin +0.06 ml. of 60.00 ml.) ' 2. Clean the viscosimeter tube as follows: A. Insert the cork, which should be clean and in good condition, in place in the bottom of the tube. B. Carefully pour enough benzene into the tube so that the latter is filled and the liquid overflows ihto the gallery. Do not allow any benzene to spill down into the oil bath, as the vapors will affect later viscosities. Caution: , V3iile using benzene for cleaning the viscosimeter, be sure * all circuits of the instrument are turned off. C. Using a thermometer fitted with a holder to prevent it touching the bottom of the tube, stir the mixture well so . that any adhering material is dissolved. Be sure the entire inner surface of the tube and gallery is wet. Pull the cork to drain the tube. With a clean withdrawal tube draw the excess liquid from the gallery and discharge it directly into a beaker -- hot into the viscosity tube. D. Repeat steps A. -- C. inclusive. E. Permit the viscosimeter tube to drain and dry. ABSOLUTELY DO NOT INTRODUCE A CLOTH OR KLEENEX INTO THE TUBE OR GALLERY FOR BLOTTINS UP RESIDUAL LIQUID. t* F. Flush ca. 80 ml. of the well-shaken {and heated if needed to insure fluidity) sample to be tested through the apparatus and follow step C. above. G. Drain this out, and again flush with a fresh portion of. sample to make certain any last drops of previous material have been rinsed out. f H. Shine a pen--light up through the orifice while looking ) . down into the tube. The orifice should be free of fibers or any other obstruction. If these are present, they should be removed by flushirg with sample only, not by use of wires. If flushing with sample fails, inform the super visor. DSW 331796 STLCOPCB4078371 ADDITIONAL PRECAUTIONS: ( A. See that the bath oil, when hot, is not less than 1/4" above the level of the overflow rim of the gallery of the tube. B. The bath oil should be a grade of light-colored mineral oil which has a viscosity of 40 _+ 5 Saybolt seconds at 210F and should, be replaced ivhen it displays a definite darkened color* C. For viscosities to be run at 100F, the bath oil temper ature shall not exceed 100.25F (+ 0.05F for 10 Min.). For viscositites determined at l37yF, the bath tenrperatire shall not exoeed 130.50*F (+ 0.05F for 10 Min. ) For viscosities determined at 210F, the bath shall not ex ceed 212.0F (+ 0.10F for 10 Min.). D. Use only thermometers standardized to the nearest 0.0r.F against a National Bureau of Standards thermometer. E. Use only the stopwatch provided for timing purposes, which should be accurate to within 0.1 per cent when tested over a 60 minute period. Electrical timers must not be used unless the available power source is known to be of sufficiently accurate frequency. The stopwatch juis-; be , left in the holder provided, since variations in its position can cause error. F. Never use the plunger, commonly provided, for cleaning the instument and never expose the viscosimeter to a draft during a determination. 3. Blot the cork dry with a lint--free cloth and insert it in the tube. Pour oa. 150 ml. of sample into a scrupulously clean beakBr which has been rinsed with sample, and heat the contents to not over 7F hotter than the temperature of test. Do not use a sample which has overheated, even if it is then cooled to with-- in the prescribed range. 4. Pour enough heated sample into the tube that it ceases to over flow into gallery. All samples must be strained through the 100 mesh soreen which has been carefully flushed with sample. 5. Stir the sample with the standardized thermometer (with attach ed holder) until its temperature has remained constant within _+ 0.02F of the desired temperature for one full minute (with constant stirring). NOTE: Stirring is a very critical point, especially in the case of more viscous liquids such as Aroclor 1260. Use the exact technique described as follows: SW 331797 STLCOPCB4078372 I 5 { , 1-- Stir the sample with the thermometer, continuously in the same direction, at a measured rate of three revolutions per second. .Alternately sweep the thermometer against the walls of the tube far five revolutions and then stir in the center of the tube for three revolutions. Do not deviate from the prescribed rate of stirring or the practice of stirring five revolutions at the walls of the tube, three revolutions at the center, five at the walls, three at the center and so on for the one-minute period specified. Regulate the temperature of the sample while stirring, by adjusting the oil bath until the desired reading holds constant within 0.02? throughout the required Interval. Do not stir by moving the thermometer up and down unless you desire to cool the sample, and under no circumstances stir in this manner during the one-- minute timed interval. 6. Remove the surplus sample from the gallery, with the scrupu lously clean withdrawal tube which is inserted at one point in the gallery without touching the over-flow rim, and which removes sufficient sample that the level of sample in the gallery is below the level of sample in the oil tube proper. Do not, rotate the withdrawal tube around the gallery. 7. Place the receiving flask in position so that the stream of oil from the outlet tube strikes the neck of the flask. 8. Snap the cork from its position, and at the same instant start the stopwatch. 9. Stop the stopwatch at the same instant that the bottom of the meniscus of the sample reaches the mark on the neck of the receiving flask. 10. Examine the end of the cork to see if it has become moistened with sample. This would denote an incomplete seal and a pre mature seepage of sample through the orifice which would produce erroneous results. The time in seconds, after applying the proper calibration correction of the tube is the Saybolt Universal Viscosity. Different operators in different laboratories should agree within 0.5$ on all readings. Report the results to the nearest 0.1 seconds. Reference: ASTM D-88-44 OPERATION OF THE TAG VISCOSIMETER The viscosimeter is heating when the lamp is off. Do not go away and leave the "quick heat" on. The "viuick heat" should be turned off when the temperature of the bath is within 1 degree of the desired bath temperature. The viscosimeter should be allowed DSW 331798 STLCOPCB4078373 30 minutes to come to temperature equilibrium before making a test. This will allow the metal parts of the viscosimeter to come to temperature equilibrium with the bath. Note: Every now and then, trouble will be found in getting the bath to hold the proper temperature. f 4 i DSW 331799 STLCOPCB4078374 Monsanto Chemical Company Anniston Method No. 14-31-48 ^OBJECT: Distillation Range of Liquid Aroelors METHOD: A.8.T.M. D-30 with Modifications The apparatus, consisting of flask, condenser tube, shield, and ther mometer, is exactly the same as described under A.5.T.M. test D-20 ... "Distillation of Bituminous Materials suitable for Hoad Treatment".^ y: '"7 ' ' 'I Attach a 6 inch auxiliary thermometer (0 - 150#C.) to.distillation thermometer. Place bulb half way between top of cork and probable average of distillation range. Cover both thermometers with a 3/4" diameter glass tube to insure a uniform temperature correction for the exposed stem, barometric pressure and thermometer error. > , -' The procedure is changed only to the extent that thermometer readings are taken when specified percentages (usually 10, 50, and 90) of Aroclor have been distilled instead of following the A.3.T.&. prooedure of weighing the distillate between specified thermometer readings. In testing liquid Aroelors, 100 gas. of sample are weighed into the distilling flask and distillate received in a tared flask or beaker resting on pan of a Torsion balance with 100 gram scale. Procedure / -Telgh out 100 grams of sample into the distilling flask. Assemble apparatus as described under A.3.T.M. D-2Q./ Insert thermometer A (A.3.T.M. high distilling 0 - 400"C.) thru cork in the neok of the -flask so that the top of the bulb is level with the lowest point of -Juncturd-of thetubulature andneckof the flasks- Apply heat to the flaBk supported on two sheets of 20 mesh wire gauze so that the first drop comas over in from 5 to 15 minutes. / Conduct distillation at rate of 50 to 70 drops per minute. Collect, distillate in a 250 ml. beaker tared on a balance. Take temperature : -93, 95, 965v and dry* Corrections for emergent stem and pressure are applied to the thermo meter readings if required. Take eoxreetion "readings at first 4ropy40/.,.50^, 90$, and dry. Report the temperatures to the nearest 1C. Example: /{Exposed stem in degrees) X (temperature difference in degrees) X Q^.000158 * degrees stem Correction The exposed, stem is read from tKe top /of the cork. The "temperature difference is the reading of the thermometer minus the temperature of the auxiliary thermometer. DS\N 33^800 STLCOPCB4078375 Distillation Range of Liquid Aroolors - 2 - S 0.00012 Tb barometric correction =*/Pg Tb - normal boiling point in decrees .absolute} A j? - change in^np assure from 760 ram. Hg x Thp oorrectiop^s added if 'barometer is below normal and subtracted if the barometer is above normal.'(Ma cDouga11 - ''Thermodynamics and Chemistry", pp. 113). Corrected Temperature Observed temperature Ti 1 T2o FABtcm 1-29-45 Copied by rs 4/22/48 oSV\/ 33A80^ STLCOPCB4078376 Monsanto Chemical Company Anniston Method No. 14-32-48 SUBJECTi Evaporation Test of Liquid Aroclors METHOD:____6 Hours Heating at 1Q0C ASTI' D6-59T - Modified Procedure Y'oigh on a rough balance about 50 grams (7 .5 gnu) of the well mixed Aroclor into an accurately tared tin box, 55 ram, dia. X 35 mm. deep (3 oz. Gill-style ointment box, deep pattern), Fisher #1-820. Let stand until box and sample are bt room temperature, then weigh accu rately. Place the box in a ventilated convection oven maintained at 100*C. 1 1 for 6 hours. Remove, cool in desiccator to room temperature and accurately reweigh. From the loss in weight calculate the evaporation in per cent. Report to second decimal place only. Notes 1. Be sure box is at room temperature whenever exact weight is taken, 2. The oven should not contain other samples which might interfere with evaporation. 3. Because the evaporation loss is sensitive to temperature, the air bath must be closely maintained at 100*C. ' FAB:cm 1-29-45 Copied by rs 4/23/48 I DSW 331802 STLCOPCB4078377 Monsanto Cheraioal Company Anniston Method No* 14-34-48 SUBJECT; Refractive Index of Liquid Aroclors METHOD: Abhe Refraetometer Refractive Index The refractive index of any medium is defined as the ratio of the ve locity of light in air to the velocity of light in that medium. It is measured by the ratio of the sine of the incident angle to the sine of the angle of refraction. The denser the medium, the Tester is the refraction toward the normal (higher refractive index). Because the refractive index is characteristic of each substance, it is useful in identifying liquids and verifying their purity, in determining the mo lecular structure of organic compounds, and in soma quantitative analy ses of mixtures. As applied to Aroeldr testing refractive index pro vides a verification of composition and purity. Apparatus . '* * Abb Refraotometer with accessories, Bauseh and Lomb, Cat. #2550, Serial No. 377. Calibrated to read directly in terms of refractive index of the D line (sodium) at a temperature of 20C. Procedure . Operators should he familiar with the Bauseh and Lomb "Directions for Use" and practice the manipulation as there described before attempting determinations on Aroclor. The abridged directions below provide a working outline but at the expense of omission of essential explanatory details which are contained in the B. and L. directions. Screw thermometer into its socket in vjster jacket of upper prism. Open prisms and check their condition. Clean if they are soiled, streaked, or spotted. With lower fixed prism horizontal, place on it 2 or 3 drops of the Aroclor from a stirring rod - sufficient to fill the spaces be tween prisms when clamped together. Close prisms and lock with lock nut. Adjust the instrument and mirror to reflect white light into the refrac- tometer. No spots on air pockets should be visible. Connect water jacket to source of constant temperature water, usually the tap, and pass water until the thermometer has been constant to 0.2C. for at least 5 minutes at 25*C. The Aroclors flow more easily at 25C., hence the choice of this temperature. * With prisms Illuminated, rotate the prisms by means of the index aims until the border of the light and dark fields passes exactly thru the intersection of the cross hairs. If the border line is fringed with oolor, rotate the compensator until the color disappears. If the boun- dS\N 331803 STLCOPCB4078378 Refractive Index of Liquid Aroclors - 2 - dary is not sharp, adjust mirror until a distinct half shadow is ob tained. If the line or the cross hairs are blurred, adjust eyepiece until a good focus is obtained. Secure final fine adjustment by means of the slow motion screw. ' Read the refractive index, estimating to the fourth decimal place. If the temperature of the water jacket is other than 25C., correct to 25 by use of the correction factor, 0.00044 per *C. This factor is applicable only to Aroclors 1348, 1254, 1260, and 1262. It vas found by careful measurement on each Aroclor thru the range 10* to 50*C. The correction is subtracted when the working temperature is below 25C, and added when above 25*C. Example: If the refractive index is found to be 1.6422 at 15*C., the index corrected to 25C. is 1.6422 - (10 X .00014) - 1.6378. Care and Calibration of Instrument Immediately after use, clean the prisms with-swabs of pure cotton dipped in benzol, finally wiping dry with a soft cloth. The prisms, especially the upper one, tarnish and scratch easily. Consequently great care must be taken in cleaning. Before use the prisms should , always be inspected and recleaned if necessary. Vfhen not in use, the refractometer should be kept in its ciosed case. For practice or for checkirg erformance, distilled water is useful. Water has a refractive index of 1.3330 at 20C., with temperature co efficient of 0.0001. A test piece of special glass of known refractive index is supplied with the instrument for calibration and adjustment if necessary of the position of the index arm. Refractive Index of Aroclors - Typical Careful measurements at 25C. have given the following typical values for Aroclors. * Aroclor 1248 Aroclor 1254 Aroclor 1260 Aroclor 1262 1.6295 1.6376 1.6460 1.6482 Substantial departures (over 0.0010) from these values should be in vestigated immediately as they - if correct - indicate substantial error in the composition of the Aroclor or contamination with other materials. % FAB;cm 1-27-45 Copied by rs 4/23/48 DSVV 331804 ^" ' !u=-,- STLCOPCB4078379 $ Monsanto Chemical Company Anniston Method No. 14-35-49 OBJECT; Resistivity of Liquid Aroclars METHOD: __ Resistance Measurements between Conductors l/'-V Apparatus ^' Megohm Bridge: General Radio Company Type 544B, AC operated - 500 volts, serial No. 171. ' This is a direct-current ./heatstone bridge for measuring high resistances, bridge balance being obtained thru use of a vacuum tube voltmeter. Range: 0.1 megohm to 10,000 megohms, covered by a dial and 5-position multiplier switch. A resistance of 1,000,000 megohms can be detected. . -. Test Electrodes: Two concentric nickel cylinders (or brass, nickel plated) with feet. Obtained from General Electric Company. The inner electrode has outside diameter of 2.8" and height of 3.25", with area of 184 sq. cm. The outer electrode has inside diameter of 3" and like height of 3.25", with area of 198 sq. cm. The distance between electrodes is therefore 0.1 inch or 0.254 cm. By theory the electrode constant, area/ length, is 191/0.254 or 752 where 191 is the average area. In practice the cell constant supplied by General Electric Company is used. For. the , electrodes now in use, the cell constant was given as 815. Glass Plate: Pyrax, about 3-1/2" diameter with concentric grooves to assist in spacing the electrodes. Obtained from General Electric Company. Oven: Cenco-DeKhotensky drying oven with two holes in back wall for pordelain tubes for lead wires^ Holes must avoid oven heating elements which occupy 2" paths vertically and horizontally intersecting at the center of the circular wall. Lead 'Vires: Provide 300 ohm Amphenol twin conductor cable to connect the electrodes in oven to the posts of the bridge. The nortion3 exnosed to oven temperature are bared and then covered with norcelain beads. Provide also a flexible lead to ground the bridge tp a water pipe. Clean the leads, beads, and porcelain tubes Periodically. Assembly of Teat Cell The grooved glass plate is placed in an 800 cc. beaker. The clean elec trodes are placed in the grooves of the glass elate with the connector posts directly opposite in order to give the widest possible spacing to reduce surface conductivity. The cylinders should be very close to equidistant. The apparatus should be dried for 2 hours at 100*C. before use. Heat the sample to be tested to about 110*0. on a hot plate and pour into the eleotrode assembly until the level of the liquid is 1/4 to 1/2" above the electrodes. Care must be used to make sure that the DSW 331805 STLCOPCB4078380 SUBJECT: Resistivity of Liquid Aroclor 3 - Page 2,, METHOD : Re si stance Measurements between Conductors lip of the container8 from which the liquid is poured, is clean,, Tilt the beaker in such manner that all air bubbles in the Aroclor will rise to the .surfa co o Air cool to 103~104C. then without removing thermometer,, transfer to the oven which is maintained at 10G*C, and connect the electrodes to tho two flexible wireB which lead to the megohm bridge, "/hen the Aroclor comes to temperature (100C.)f remove thermometer, check csnterlng of electrodes, and procede to measurements. * ' . . Measurement with lTegohm_Bridge Connect the two lead wires to the megohm bridge with the lead from the outer electrode to the L07 unknown post of tho bridge; the inner elec trode to the W+K ur.kaov.ai post-. Connect the GROUND post on the left side to a water pipe. Giving tho spring connectors, pivoted on the "G" post, to the L07 post. Connsot the attachment cord to the 110 V po:,sr supply/ - 7ith the Aroclor at 10CC. t turn the control knob (CJ1SCK~0?RRiTE^OJIARGih to the CHUCK position. Throw all 3 switches at the rear of the Panel to ON. After S minutes bring the galvanometer pointer to zero by means of the ZERO ADJUST knob. * Then turn the control knob to CHARGE for one minute. Turn the knob tc OPERATE and return the galvanometer pointer to zero by adjustment of the MJLTIFLT BT switch and the megohm dial. Read after one minute,, Re peat the CHARGE and OPERATE positions for verification. The resistivity of the Aroclor is the product of the "multiply by" reading times the dial reading times the electrode constant. Report in units of 10^ ohm cm, rounded off to two significant figures. Example: ' "Multiply by" reading: 100 . Megohm dial reading 5.4 meg. ohms Electrode Constant 815 cm Resistivity 100 X 5 A X 815. a 4,4 I 10^ meg. ohm cm ' 440 X 10s ohm cm Values for resistivity are qualified by designation of temperature and voltage. These are 100C. and 500 volts for the test above. Like- con ditions are used at Plant B,, DSW 331806 STLCOPCB4078381 3U3JJD0T;__ Hoalst-iyjty of Liquid Aroclors ~ Por;e 5 HuTHOD: Resistance ''tea gur ement 3 bstv;eon Con flue tor 3 Caro of Apparatus The "Operating Instructions", General Radio Form 458-B, which accompany the megohm bride, recite details of installation, measurements, uses, and construction, illustrated by figures and circuit and firing diagrams No attempt is made to reproduce such information here. The operator should acquaint himself viith the contents of the G.R. manual and refer to it for maintenance of tubes and parts. Then not in use the megohm bridge should be closed ana stored in cabinet. Cleaning Electrodes After the measurements are made the electrodes are removed from the tested liquid, and allowed to drain until the liquid stops runninr from the electrodes. VJhile still hot they are placed in a beaker filled with benzene under a well venilated. hood and allowed to cool. Then cool,, the electrodes or removed from the benzene and scrubbed with povjdered tri sodium phosphate end a benzene carbontetraehloride mixture (50-50 by volume). This scrubbing can be done vrith either, a brush or the hands* The electrodes are then rinsed with acetone, followed by tap water and then distilled water*. The electrodes should not be touched by the hands after the acetone wash. After final rinsing the electrodes are placed in an oven at 1206C. for one hour or until they are used again. The glass spacer plates are cleaned and handled in the same manner as tli electrodes except that they are wrapped in Ions paper before being pljaeed in the oven. \ Calibration For a rough check on the condition of the bridge, one or more cartridgetype resistances of known approximate value should be kapt on hand for periodic or emergency verification of the meter itself. rs 8/3/48 ( - s V . ' ' OSw 331807 STLCOPCB4078382 Monsanto Chemionl Company Anniston Method No. 14-56-52 METHODS Cleaning Dielectric Testing Cells The following method is currently in use in Monsanto laboratories, for cells for the dielectric testing of Aroolors, particularly the GE resis tivity cellso All steps up to (7) ere performed with the cell assembled and in the beaker used in testso (1) Drain cell while hot. (2) Fill with hot trichlorobenzene (TCB); heat for 10-15 minutes. (3) Dlsoard TCB from (2), fill with unheated TCB; let stand a few minutes, drain. (4) Rinse at least twice with methanol, and twice with top water. (5) Fill with hot 10 to 12$ trisodiua phosphate (TSP) solution, heat for 10-15 minutes, drain. (6) Rinse thoroughly with tap water. ' '| (7) Disassemble the cell, rinse the members thoroughly with distilled water. Dry at 120-130*0. for at least one hour. (8) If oell is left in oven over 8 hours, it must be reoleaned immediately before use. . ROTES ' The TSP solution should be .heated to about 100. The TCB should be heated to about 100 to 140*. # Hot TCB is necessary to out Aroolor 1260o Other solvents, e.g., benzene cam be used on lower Aroolors. These suffer the handicap of flamability and lower boiling point. The second filling of TCB, from (3), nay be saved for re-use in (2), provided the sample in the previous test was not too badly contaminated. The ISP solution should be made up fresh about every two days if in continuous use. If a thermometer is to be used in stirring the Aroolor while heating, it shoul< be cleaned by the method outlined above. Developed by: R. J. Good 9/24/52 DSW 331808 STLCOPCB4078383 Monsanto Chemical Company Anniston Method No. 14-36-48 SUBJECT: Dielectric Constant of Liquid Aroclor METHOD; Measured at 100*C. and 1000 cycles Scope ' This method applies to mineral oils and oil substitute used for insu lating purposes. Apparatus Capacitance Bridge Cathode Ray Null Detector Oscillator Constant Temperature Oven --Sarlahls :^r-DoMdauser-^^ 1500 oc. Pyrex Beaker Ceneral Radio Co., Type 716-AIS General Radio Co., Type 707-A " General Radio Co., Type 606-A ^ Cenco-DeKhotinsky #95050 "Pi Procedure Electrode and beaker must be cleaned as directed under "Cleaning Appa ratus for Dielectric Constant", and be at 100C. Heat Aroolor in the -e*as-to Pour over electrode unti 1 plataa-and------ ^ caraf&lo-4.naulatltyn are covered. ( Coane^-Teadsy'^tir with thermometer outside oven until temperature reaches 101f; place in ovett-whrcir-faas-been ffn-nn-riiiTy-fiA-ftrrrtwd^t.n \QQoG. At the time sample is placed in oven its temperature should not have fallen below 90C. Connect leads to capacitance bridge, observing that the lead from insu lated side of condenser goes to insulated terminal on bridge. Balanoe^ "bridge carefully according to direction under "Balancing Capacitance Bridge". Until Aroclor and oven temperatures have become identical the bridge balance will constantly shift. After oven temperature reaches 100C., maintain bridge balance until no pronounced shift is evident. Record reading of capacitance scale multiplied by multiplier setting. Dielectric Constant Capacitance in Aroclor at 100C. Capacitance in air at 100*C. Balanolng Capacitance Bridge Condensed procedure. Operator should read operating instruction for Null Detector for complete details. 1. Connect to power supply leads to oscillator and null detector. Ground the oscillator. 2. Turn on oscillator by pushing 5000 ohm, 10 multiplier, 100 cycle frequency buttons. Adjust harmonic control until oscillation begins as shown by closing of sector in cathode ray tube. DSW 331809 STLCOPCB4078384 Page #2 Dielectric Constant of Liquid Aroclor - Test 14-36-48 . 7'-"'V' 3, On null detector turn brilliance knob to extreme lefft^ the focus knob to extrema right, gain control to extreme left, sweep amplitude 8t raid-scale position, the sweep frequency switch on line side, 1 4, Turn on power switch, lighting pilot light. 5. t'ait fifteen seconds, turn brilliance knob to extreme righto & K' 'j '' . 6.Adjust focus and brilliance knobs until sharp fine line. 7. Connect external terminals on detector to output terminals on oscillator. Switch sweep frequency to external side. 8. Connect detector terminals of bridge to innut terminals of detector, taking care that the black wire (ground wire) of the lead goes to grounded terminal on both ends of lead. 9. Set gain control at mid-scale and selectivity to extreme left. Turn sweep amplitude to extreme left, obtaining vertical line. "7ith 10. V;ith turning control knob obtain the maximum length of this line, keeping it always under l/4- inch with gain knob. p . - ` / -... 11. Set sweep amplitude to extreme left. 12. Set gain control to give vertical straight line of about 3/8 inch. 13. Balance bridge by adjusting power factor and capacitance dials until only a dot remains on the screen vhan the gain control is at extreme right. 14. Set sweep amplitude beyond mid-point,and slightly displace the power-factor dial to obtain a tilted elipse. 15. Adjust phase control until this ellipse closes into a straight line inclined to the horizontal. 16. Bring power-factor dial back to balance position, which should restore the horizontal strai^it line. Displace this control the same amount in the opposite direction. This should again tilt the straight line but in the opposite direction. Adjust phase control until there is no tendency for this lin9 to open up when it is swung 30 degrees . from horizontal in both directions. 17. Throughout these adjustments the other bridge control (the DSW 331810 STLCOPCB4078385 Page #3 Dielectric Constant of Liquid Aroclor - Test l<i-36~d8 capacitance Dial) must be in balance position. If the ellipse grad ually opens when the line is horizontal it nay be brought back to the line again by making alight changes in this control. If confusion results, balance both controls again as in (13) end repeat the suc ceeding adjustmentSo This is the position of bridge balance: An alteration of the power-factor control will tilt the line which does not open apprecia ble thru an angle of 30 to the horizontal both ways; an alteration of the capacitance dial opens the ellipse but does not change the inclination of the major axis. The apparatus may be left this balanced condition,, turned off by switching off first the brilliance knob of the detector, then the power switch, then turning off the oscillator. For successive measurements the controls are not changed, the apparatus left in adjustment. Then the following steps define the procedure: ' 1. Connect all leads as previously directed including that from null detector to bridge. 2. Turn on oscillator by pushing 100 cycle frequency button. 3. Turn on null detector, wait 15 seconds then turn on cathode ray tube. Turn sweep amplitude to extreme left end adjust brilliance to obtain a fine vertical line on screen. 4. Brirp this line to a dot by adjusting the two bridge controls. Initial adjustment is facilitated by having "Gain" control to left. When final adjustment is obtained this knob must be at extreme right. 5. This dot remaining unchanged shows condition of bridge balance. Cleaning Apparatus for Dielectric Constant The condenser is removed from the tested dielectric and allowed to drain while still in the oven at 100C,, The condenser is then placed, while still hot, in a beaker of benzene under a well ventilated hood and allovjed to cool. It is then thoroughly washed with powdered tri sodium phosphate and a 50-50 mixture of benzene and carbon tetrachloride followed by an acetone rinse. The operator should be very careful not to touch the metal plates of the condenser .after this point. The condenser is then rinsed thoroughly with tap water followed by distilled water and dried on a clean paper in an oven at 120*C for at least ,one hour or until it is again used. mwb 3/1/48 . DSVV 331811 M STLCOPCB4078386 Monsanto Chemical Company Anniston Method fto. 14-42-48 SQBJECT: Acid Number of Liquid Aroclors MlTHOD: Titration with Alkali using Phenol Red Scope / The Acid Number is the weight in milligrams of sodium hydroxide re quired to neutralize one gram of Aroclor to pH 7.6. It thus includes any hydrochloric acid, ferric chloride, and other inorganic or organic constituents having acid characteristics. It corresponds to the Neu tralization Number of A3TM Designation D188 except that the latter is expressed in terms of KOH instead of NaOH and has a somewhat higher (phenolphthalein) end point. Procedure To 100 ml. of adjusted (pH 7.6) solvent containing indicator slowly add 0.1 N NaOH dropwise until the color corresponds approximately to pH 7.6 when compared against a suitable reference solution. Readjust if necessary to maintain pH 7.6. Add 50 grams (1 1 g.) of Liquid Aroclor and mix well. Titrate from micro buret with 0.01 N NaOH until the original red color of the solvent is restored. A portion of solvent in a similar container is a useful reference in determining the end point. The match is governed by estimation of the intensity of red because the hue is not exactly reproduced on account of the yellow color introduced by the Aroclor. 1 ml. of 0.01 N NaOH 0.4 Mgri. NaCE. Calculate in terms of Mfja. NaOH per a. of. sample. Report to 4 decimal places. g, of sample ,, Ugm. NaOH/gm. '. Example: If titration is 0.08 ml. for 50 g. of Aroclor, the Acid Number is 0.08 X 0.4/50 0.00064 Kgra. NaOH/gm. Report as 0.0006. Solutions Required I Solvent: Mix 600 ml. of benzol, 200 ml. of 3-A alcohol and 200 ml. of acetone. Add 5 ml. of 0.2/ phenol red solution. Phenol Red Solution, 0.2/: To 0.1 gm. of dry indicator in a small, beaker add exactly 2.0 ml. of 0.1409 N NaOH. Stir to dissolve and dilute with 3-A alcohol to 50 ml. Reference Buffer pll 7.6: Dissolve 0.41 g. NaH2P04 and 0.59 gm. Na3IIP04 (both anhydrous) in 100 ml, of water. Add 0.5 ml. of 0.2,. phenol red. Solution is used for reference in adjusting the solvent if Lal'otte pH 7.6 color standard is not available. DSW 331812 STLCOPCB4078387 t Acid Number of Liquid Aroclors - 2 - Standard 0.01 N NaOH: 5 ml. of .5 N NaOH to 250 ml. vol. of 3-A al cohol. Protect at all times from atmospheric C02. Note By using 250 ml. acetone in solvent instead of 200 ml. a 100 gra. sample of 1254 my be taken for analysis. FAB:cm 1-30-45 Copied by ra 4/23/48 1 DSV\/ 331813 STLCOPCB4078388 Monsanto Chemical Company Anniston Method No. 14-45-48 ' SOBJECT: Color of Aroclor on N.P.A. Scale METHOD; Helllge Pocket Comparator Scope * . * The method is applicable to Aroclors 4465, 5460, or others having N.P.A. colors in the range 1 to 5. Procedure .' ^arm the Aroclor is necessary to obtain pouring consistency* Fill the test cup of the Hellige Pocket Comparator, Model 605, with Aroclor, insert cup in the comparator, and compare against the color disc (No. 620C-50, Lubricating Oils and Petrolatum) which has N.P.A. colors from 1 to 5 in one-half steps. Report color to nearest 1/4. Clean the test cup with a mixture of CCl^ and benzol, with final rinse of benzol. ASTI' color numbers coincide with National Petroleum Association color number (1915). The relation of the N.P.A. color numbers to other color scales i3 tabulated below: ! NPA Color Nos# (1915) NPA Names Union Petro leum Co. A3TI* Color Nos. Lovibond Analysis Red Yellow .Blue 200 510 1180 1/4 1/2 3/4 1 1-1/2 2 2-1/2 5 3 -3/2 4 4-1/2 5 6 7 8 . -- Lily white Cream wHite Extra pale . Extra lemon pale Lemon- palu Extra orange Orange pale Pale Light Red Bark Red Claret Red ^ G H I J K L .K N 0 P R . -' * -. . 1 0.12 1.5 0.60 2 2.5 2.5 4.6 3 6.9 3.5 9.4 4 14.0 4.5 21.0 5 35.0 6 60.0 7 60.0 8 166.0 0.6 1.1 1.7 2.4 8.0 26.0 27.0 33.0 45.0 50.0 56.0 * 93.0 60.0 106.0 64.0 ~i wm 1 - .55 .55 .55 1.80 FAB: cm 1-26-45 Copied by rs 4/27/48 oS'N STLCOPCB4078389 Monsanto Chemical Company Anniston Method No. 14-44-48 SUBJECT; Color of w'.Tater -Thite" Aroclors METHOD: Comparison against A.P.H.A. Scale Scope The method is applicable to Aroclors 1254, 1260, or others having color less than N.P.A. #1 ("2ater Ivhite") . A.P.H.A. Standards These color standards are acid solutions of potassium chloroplatinate and cobaltous chloride. The unit of color is that produced by 1 mg. of platinum per liter. The ratio of cobalt to platinum may be varied if necessary to match the hue. Because the hue of Aroclor 1254 and 1260 seems best matched without`cobalt, this has been omitted in the prepara tion described. Dissolve 1.245 g, of potassium chloroplatinate (KgPtClg) containing 0.5 g. of platinum in water with 100 ml. of concentrated hydrochloric acid, and dilute to 1 liter with distilled water. This solution has a color of 500. Prepare standards from 10 to 100 in steps of 10 by diluting 1, 2, 5 ml. etc. of the above solution with distilled water to 50 ml. in standard high form Nessler tubes. Protect the tubes from evaporation. Refer to page 13 of "Standard Methods for the Examination of 7afcer and Sewage" eighth edition (1936) for details of standards containing cobalt. Published by American Public Health Association, 1790 Broadway, New York. Procedure Fill a matching Nessler tube with Aroclor to a height equal to that in the standard tubes. Compare with standards by looking vertically doivnward through the tubes upon a white or mirrored surface placed at such an angle that; light is reflected upward through the column of liquid. A color tube support (Fisher #7-065, 50 ml.) is convenient. Inasmuch as the proportions of the standard color solution in the compari son tubes are such as to represent an Gliquot part of a liter, the readings are direct as parts per million* Colors up to 100 are recorded to the nearest 5. Direct comparisons are satisfactory up to 100. Above this the sample should be diluted with Carbon tetrachloride (maximum A.P.H.A. color, 6), and the color obtained to nearest 10 by multiplying by the dilution ratio. FAB:cm 1-30-45 DSW 331815 Copied by rs 4/27/48 STLCOPCB4078390 Monsanto Chemical Company Anniston Method No. 14-46-46 'SUBJECT: Acid Number of ^olid Aroclors and Heavy Liquid Aroclors METHOD; Titration with Alkali U3lng Phenolphthalein________ ___ Procedure Dissolve 50 grams of the Aroclor in 50 ml. benzene in a 400 ml. beaker, warming to hasten solution. Add 50 ml. 3A alcohol, 200 ml. distilled water, heat to boiling, add 1/2 ml, 1$ phenolphthalein solution, and titrate, in the case of the distilled Aroclors with 0.01 N sodium hy droxide solution, to a faint pink color which is permanent for at least two minutes after vigorous stirring. A reagent blank should be run con currently. The acidity of the sample is calculated as milligrams of sodium hydroxide required per gram sample. _ Calculations Using 0,01 N_ NaGH, Acid No. = ml. titration X 0.4/sample weight For 50 gm. Aoid No. (ml. tit. ml, blank) X 0.008 Using 0.1 N NaCH, Acid No. ml. titration X 4.0/sample weight For 50 gn. Acid No. =* (ml. tit. - ml, blank) X 0.08 Apparatus 10 ml. burette in .05 divisions. , Conversions 1. To obtain Neutralization Number in terms of KOH, multiply the Acid Niuriber in terms of NaOH by 1.402. Inverse factor is 0.713. 2. Multiply the Acid Number by 1000 to obtain the parts of NaOH re quired to neutralize one million parts of Aroclotr. Thus Acid Number of 0.0006 is equivalent to 0.6 parts of NaOH per million parts of Aroclor. 3. The large amount of water used causes sharper separation of the aqueous layer from the non-aqueous layer, thereby making the endpoint more eaeily distinguishable. If the titration is carried out against a very light background or in a fluorescent light, the end point is easily seen. 4. Aside from free acid as a cause for NaOH consumption, ferric chloride which is usually present in small amounts, also consumes NaOII in neu tralization to phenolphthalein. It therefore, follows that an Aroclor of very low acid number nust be also extremely low in ferric chloride. FAB:cm 1-26-45 DSW MA81& Copied by re - 4/27/48 STLCOPCB4078391 Monsanto Chemical Company Anniston Method No. 14-47-48 SUBJECT: Pour Point of Liquid Aroclorg METHOD: A.S.T.M. D-97-39 The pour point of an Aroclor is the lowest temperature at which the material will flow when it is chilled under certain, prescribed condi tions ,listed in A3TM D 97-59. . Apparatus x ' Apparatus consists of test jar, thermometer, cork. Jacket, disk, gasket, and bath as described under A.S.T.M. method D97-39. The thermometer is the A.S.T.M. Cloud and Potir Test, range -38 to 50*C. Present apparatus is the Emil Greiner Co. #GR 2234 bingle unit with Gr2242 test jar. Procedure for Aroclor Follow D97-39 in all respects except that the centigrade scale is sub stituted. Only an outline follows: Add 40 ml. of Aroclor to test jar.: Adjust thermometer to center of Jar with beginning of capillary 1/8 inch below surface of the Aroclor. VTarm the Aroclor without stirring to 46C. in a bath at 46~48C. Cool to 32C. in air or water bath at 25C. Trans fer the jar to the jacket of the cooling bath which is maintained at 0 to 3*C. Beginning at a temperature 8 to 10 degrees above the pour point, at each interval of 2C., removh the test jar from the jacket and tilt Just enough to datemine if there is movement of ths Aroclor. This inspection should not require more than 3 seconds, ".'/hen movement is not promptly apparent, the test jar should be hold in a horizontal position for exactly 5 seconds as noted by a stop watch. If movement occurs, immediately return the test Jar to the jacket. Repeat test for flow at the next temperature 2*0. lower. Continue the test in steps of even degrees centigrade (14,12,10, etc.) until the Aroclor shows no movement when the test jar is held horizontally for exactly 5 seconds. This is the solid point. The pour point is the previous temperature, 2#C. above the solid point. The pour point is thus the lowest temperature at which the liquid will flow or pour under the test conditions. Technicians must familiarize themselves with D97-39 which gives complete details of apparatus and procedure, reproducibility of results, effects of thermal history, etb. The directions above are inadequate except as a working outline. The bath temperature is controlled by adding dry ice to acetone for pour points below 0*C. FAB:cm - 1-30-45 DsW 331817 Copied by rs - 4/27/48 STLCOPCB4078392 Monsanto Chemical Company . Anniston Method No. 14-48-48 SUBJECT: The Testing of Aroclors for Inorganic Chlorides METHOD: Solutions Required Standard Chloride Solution: Dissolve 0.660 grams of pure sodium chloride in sufficient water to measure exactly 500 ml.; 1 ml. then contains 800 micrograms Cl. Pipette 25 ml. of this solution to a 500 ml. flask and make to the mark to give a *0.00113 M NaCl solution, 1 ml. of which con tains 40 micrograms of Cl. Preserve Id a Pyrex bottle. Caution: The water used in preparation .must be chloride free by the Tyndall Beam test; the 0.00113 M solution should not be kept over 1 month. Silver Nitrate Solution 10$: Dissolve 5 grams of silver nitrate orystals in 40 ml. of water and add 10 ml, of concentrated nitric acid. Chloride free distilled water. Apparatus Required . . LaMotte 10 ml. color tubes (13 mm. X 100 ram). Test tube rack with a black surface at the base for uniform comparison (Note: we are using black gasket rubber over the entire board that sup ports the base of test tubes during comparison.) . Box. About 7" long and 4" wide. This box contains holes in top and notches in the bottom to hold Lamotte color tubes. It is just higfr. enough to allow 1/4" of test tube to extend through the holes in the top. The hox should be painted a flat black on the inside and on top and should contain enough holes to accomodate at least sevea tubes. Method Clean all flasks, tubes, and pipettes to be used. Then rinse with dilute nitric acid then with chloride free distilled water. . ' ' <>{/<' / ' Add 50 ml. chloride free water to a 250 ml.^Erlenmeyer flask, heat to boiling, add 200 gram of the Aroclor to be tested, which has been heated to 100*0, shake vigorously for 1 minute, cool in cooling pan. Carefully decant some of ths water extract to a separatory funnel. V/ash with pure ethyl ether (chloride free). Transfer 10 ml. of the ether washed extract to a 10 ml. Lalfette color tube after rinsing tube with portion of extract. Prepare standards by diluting exactly 5 ml. of the 0.00133 M NaCl solution to 100 ml. in a OS'N STLCOPCB4078393 The Testing of Aroolors for Inorganic Chlorides - 2 - volumetric flask. One ml. then contains 2 micrograms of Cl. Transfer 1, 2, and 3 ml. portions to 10 ml. tubes. I5ake to the 10 ml. mark with Cl free H0. Place standards and sample in light free box from which only the top of tubes are exposed add 0.5 ml. of the silver nitrate to each tube compare in a specially preoared test tube rack. The comparison is to be made quickly and from a constant source of light, preferably day ligjit from a window away from ths sunlight. Comparison is. easier when other sources of light are shielded from the comparison ' rack. Look directly into the top of the tubes and compare. Note the known solution which most nearly matches the water extract estimating to the nearest whole microgram. The extract blank and the distilled water should show no turbidity. Calculation- Divide the chloride content in micrograms of the known solution which matches the extract by the weight of the Aroclor represented by the extract to obtain the chloride content of the Aroclor in p.p.m. In the procedure described, the 10 ml. extract represents 40 grams of Aroclor (1/5 of 200 g. ta2cen). The three knowns contain 2, 4, and 6 micrograms of Cl, thus representing 0.05, 0.10, and 0.15 p.p.m. respec tively. Values should be reported to the nearest 0.025 ppm. Precautions . Because of the sensitivity of this test, serious errors may result tteough very slight contamination or inattention to details. All equip ment must be scrupulously cleansed, the distilled vjater absolutely chloride free and testing done away from fumes of HOI or chlorine fumes. 4/27/48 . - 7 'X k DSW 331819 STLCOPCB4078394 Monsanto Chemical Company Anniston Method No, 14-53-48 SUBJECT; Water Content of Liquid Aroclors METHOD: Titration with Karl Fischer Reagent Outline The Aroolor is dissolved in a mixture of benzene and methanol which has been titrated with Fischer reagent to the characteristic end pointo Fischer reagent is a solution of iodine, sulfur dioxide, and pyridine. Iodine is consumed as long as any water is present. The solution is again titrated to obtain the water content introduced by the Aroclor. ' Solutions and Apparatus Karl Fischer Reagent: Wei^t into a flask 264 grams of pyridine, Barrett 2-A or Eastman 214-H, and add 61 grams of liquid or gaseous sulfur dioxide* Add the liquid sulfur dioxide directly from the inverted cylinder by attaching to the outlet valve a glass tube extending into the pyridine. Sulfur dioxide gas can be bubbled into the pyridine until proper amount is added. Store in a glass stoppered bottle. Transfer 65,6 grams of the pyridine-SO2 mixture and 134 ml of absolute methanol to a 1 liter Florence flask. Cool thoroughly in an ice water bath. Add 16q9 grams of iodine, stopper, cool again before shaking. Alternately cool and swirl until the iodine is in solution. Makes 200 ml of resgent. Store in glass stoppered bottle. Let stand 24 hours before asing. vjhen fresh, one ml of reagent is equivalent to about 0,0033 #ns. of water. Aroclor Solvent: Mix 2 parts dry benzol with 1 part anhydrous methanol. The dry1 benzol is prepared by shaking the commercial grade with anhydrous calcium chloride, decanting into a flask and distilling, rejecting the first 10 to Come over. Keep in glass stoppered bottles with minimum exposure to air. Micro Buret: 10 ml. x 0.05 ml. Koch automatic with glass stoppered reservoir. Eck and Krebs #2460, Equip reservoir with a moisture guard tube containing Drierite or a similar dehydrating agent. Procedure Heat a clean 500 ml. narrow mouth Erlenmeyer flask in an oven or on hot plate until thoroughly dry. Sweep out for 10 minutes or until cool with air which has been thoroughly dried by passing thru tubes containing 8 mesh Drierite. Disengage the flask from the aspirating train and imme diately close with a paper cap held by a rubber band. DSW 331820 STLCOPCB4078395 Y/ater Content of Liquid Aroclors - 2 - '.Jithout delay, transfer 100 ml, of the benzene-methanol solvent to the . flask thru a snail hole punctured into the paper cap. Cover again with paper. Titrate at once with Karl Fisoher reagent to distinct red-brown end point which does not fade after swirling several times. The Fischer ( reagent is dispensed from the microburet the tip7 of which projects into the flask thru the puncture in the paper cap. At the end point any water content of the solvent has been reacted. Superimpose a fresh paper cap . s immediately. ' / . Obtain weight of the solvent and well-covered flask on a Torsion balance or equivalent. Quickly introduce with a dry pipette about 100 grams of the slightly warmed Aroclor to be tested. Cover at once and weigh again to obtain the weight of Aroclor to nearest gram. Shake until the Aroclor ' is dissolved. , If the mixture is cloudy, warm sli$itly. If cloudiness persists another 7 mixture should be prepared. Puncture a small hole in the paper cap for the insertion of the buret s tip and titrate with Fischer reagent to the first definite broym color, ' agitating with a gentle swirling motion. The end point should persist . through several swirls. The end point may slowly fade througi slow aoeess of atmospheric moisture in which case it is rest cared by a drop . . or two of reagent. If not so restored, the end point may have been a false one or the closure is faulty. A definite end point is impossible if humid air is not well excluded. From the amount of reagent required and the weight of Aroclor used, cal ' , culate the water content in p.p.ra. Calibration of Fischer Reagent and Standard "feter Solution Standard water solution in methanol: Transfer exactly 0.40 ml. of water from a micro buret or a 1 ml. measuring pipet to a 100 ml. volumetric flask. Fill to the mark at once with anhydrous methanol and mix. One ml. of solution then contains 4000 micrograms of -rater in addition to any water which may be present in the methanol. Transfer exactly 5 ml. of the above standard water solution (equivalent to 0.02 grams of water) to a 250 ml. Erlenneyer flask which has been dried and swept with dry air. Close with paper cap end titrate with Fischer reagent in the same manner a s the sample. The end point is sharp. A methanol blank, found by titrating 5 ml. of the methanol used in making up the standard water solution to a like end point, must always be subtracted from this titration. Divide the amount of v;ater taken by the -net Fischer reagent required to obtain the titer of the Fischer reagent in terms of water. Example: A 5 ml. aliquot of standard solution, equivalent to 20,000 microfTams of water, required 6.61 ml. of Fischer reagent while 5 ml. DSW 331821 STLCOPCB4078396 WatervContent of Liquid Aroelors - 3 - of the methanol required 0.55 of Fischer reagent. 20,000/(6.61 - 0.55) 20,000/6.06 .. 3300 micrograms water/ral. Reoalibrations: Because the Fischer reagent deteriorates rapidly, its titer must be determined for each days use. If the same standard water solution is used in recalibration as in the initial calibration, the titer of the Fischer reagent must be calculated from its total water content (Including that introduced by the methanol). Hie total water is the product of the initial gross titration and its titer. This in the example above the total water content of a 5 ml. aliquot is 6.61 X 5300 * 21813 micro grams. If on recalibration 7,37 ml. of Fischer reagent, is 21813/7.37 2960 micrograras of water per ml. Two or more calibrations should be made with agreement within 0.025 ml. Calculation of HgO sample standardization of Standard H^O sol. . . Titrate 5 ml. mixture HgO sol. Titrate 5 ml. of methanol Tit of 5 ml. mixture A Tit of 5 ml. methanol B , A - B 'ml. reagent for HgO added 5/100 of .4 Divide 5/100 X A by A - B factor grams of H20/ml. . Multiply factor X B giving gms. of Hs0 in 5 ml. of methanol. Add this wt. of HgO to .02 already added giving HgO in 5 ml. (Total) Factor ^^ . HgO St'd Titration ^ ^ X sample Titration Ta Tg X 1,000,000 ppm HgO wt. sample . . , FAB: cm 1-27-45 Copied by rs 4/27/48 DSW 331822 STLCOPCB4078397 I-A-d-B-4000 -O c >> ' *3 CO Pr4.."W"```s,* DSW 331823 STLCOPCB4078398 From 1 'PROPERTIES OF BASIC "HALOUAY" I RODUCTS L e tte r to VI.C T.,Bolaer (Halowax P ro d u cts D iY 0,,U nion C arbide and Carbon C o rp ,,t 30 E, Forty-S econd S t,* N,Y= 17,; N 0Y c )0 L e tte r dated Feb. 27,, 1948. . I-A-B-4000 From - Halowax Products Division Union Carbide and Carbon Corporation 30 East 42nd Street New York 17, New York Letter - N.C.M./J.1T. Cole, Tech. Pep, 2/16/48 Zyrox 3009 (11-313) GENERAL INFORMATION Color Sp. Gravity Softening Pt. Stormer Viscosity Saybolt Furol Viscosity Penetration at 50*C. Penetration at 25eC. Flash Pt.' Fire Pt. Combustibility Fracture Acid Resistance Alkali Resistance Volatility P.F. at 25*C. (1000 cycles) Diel. Constant at 25#C. (1000 cycles) DC Resistivity at25C.- - Brown - 1.40-1.45 at 25C. - 79-83C. - 59-89 at 130*C. - 79-180 at 130*C. - Approx. 15 (200 gm. load) - Less than 3 (200 gm. load) - Approx. 590#F. - None to 600*Fc - '.7 ill not support combustion - Conchoidal - Excellent - Excellent - Average for 24 hours at 130C. Less than 0.10 mg./s^.cm./hr. - Approx. .001 - Approx. 2.96 - Over 10 meg. cms. Copied by rs 4/2/48 DSW 331824 STLCOPCB4078399 From - Halowax Products Division Union Carbide and Carbon Corporation 30 East 42nd Street New York 17,, Nqw York < ' Letter - j'.C.H./T.M. Cole, Tech. Rep. 2/16/48 Zyrox 3007 (11-308) GENERAL INFORMATION Color Sp. Gravity Softening Pt. Stormer Viscosity Saybolt Furol Viscosity Penetration at 50 deg. C. Penetration at 25 dega C. Flash Pt. Fire Pt. Combustibility Fracture Acid Resistance Alkali Resistance Volatility P.F. at 25 deg. C. (1000 cycles) Diel. Constant at 25 deg. C. (1000 cycles) ~ DC Resistivity at 25 deg. C. - Brown - 1.29 - 1.32 at 25 deg. C. - 65 - 70 deg. C. - 20-27 at 130 deg.- C. -20-30 at 130 deg. C. - Approx. 75 (50 g. load) - Less than 3 (200 g. load) - Approx. 530 deg. F. - None to 600 deg. F, - 'ill not support combustion - Conchoidal - Excellent - Excellent - Average for 24 hrs. at 130 deg. C. tfrSo mg./sq.cm,/hr. - Approx. .004 . - Approx. 3.0 - Over 10s meg. cms. Copied by rs 4/2/48 STLCOPCB4078400 STLCOPCB4078401 c 1-,r ' . - J STLCOPCB4078402 ,,r ^ STLCOPCB4078403 Clopkens a re n o t com bustible and do n o t support com bustion o f m a te ria ls .in to vfriich they are im pra/pieted. Pages 108 109 Item Nos* t 7, 28, & 31 From" : B Ia0 .3 . Fl-in a l R ept. Nb. 893 . ' (a s quoted In I . CL F arbens s a le s sheets) PHYSICAL AND CHEMICAL PRQPSRTIE3 OF CLOPHEH OILS m 23 fi a8 II . tHOO <J * erl Bds n & o ts rH O I oCO o I I I CQ rH A o& ' ' ' 0> M rH CQ o <0 03 oH M 4 ^ s 0o *fCaD 0o *V CQ 2e S ! QR > * ''Is2 ^5. 6 (D O {3 roH in + H* CQ Ti if; in to S'- CQ O 10 VO O O O, CQ g 0c as o (m9 & rtfHi>dId Oto .2 !s 3 oo Oo k CncqO-og,fH2H` Vtcs vnA C--li o iOcnv> m S $o o Nf so o V 8 Xg-in & a > to Hpi rf-tl Iinf) Vs h K1 . w0 in cq n o 2 IB O + CQ 2 CQ M rH rH OO o to CQ H VAf oCQ o- o 'aG" oO o V t8 .c o fs 2cr > rraa re22H iO22H 'HC(JDi m< co ` --. 2VlOJ.'toOi- m O rH ^rH 0 ii--ni CQ VOi. Nf5. o O C3 as2 3^ u a iH X m rUH H in f2j. to *3 H CQ 2 . ViVi. fH rH C0 Pc CO 10 t rH ~--" fH Oo 165 0 in 3 .8 1 9 O 'E* O O O I-A-B-10 iH a V) M rH A o CD o rH W o rH O S fH H H* O Q gj \ rH o |BvSM V O iH > CQ 0 tn 00 3 rH i^o S0 0 Qe O \ tH O 0 > M 0 0 OO Ni O CQ rH |! APPENDIX. I I . t , O oP4 o o CQ tPo >> +> 43 H orl >2 Pd 6 0 0 oo CQ CQ II :a -p P oo ion 4a fH iH +03 O 8 rH -+r3l 43 81 O2 d-', A I$S* s:o Bo 3fH rOH o *4 COpO>- too .2 rPHh t >1 I f> Pd O M; tH foH CQ ss a --a) Ca* o l-s, p, =! ft ffl fH DSW 331829 STLCOPCB4078404 CtoD 03 k OC~ c O 0to3 03 rH PS3 <T> P l? to n to e $ % V' Ito "0 <90 Pa 01 5 ft <2 I E* s to IWI (b) (g) B (a) - 300, 2100 w HO'--' P p o P 0 O O O O rH P o -p HOHaOWPrHa 'H-- S tno ccon tcso tno to tcot> 'l1 v}< ^ tj< 8 8 PO a Vi p H *H P ttfo> a \ n03 otjiintootj*g*3Nto 5 VOi co & to H rH rH H rH rH t a p s 3 - popto ft to I phoj r>ao> pa to o p O rH O BOOH r-l P CVJ c- in co cc WOOm M.OO to Oo>J to << ^ *4* r8H o Voi {> CT a H sI s Ao u 01 to N W O rf o ao u ctoo Ot* H^ tNn 0x3* tton to PUtoo a 3 oa oucoO ^PoQ ft I' ? 0 to l c^rti rH ClO H w r0 OH HrH 0*fi r-HH O 00 PO.O Oto I rtHo O a P O1o3 oOrH oIO--lwOwOtOnnO P to to*o43 o o Soto oto otn to iwn 8to oo o txOH <* oo a ttnt* 0tj3i oo oo oo rH rH IIII I I I tI ill I I iH 02 to tn to II tI II CS CO u to p r0 \ctof 03 *v~; ooto 03 SW331830 STLCOPCB4078405 I-A (j) - 500 Stability of Grade P Hycar and Teflon in Aroclor 1254 at 130C and 45C Short Form Report No. 2179 File No. 141-27.1 December 29, 1947 Notebook references: Smith 45137 Grade P Hyoar and Teflon Immersed in Aroclor 1254 Material Temp. Hours $ Gain in 7t,, % Gain in Thickness Grade P Hycar Grade P Hycar Teflon Teflon 130C 45C 130C 45 *C 285 285 285 285 68.6 26.3 Negligible Negligible 26 6 Negligible Negligible re 1/14/48 OSIN STLCOPCB4078406 I-A-l - 500 From - ICemo P.G.B./R.L.J. 3/22/48 Aerovox Corporation New Bedford, Massachusetts Determining Fluorescence in Aroclar "The ultraviolet light we use for determining fluorescence in Aroclor is manufactured by George ?J. Gates and Company, Franklin Square, Long Island, New York. It is a CH 4, 100 Watt, G. E. Mazda Lamp with filter. .. "Our procedure is to pour a small amount of Aroclor into a 5" watch glass or a 5" Pyrex evaporating dish end observe for the degree of fluorescence under the CH 4 lamp, preferably in a dark room. If the sample has been contaminated with Mineral Oil it will show up as a streaky or milky fluorescence as compared to pure Aroclor. The fluorescence around the meniscus of pure Aroclor is not to be confused with the fluorescence resulting from contamination. "This test is qualitative and, as such, is based on the experi ence of the person performing it. We keep a standard sample for comparison. If there are any further questions please feel free to contact us". Copied by rs 4/2/48 DSW 331832 STLCOPCB4078407 T3 - ioo December 2, 1947 ELECTRICAL DATA ON AR0CL0R3 Introduction Time has not permitted ua to carry out electrical measurements on all of the Aroclor samples sent by your laboratory and as listed in your letter to Dr. C. K. Bump of June 27, 1947. It was believed that dielectric constant, loss factor, and direct current resistivity measurements over, a temperature range for a low chlorinated and highly chlorinated biphenyl; also one sample each of the terphenyl and the mixed biphenyl and terphenyl series would represent the electrical be havior of Aroclors. The trend of the electrical properties of the samples not measured can be estimated; i.e. as the viscosity of the Aroclors of a particu lar series increases, the loss factor will decrease and the loss factor maximum (if within the temperature range measured) will be shifted to higher temperatures. An increase in viscosity will increase the resis- . tivity of the Aroclor, The dielectric constant of a material is a measure of its polarizability. Therefore, any change in the structure . of the molecule which will increase its polarizability will cause an increase in dielectric constant. Accuracy of Data . The accuracy of the alternating current data is dependent on the dissipation factor of the dielectric at a particular frequency and a particular temperature. The dielectric constant values are accurate within .2$ provided the dissipation factor is less than 10$, The error is greater with increasing dissipation factor. The accuracy of loss factor (dielectric constant X dissipation factor) is also dependent on dissipation factor. Aroclor 5442 was the only sample which had a dis sipation faotor greater than 10$ and that occurred at the folloiving conditions: 41"0, 500 cycles 41C, 750 cycles 35C, 500 cycles It will be noted that the dielectric constants extrapolated to 100*C. oheck satisfactorily with the values listed in your letter to Dr. Bump. The direct current resistivity values have a 30$ error for the greatest resistance readings on our instrument. For lower resistance values the error decreases. Aroclors 1221, 1254 showed an increase in resistance with time which is indicative of polarization effects. For these materials then, resistance was read after the voltage was applied and then at the end of one minute - an empirical method used for taking a readable value. Aroclors 4465 and 5442 did not show noticeable pola- DSW 331833 STLCOPCB4078408 - 2 r IB - 100 December 2, 1947 rizetion effects^ even at the hi$i temperatures. Data The dielectric constant of Aroclor 1221 and 1254 is Independent of frequency. The dielectric constant of Aroclor 4465 and 5442 is also independent of frequency at the high temperatures. The liquid-like properties of 4465 and 5442 disappear at the lower temperatures where a dispersion region becomes evident. It will be noticed that the dielectric constant curves (at the lower tempera tures) have the same order as those of the corresponding loss factor , curves and the inflection regions occur at the loss factor maxima tem peratures P '. The loss factor curves of 5442 at the higher temperatures show a sharp up-swing, indicative of a large conductance component in the loss factor. Similarly, the loss factor curves of 1221 and 1254 seem to be in the conductance region. Aroclor 1221 showed an unusual sensitivity in changing loss factor values and as great an insensitivity to change in dielectric constant. It was found that a sample measured initially at room temperature and measured at successively increasing temperatures gave different loss factor values when conqpared to measurements made with the initial tem perature high and then successively lowered. Results showed that raising the temperature of the liquid or allowing the material to stand in the open for long periods always lowered the loss factor, probably volatilizing the more conducting or the hi$i loss substances in the Aroclor. Below 5000 cycles this effect was very noticeable, the diffe rences increasing with decreasing frequency. It may be mentioned here that loss factor measurements at low frequencies might possibly be used as an analytical tool or as a control method of indicating volatile sub stances contained in the Aroclor 1200 series. The log resistivity versus l/T graph is useful as an indication of the change that occurs in resistivity with temperature - or what is related, the change in viscosity with temperature. The actual slopes of 4465 and 5442 cannot be assured since there should have been more measurements made at high temperatures. However these two Aroelors have a much larger viscosity-temperature coefficient than the other two plots. It is hoped that the enclosed Taphs will summarize the dielectric properties of the Aroelors measured. More complete information or any questions concerning the data will be sent on request. aom/ . Copied by rs 1/15/48 R. Levreault Monsanto Chemical Company Plastics Division 3pringfield, Massachusetts DSW 331834 STLCOPCB4078409 V 8 DUNLAP ANNISTON DATA ON AROCLOR 1242 FkXX FOUND AFTER TALKING WITH YOU. RESISTIVITY 50 DEGREE C. 9200 X 109 100 DEGREE C. 2400 X 109 150 DEGREE C. 1800 X 109 AH ELLENBURG MONSANTO ST LOUIS DSW 331835 STLCOPCB4078410 KCUPPCL 4 CSSCn CO., H. Y. NO. 359*11 10 X lp to tlie H In c h , Stti H oc* accented* E n ffru v fn g 7 X 10 f:i. MADS m u . 5. A. . STLCOPCB4078411 .oo .0 0 3 4 .oo$%. .0 0 3 / ,oo3o .o o jto . .0 0 * 3 r > ooy ' i 6v l, STLCOPCB4078412 --- ----- J ----------*~1~:r -j--.---------- -........-f---*- - ..........rt~^i io jo : .. j :' t i : ; / Ujt m l -|U> 7o' STLCOPCB4078413 STLCOPCB4078414 II--B From - B.1.0.3. Final Report No. 895 Item Nos. 1, 7, 22, and 31 PaRes 12, 13, 14, 15, 16, & 17 III. CHLORINATED DIPHENYL. ' 3-* General. \ . Chlorinated diphenyl is manufactured by I.G. Farben under the trade name of Clophen. Some types are liquid and others solid at normal temperatures* They are used as impregnants as alternatives to hydrocarbon oils and waxes. Clophen shares with other chlorinated materials a high permittivity and has the same dangers in handling, due to noxious properties. In addition to the grades suited to capacitor impregnation, a grade known as T64 is made by I.G. Farben, suitable for trans former cooling. The total output of Clophen A50 and A60 for the years 1938 and 1943 was: - 1938 Type A50 21 tons A60 132 V? 1943 VI A50 170 vt n A60 506 t? The cost of the material in Germany is:- Type A50 llff, SOpfg. to HA. 60pfg. per Kilogram " T64 1H. 20pfg. per Kilogram. The following is a list of the principal prewar consumers of Clophen:- Siemens-Schuckert, Berlin. A.E.G. (Hydrawerk), Berlin. Klcafll (Brown Boveri), Zurich, Switzerland. Alsthoiii, Paris. Ducati, Milan, Italy. ; ' It was stated that no German capacitor manufacturer uses Clophen for the manufacture of small capacitors for radio and telephone purposes and whore these have been used by the Ger man fighting services they were supplied by the Italian fiiro, Ducati. 2. Manufacture. ' (1) The synthesis of diphenyl from benzene. Diphenyl is synthesised from benzene as shown in the figure, following DSW 331840 STLCOPCB4078415 SSSL --v/W'V----- * Condenser Distilling } 11 Column 500-650 0 200*C Two-stage Heat 'Exchanger Reaction Coil 800*C Synthesis of Diphenyl from Benzene The synthesis occurs in the vapour phase* at 800*C. and atmospheric pressure* in an electrically heated reaction coil of copper-manganese alloy* Ho catalyst is required. The apparatus, apart from the reaction coil* is of iron* and operates at the temperatures shorn above. About 10a of the benzene vapour is converted Into diphenyl in one passage through the reaction coil. The purity of the benzene is of importance for the elec trical quality of the ultimate chlorinated products and a specification is attached overleaf* The benzene used was believed to contain 0.2 to O.Z% of paraffins but little definite infomation could be obtained regarding any undesirable impurities or the mechanism by which they cause poor electrical performance. Thiophene was stated to be definitely harmful, and vague reference was made to "nitro-compounds"* to "aliphatic hydrocarbons" and to "substances which could not be chlorinated". The precise nature of these materials was not known* but their absence was ensured by obtaining benzene always from suppliers whose product was known to be satisfactory. Analytical Specification for Pure Benzene Appearance: Clear and colourless. Density at 20*C.t 0.876 Distilling range: First 5% within 0.25*C. 5% - 95a " 0.25*C. 95a - end " 0.25*U. Solidification point: Not less than 5*C. Bromine consumption: Sulphuric acid test: Hot more than 0.5 gm. bromine per 100 c.c. Hot more than 0.15 gm* HaCrg07 Carbon disulphide; Shall be free from CSg. DSW 331841 STLCOPCB4078416 Difficulty in the synthesis was still being experienced, due to rapid corrosion of the copper-manganese reaction coil, operating at 800*C. A small scale experimental apparatus using a fused silica coil had been made, hut had not been developed for production use# In addition to diphenyl, about 5$ each of 1-3 and 1-4 terphenyls are produced by the process. These are se parated, chlorinated and used in sealing varnishes; present production is about 4 tons per months No use is made of chlorterphenyls as paper impregnants, since the materials ar resinous and tend to crack; moreover the permittivities are lower than those of the ehlordiphenylso The crude diphenyl is next purified by distillation# During thi3 process the terphenyls remain in the residue. They are extracted in the following manners-- The residue is dissolved in hot benzene, filtered, and the 1-4 isomer obtained by fractional crystallization,, . The crude product is distilled in vacue, yielding 1-4 terphenyl with malting point of 208*C0 The 1-3 isomer, , remaining in solution in benzene, is more difficult to isolate. The solution is clarified with activated char coal, filtered, and the benzene evaporated# The residue ! is distilled to yield 1-3 terphenyl with melting point 80-84*0. (2) Chlorination of diphenyl. For the chlorination of diphenyl a lead lined vessel of 10,000 litres capacity is used. It is charged with 6000 kg. of diphenyl and 15 kg. of ferric chloride. The mix ture is heated to 110C., agitated and chlorine passed in. The addition of chlorine is continued for 100 hours at a rate of 130-135 kg/hour during which time the tem perature is raised gradually from 110*C,, to 130*0. The end point of the chlorination is determined by measuring the density of the product. To remove hydrogen chloride formed in the process, dry air is blown through the liquid for 2 hours and this hy drogen chloride is recovered. The product is transferred to another vessel and treated with 1/2$ of solid sodium hydroxide, heated and agitated. The sodium hydroxide is allowed to settle out and the Clophen drawn off from the top, transferred to another vessel to which Fullerfs earth and soda are added and the liquid redistilled. The stills for this process are gas heated. DSW 331842 STLCOPCB4078417 3. Proport le So (1) Capacitor impregnating grades, - A summary of the physical and chemical pro-pertles of the capacitor impregnating grades of Clophen Is given in Appendix n. There are six grades of capacitor Irapreg- nant, A30, A40, etc. up to A80, the 3, 4, 5, etc. indi eating the number of chlorine radicals combined with the dlp&enyl. Each grade contains a proportion of the adja cent homologues not exceeding 20$. Grade .450 has the highest VBlue of permittivity. Theoretically the highest value obtainable with a chlorinated diphenyl Is 9.0, and a grade having a permittivity of 7.0 has been prepared, but is chemically unstable, and very sensitive to moisture and impurities. The most commonly used grades are A50 and A60; A50 is the most stable grade and has the lowest dielec tric loss. Grade A60 is considered by I0G. to possess the . optimum combination of non-inflammability, stability and viscosity. As with Nibrea, it is considered that no addi tives are required since the substances are stable in use, provided that the capacitors are efficiently sealed against the air. Kicafil of Zurich ere the only users of A30 and A40. The following table shows the variation in capacitance and power factor with temperature for a Clophen iapregnated paper capacitor. The impregnant is A50, the dieleotrie is Schoeller and Hbescb "A" finish rag tissue (density 1.2 - 1.25) with a thickness of 10 uj frequency of measurement is 800 c/s. Power factor shows a maximum value of 0.052 at about: +4*C, while capacitance falls off by some 20$ at temperatures below this critical value. Variation in capacitance and power-factor with temperature for a Clophea-impregnated capacitor. Temperature (*c.) -60 --40 -20 0 +4 +20 +40 +60 +80 Relative Capacitance 0.87 0.91 ' 0.94 . 1.02 1.06 1.10 1.10 . 1.10 1.11 Power Factor 0.035 0,024 0.013 0.048 0.052 0.006 0.005 0.004 0.005 Ho evidence was obtained from I.G. on the use of any type of additive with a view to depressing the temperature at which the change of state occurs. . DSW 331843 STLCOPCB4078418 The method adopted for evaluating the water content in oils such as Clophen is described in Appendix III* It is also applicable to such solids as Nibren, ' Engelhardt stated that no source of failure had been ex perienced during the viiole period of production of Clo phen, which is about 17 years. Consequently no improve ments or modifications had been made or found necessary . during this period. (2) Transformer-cooling grade (Clophen T64). No detailed information was sought on this material, since it is unsuitable as a capacitor impregnant and is only used as a coolant for transformers and phase shifters,. A summary of its physical and chemical properties is given in Appendix 17. It has a low viscosity, is moderately stable under electrical stresses and has the distinct ad vantage over mineral oils of being non-inflammable. t The principal users of this product are A,EG. and Siemens, but it is understood that, as with other chlorinated eompounds, conservatism and prejudice among customers have prevented its wider use. No stabilisers are added to the material as their function of absorbing hydrochloric acid would be defeated by the * formation of "chloride salts", which in turn become elec trolysed. It was said to be very important to avoid contamimtion of Clophen T64 which may occur in transit and for this reason the use of leather for gaskets must be avoided. do Methods of use, precautions, etc. No details were obtained on the method of impregnation used by I.G. for the construction of test-specimens of Clo-. phan-Impregnated capacitor. This was partly caused by the non appearance, after the first day, of Engelhardt, but it is not considered likely that any novel processes are involved. For information on the precautions necessary in the use of Clophen, see Section II, 5, above. rs 11/19/47 DSW 331844 STLCOPCB4078419 ' III-A-b - 500 ^om - B.I.O.S. Final Report No. 8S5` Item Nos. 1, 7, 22 and 51 Page xiv Clophen ia made in several erodes, which correspond closely with their U.S, counterparts, A.50 being the grade most commonly used for capacitors, . Except for very rare use by Siemens and Hialske for special orders, Clophen has not been used in Germany for amall capacitors of the tele communication type, but it has been used extensively by Sienens-^ohuckert for power capacitors. It Is interesting to note that the German forces used Clophen impregnated and filled tubular capacitors made by1 Ducati, of Milan, who obtained the impregnant from I.G, The prejudice against Clophon was, however, being gradually overcome and several manufacturers were contemplating an extended use of this material. Some of them con sidered It to ho equal to or possibly better than mineral oil for opera tion at power frequencies. rs 11/24/47 DSW 331845 STLCOPCB4078420 III-A-b-50 From - B.I.O.S. Final Report No, 893 Item Nos# 1, 7, 22, and 31 Pages 98, 99 (2) Clophen The only chlorinated impregnant used hy 3iemensSchuckert is Clophen, supplied by I.G. In power factor correction and high voltage applications it is consider ed practically ideal. The only type of Clophen used in bulk is A.50, pentachlordiphenyl, (corresponding to Aroclor 1254). _-2Ql and A.40lhave been tried and found unstable. A.60, A.70 and A,80 are too vlscoui^b'allOTrTSF'gOOd^Impregnation * and have lower permittivities. Although the viscosity of A.50 at room temperature is much greater than that of oil, the viscosity at impregnation temperature is sufficiently low to give no trouble in attaining thorou^i impregnation. A routine check on conductivity is made on each drum of 1 Clophen, and formerly if the conductivity were too high, the Clophen. was treated with powdered chalk to neutralise the free acid. As the result of continual pressure on I.G. over a period of years, the acid content had gra dually diminished, and it is now possible without chalk treatment to work to the same rejection limit of resis tivity as for oil, viz. 10^- ohm.cm, at 20*C. Drums of Clophen failing to pass the conductivity test are returned to I.G., unless urgently needed, A certain elasticity is permissible in view of the histandard set. Apart from conductivity, further acceptance cheeks are specific gravity (1.54-1,55) and permittivity (5.0 5.2). Permittivity is measured at 800 cycles and 20*C. on a Schering bridge at low voltage. The acceptance standards for Clophen A.50 are shown graphically in Appendix XXXIV. Clophen costs about 1 K. 60 pfg./kg- and is therefore much dearer than oil (30 pfg.Ag*). This extra expense is offset, however, by the use of a special design which reduces the amount of Clophen required. An ad vantage claimed for this impregnant is that is has a similar permittivity to paper (viz. 5), 2,, Other impregnants studied. As Clophen is considered nearly ideal, no serious attempts have been made to find superior materials or addi tives to improve its performance. This attitude is sup ported by service experience, in which no failures have been reported. It is realised, however, that on freezing discharges may occur in the contraction voids, which may result in decomposition of the Clophen and failure of the DSW 331846 STLCOPCB4078421 dielectric. Tests were performed (see Section 17, 2# (3)) to check whether this degradation does in fact occur, and no failure was noted. Nevertheless, I.G. supplied small samples resembling Clophen A.50 hut having a lower melting point so that this possible source of failure could be investigated. De pression of the temperature at which the dipoles become immobile should raise the maximum usable frequency and hence broaden the range of applications by introducing those tor audio-frequency furnaces. Two of these I.G,. samples, with references A. 1621' and A.162N, are, like Clophen, made from benzene, hut have a lower chlorine content because of the presence of an additional alkyl group (C^H^+l), and hence a lower density. Their advantage over Clophen A.50 is that the setting point (i.e. temperature of maximum dispersion and of capacitance diminution) is lowered from -8*C. to -17*C. The permit tivity, viscosity and non-inflammabillty resemble those of Clophen A.50. The viscosity/temperature curves of these two samples, K.7 mineral oil and Clophen A.50,, are compared in Appendix XXX7. ra 11/19/^7 DSW 331847 STLCOPCB4078422 III-B-2500 Dccomber 22, 1947 TO: FHOIPHATE DIVISION SALESMEN 3UBJ: Aroclor 5460 aa Used in Ethylcellulose Lacquer RE: Federation of Paint and Varnish Production Clubs Official Digest (October, 1947), Aroelors used as plasticizers and resins impart excellent qualities to ethylcellulose. Ethylcellulose is used in lacquers of various types, the ethylcellu lose acting as a long chain polymer to impart toughness and flexi bility and to increase the speed of drying. . Some of the principal uses for ethylcellulose lacquers are for the coating of high tension ignition cable; heat sealing lacquers for foil and paper where the slight discoloration which may develop in nitrocellulose lacquers on heat sealing is not permissible; linoleum lacquers where alkali resistance is essential; textile printing; printing inks, particularly in multicolor designs where hydrocarbon solvent does not soften or bleed into previously printed designs; aircraft lacquer for resistance to both heat and cold and to quick temperature changes; record lacquers, especially for home recorders; and in wood sealers where good sanding and flexibility are essential, A good pigmented ethylcellulose lacquer has been made, based on the following formula: Ingredients Ethylcellulose N-22 Aroclor 5460 TiOg Kenthylphenol Toluene Ethanol Parts (by vieight) 6.4 6.4 4.2 0.06 67.0 16.0 100.06 .rh Copied hy rs 2/2/48 Benignus STLCOPCB4078423 III-G-300 From - Memo G.Y. Frankle/P.G. Benignus March 11, 1948 Soil-Poison Concentrate As described below, these materials are formulated into a water emulsifiable soil-poison concentrate carrying almost 30 per cent by weight of active Ingredients. Aroelor 1242 Triohlorobenzene (Mixed isomers) Pentachlorophenol Isopropyl alcohol Toluene or Xylene Sterox SE* Santomerse 3 Paste 33.5 33.5 10.0 3.3 16.7 1.5 1.5 100.Of, * Other non-ionic type emulsifying agents such as Triton KE or Span and Tween can be used to replace the Sterox SE. Copied by rs 4/2/48 os-n M*9 STLCOPCB4078424 Chemical Abstracts P03SIBLE USB OF AR0CL0R3 Vol. 41 Page 6867 III-H-10 U.3.P. 2,425,978 to Anderson and Coalahan, (Hercules Powder Company). Foundry cores sprayed with 15 solution of chlorinated naphthalene In hydrocarbon solvent show greater scratch resis tance than untreated cores. Cl2 content remains from 40 - 80 Cls. Particularly good for use with A1 castings. rs 12/2/47 DSW 331850 STLCOPCB4078425 17-10 From - B.I.0.3. Final Report No. 895 Item Noe* 1, 7, 22 and 51 Pages - 10 and U Much lees trouble has been experienced with chlordiphenyl than with ohlornaphthalene, probably because the former, being liquid, in volves less physical Contact in disposal. {2) Prevention. *. Very thorough washing of all areas of the skin likely to be contaminated with solid, liquid, or fumas has always been the basic principle in prevention of skin troubles, and is still looked upcn as fundamental, 'Then fatty soaps ceased to be available, because of the di version of fats to food, it became essential to insist upon the use of barrier creams, of which the best was one named ''(JUMBO", made at Trommersdorf. This has now been replaced, for lack of supplies, by an alternative made by I.G., named "MITIGAL", which is considered inferior to ruimbo but satisfactory. , The Flssan firm put up a special powder named "sCH'.'EFEL-- HJLVFR" to act as a barrier, but this was found to be inefficient except to allay irritation on skin areas exposed to fumes only. For this purpose it still finds use at Leverkusen and at the Hydrawerke factory at 3erlin0 A special point is made of fume extraction,"and the minimum air speed away from the operator is 1 metre per second. To check the efficiency of the precautions, a thorough exami nation is made every 4 weeks of every worker coming into contact with chlorinated hydrocarbons, and since the enforcement of the precautions, no deaths or symptoms of internal injury have occurred. Since superfatted soaps have ceased to be available, a cleansing composition containing dichlor-methana has been devised. This is so powerful a detergent for chlorinated materials that barrier creams are considered unnecessary, but it is uncomfortably irritant to many skins. (3) Cure. '.hen severe attacks of chloracne and internal sickness were encountered, in the early years, when the properties of chlorinated materials were not well understood, extensive rest periods had to be prescribed, together with a generous diet, entire absence of further contamination, and long periods in the open. Since precautions have been taken to minimise the effects, only a few mild cases of chloracne have been met. These have been treated with a solution of acetic and salicylic acids in methylated spirits. DSW 331851 STLCOPCB4078426  2 (4) Gonelaalong and RecommendstIona, 1.(5. consider that neither toxicity nor skin affection need now be any deterrent to the use of chlorinated naphthalene,, and that chlordiphenyl is if anything less troublesome, . Certain people, notably those v?ith fair skin3, show distinct allergy, and are best diverted to other work not involving contact. Scrupulous cleanliness of the skin (including the face, neck, and arms) and of the clothing (especially undergarments) is essen tial and needs strict enforcement, -lashing with hot water and good , soap is sufficient, so long as the soap is superfatted,, since the skin becomes sensitive to irritation by alkali. Barrier cream should be used on those parts of the skin which come into contact with solid or liquid material, and the area of contact should be minimised by the uee of protective clothing and gloves where possible. Areas of the skin which are contacted by fumes only, and particularly those chafed by clothing (e.g. the neck adjacent to the edge of the clothing) need protection by a suitable soothing powder. .. "'here fums3 are generated, they should be drawn away from th ; operator at an air speed of at least 1 metre per second. It may be found essential to have two ducts, one at floor level and on overhead, with exhaust in two directions simultaneously. In cass the precautions are being evaded, or lest there should be soma idiosyncrasy, monthly medical inspection is desirable. 11/24/47 DSW 331852 STLCOPCB4078427 IV-B-100 From - The Journal of Industrial Hygiene and Toxicology Volume 20, Number 2 February, 1938 1-ORPHOLOGIChL CHANGES IN TIE,' LIVENS OF iL-vrs RESULTING FROM EXPOSURE TO CERTAIN CHLORINATED HYDROCARBONS * Chlorinated hydrocarbons, particularly chlorinated naphthalenes and chlorinated diphenyl, have been, used extensively in certain in dustries* Their use in the manufacture and preparation of many types of olectrlcal equipment is constantly increasing. Although it is known that some of these compounds cause acne, only recently has the possibility of more serious systemic effects been recognized. The present paper describes the pathological changes observed in rats that had been exposed to various chlorinated naphthalene com pounds and to chlorinated diphenyl. Compound G (chlorinated diphenyl) was administered to two groups of animals in low concentrations. An average concentration of 0.57 mgms. per cu. m. was employed 16 hours daily for 134 days in the first experiment. In the second 'expariment (employing an average air con centration of 0.93 mgms. per cu. n.) the animals were exposed 8 hours daily for 143 days. The present experiments demonstrate that chlorinated naphthalene compounds and chlorinated diphenyl are capable of producing marked liver damage in the white rat without demonstrable microscooic changes appearing in the other organs. Furthermore, the characteristics of the liver lesions resulting from comparable amounts of any given com pound are the same, regardless of the method of administration (inha lation, feeding, or subcutaneous injection). . Of the various chlorirated hydrocarbons tested, chlorinated di phenyl gave evidence of being the most toxic, when administered by inhalation in very low concentrations (average 0.57 to 0.93 ragms. per cu. ra.) liver cell changes were very pronounced after the first exposure period. The most striking change was the hyalinization of t the cell cytoplasm (see fig. 6, plate III). Such cellular alterations were essentially unchanged after a 2 month recovery period. In these animals small sublethal doses of carbon tetrachloride and alcohol uni formly produced extensive liver necrosis and was highly fatal to them (fira. 1 and 2, plate VII). Chlorinated diphenyl fed in small doses produced similar but more marked liver injury (see fig. 5, plate III). In large doses this compound was highly fatal. The liver changes in animals dying after short exposures were inconspicuous and consisted mainly of swelling of cells and active regeneration (see fig. 4, plate IH). However, animals removed from exposure before being futally DSW 331853 STLCOPCB4078428 2 poisoned, subsequently developed hyaline degeneration of liver cells similar to that produced by prolonged administration of small doses of this compound. Thus the results of the jr.esent study, as well as certain field studies that have been made (1) surest that the solution of the in dustrial hazard Involved is dependent largely on a reduction of the air concentration of these compounds to a level that will not produce liver damage. The present experiments indicate that lower air con centrations must be obtained in the case of the more highly chlori nated naphthalene compounds and chlorinated diphenyl than for tric'nlornaphthalenes if a safe environment for workmen is to be assured. Be cause of the pronounced toxic effect of small doses of carbon tetra chloride on the livers of animals already injured by exposure to . chlorinated naphthalenes and chlorinated diphenyl, its U3e as a sol vent for these compounds would appear to be very hazardous. rs 2/5/48 33A85A OS'N STLCOPCB4078429 Ito K January 27, 1949 Distribution: 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. __ 14, .This Copy For^-15. 16 ,17. 18 Research File R.L. Jenkins - C.B. Durgin J.L. Christian - R.S. Weatherly W.T. Durrett -F.P. LaBelle v H.F. Weaver C .A. Hochwalt E.P. Rucker Edgar E. Hardy J.F, Reeves J.F. Reeves A.M, Ellenburg R.R. Knight Paul Logue P.G. Benignus . ' V. \ Please Insert the attached data in your copy of Report No. 2215, "Aroclor Data Book", issued April 27, 1348 by R. R. Knight, Research Department, Phosphate Division, ~ AME:rs / A. M. Ellenburg STLCOPCB4078430 T~A~a-2G0 OI.'i; H.-sst.;. iy n&ge-scch Repac Go. - : Final Report on "Evaluation at Monsanto Materials as FlaotiU oizex,sr . Job No. 589. AROCLOR 1232 Calculated molecular weight: 223 Refractive index*: 1.620 at 20WC. Saponification equivalent*: none Crystallization point*: ~52e5>C. Boiling point*: 290-525C. at 760 m. Acidity*: O01 milligrams KOR/gm. ' Acidity after haat: none Color (Gardner Standard): 0 Color after heat: 0 Color after light: 11-12 Specific gravity*: 1.2625 at 25/25C. Water solubility: .0016ft. at 25C. Stability to hydrolysis*: essentially none Odors chloroeromatic Viscosity: 25Cc - 6,,4 centipoiss 0eC. - 65 centipoise -20C. -627 centipoiae Solubility: Soluble in: octyl alcohol6 acetone6 ethyl acetate9 benzene, Shellysolve 0. Shellysolve S, turpentine, castor oils. cotton seed oil. Partially soluble in: methanol8 ethanol, gly cerol, linseed oil. Insoluble- is.: glycol rs 8--20--48 STLCOPCB4078431 I-A-b-300 ( TABLE I DENSITY AND SPECIFIC VOLUME 0? AR0CLQR5 AROCLOR 1242 Temperature (c.) ' 49.9 102.2 150.3 201.7 254.0 298.2 Density (g./ml.) 1.3546 1.3051 1.2587 1.2080 1.1549 1.1071 Specific Volume . (ml./g.) 0.7382 0.7662 0.7945 0.8278 0.8659 0.9033 . Temperature (*C.) 25.1 49.9 103.3 150.1 201.7 254.0 298.2 AROCLOR124f Density (g./ml.) 1.4439 1.4192 1,3673 1,3210 1.2691 1.2148 1.1664 Specific Volume (ml./g.) 0.6926 0.7046 0.7314 0.7570 0.7880 0.8232 0.8573 [ I | AROCLOR 1254 . Temperature (c.) Density (g./ral.) Specific Volume (ml./g.) 25.1 1.5392 0.6497 49.9 1.5139 0.5605 102.9 1.4607 0.6846 150.1 1.4127 0.7079 201.8 1.3595 0.7356 205.5 1.3096 0,7636 298.2 1,2546 0.7971 ( oSVM 331857 STLCOPCB4078432 I-A-b-300 ( TABIE I Cont'd DENSITY AMD SPECIFIC VOLUME OF ARQCLORS ARCOLOR 1360 Temperature (c.) 49.2 102.8 150.2 201.9 251.0 298.3 Density (g./ml.) 1.5956 1.5424 1.4931 1.4386 1.3854 1.3322 Specific Volume (ml./g.) 0.6267 0.6483 0.6698 ' 0.6951 0.7218 0,7506 Copied by ra 1-20-49 D. Ward Central Research Department December 21, 1948 DS 33-1858 STLCOPCB4078433 x-^-g--iou vaa-Colty --ypYACT ' co; oj rr1,'. .v-'; or/airat:::; ;.raya :? r 5 R, B, Dov?t Rr 7-' v JIC. j .. ".rj> n .Pv.'<: ' A ' i .OcYA..v. Industrial .o :>. Chorni stry ' Volu 29i,..lC?C-2DP {1937} The following 3ata aro taken from tables in the article and should bo views! critically. Specific rest data aro out of line viitfc our Aroclor figures. . . ' TABUS 1 Arselor S-). Ht. Ua \./{y/C* Cent ipoi sos Vice. 3D4Cc Ti. at ,, 75 "Cc Viseesity Inc_az __ DaneLty lAACA 1348 1254: 0.S3 1,49 189 ?40 . 3,7 rv */* ' -1939 J. oiO 5.C.540 t OossraaAiqrs ''.:C .TO TV1 C *:_i at-a i. a the :Ajr:;::o in ?k:"3ih: was very gas a't the A:, Yoyo and Ay? X?A Y v : A A ci9 -V 1 highest ratio of increase h: ov;;;. ' for sn oil. ; 33la59 oS'N STLCOPCB4078434 I-A-g-400 VISCOSITY VARIATION OTiTJ^PSSOTS Pressure _P3l t t 14.2 500 1000 1500 2000 2500 3000 3500 4000 5000 .6000 7000 8000 9000 1GQQ0Q 12,000 14,000 16,000 18j000 20,000 22;000 24,000 26,000 28,000 50,000 52,000 30 cC 1248 1254 I--r Cf-Oi 129 ops -- 155 223 287 384 553 G33 1270 1950 I- -..w 2740 eps 3140 4020 5S70 8740 14500 23600 40500 ------ -* .<*** ---- .tE!. 1248 1254 8.7 eps -- 9.3 -- 10 -- 11 -- 12 13 15 17 19 . 21 24 30 39 52> 75 in 176 300 494 816 ' 1350 21S6 . 24 cps 25 ~~ 26 -- 29 33 40 48 59 73 92 117 19 e 345 642 1290 . 2580 Copied by ra 7-12-48 ( SW 331860 STLCOPCB4078435 I-A-g-400 (' TABI II orviscosity aroclors AROCLOR 1248 Temperature (C.) 24.80 25.10 25.41 49.9 99.4 150.2 200.4 251.8 297.7 Kinematic Viscosity (Centistokes) 151.0 144.7 140.2 18.27 3.04 1.257 0.777 0.533 0.412 Absolute Viscosity (Centipoises) 218.1 208.9 202.4 25.93 4.17 1.660 0.987 0.649 0.482 Temperature 24.80 25.41 49.9 50.1 98.7 150.6 200.4 250.3 251.8 297.6 AR0L0R-lg54 Kinematic Viscosity (Cent!stokes) 585x10 505x10 96.7 95.9 5.86 1.785 0.991 0.658 0.652 0.485 Ab solute Visc osity (Centipoises) 901x10 777x10 146 .4 144.9 8.59 2.521 1.349 0.863 0.853 0.608 Copied by rs 1-20-49 D. YJard Central Research Department . December 21, 1948 DSW 331861 STLCOPCB4078436 I-A-a-500 KON-PLAlit 3LS DA^L:5GTiyC_OHGAKXC COI'iPCGivDs F, 1.1 * Clark ~ G-sueral Electric Company Industrial and Engine grin-? Chemistry Yolc 293 693, (1937) " Cliara.ctorlet-lcs_ o_ Dielectric LiquiG 1 qir>|xreads Property Fontschior Pontaahlor Eexaehloro Porhachlor- diphenyl dipheayi diphenyl-' Tricolor Biphenyl Osid Ketoixe Methane Benzere Burn Point ' K.F. Sp. Gr,, ( C/15.5C) 1.51 {65} Viscosity, SOS, "G. 45 (98) Pour Point, Cc + 10 Rcfr. Index (258C.) 1,6580 Dielectric Strength;. Kv. 40 Dielectric Constant (25C,) 5.1 Arc formed Gasos E.E. Sludging ITono Free- Acid None Distillation Range, *C 350-1CC H.F. 1.59 (100) 5S0 (57.0) 0 1,6220 40 5,0 rc.E. Pons None O<0 ruy ^V'w-n-JtrUr\ (15 r.,;-:;) HJf. 1.43 (100) 54 (100) + 15 1,6370 40 . 8..0 N,,E. Hone None 250-.-300 (25 RK.} 1J.F-. 152 (100) M (100) a- 20 1.6370 40 4,3 N .E, SOma Nona 290-340 . (25 mm.) E.F. 1.46 (05) SO (37,0} 0-10 t" do 1.57C0 40 4.8 N J3. None Eonc 200-220 NJ, - Hon-flaicT.elile. N.E. - Non-szplo aiv. Aroelor -1354. ' ' Vi sco si by - HoiaehQal -_Centlpol son Temperature^ - C, 28 51 40 50 60 70 80 90 100 Viscosity - epa,, 6000 SCQO 700 180 70 33 26 19 17 Copied by 7-12-43 ( DSW 331862 STLCOPCB4078437 V. St. Louis ( Dr. R. L. Jenkins Mr. C. B. Durgin Anniston May 25, 1948 III-G-100 Messrs. Edgar E. EEi-ay - Anniston A.M. Eilenburg - Aimiston Paul Logue T.H. lYheelock Aroclor-- Silastic Facto Attached are two copies of the No. 5 series about, silastic Facts Recently Dow Coming submitted the following information to us: ''Silastic is swollen quite badly when subjected to most organic solvents such as toluene, benzene, etc. However, our laboratory has recently submitted a report concerning the effects of chlori nated diphenyl on Silastic. Silastic immersed in chlorinated diphenyl for seventy hours at 150*C. The change in the physical properties were noted and the figures indicated that Silastic is remarkably resistant to deteriorations from contact with the hot chlorinated diphenyl. The changes in the properties are similar to those produced by hot lubricating oils and can be summed up as follows: ` (1) Lowering of the hardness by about 30 points. (2) Improvement in the elasticity by several points;. (3) Practically no change in tensile strength. (4) An appreciable increase in the ultimate elongation." Western Felt Manufacturing Company at Chicago, Illinoisf quoted Silicone 180 in sheet form as follows: 828" sheet, 1/4" thick 20x20" sheet, 1/4" thick 24x24" sheet, 1/4" thick $11.25 63.50 89.50 Apparently the greatest drawback to the use of Silicone as a gesket material for hot Aroclors is the high price of the plastics. rh encs Copied by rs 9-24-48 ( Benignue DSW 331863 STLCOPCB4078438 * m-3~ioo HANDLING AKOCLORS - 4'v. - Gaskets - Aroclor and Pyr&nol , Letter F. B. Zienty to Ho M. Hitchens - 9-20-48 "At a recent meeting it was stated by Dr. Suita of General Electric that silicone rubber gaskets were found to hold Pyranol effectively under conditions where other gasket materials gave poor performance with respect to freedom from leaks." 3/UES DEVELOPMENT REPORT .. . P. G. Benignus - 2-18-48 Precision Die Casting Company, Cleveland, Ohio "Ball-bearing swing joints made by Chiksan Tool Company at Brea, California used on flexible connections with Aroclor installations. "G. E,, Glyptal # 2 Red is excellent for sealing fluid on application to threaded pipe." rs 9-34-48 I V ( DSNN 33^864 STLCOPCB4078439 X -A - *>-Zoo no- z, ( / STLCOPCB4078440 I-A-b- 30, Fib. I im* rfl|c<tir *os ' .i* i t o ?c*c *rp s:n ^ 3}/S<f6 ^&yf) STLCOPCB4078441 V STLCOPCB4078442 I DIRECTIONS FOR TEST NO. 14-02-48 { V. suBJEfrr: Evaporation fast of Liquid Aroolors METHOD: 6 Hours Heating at 100* 0. ASTM D6-39T - Modified Procedure /V.'--. . - , / '!' Weigh on a rough balance about 50 grains (+ *5 gm.) of the well mixed Aroolor into and accurately tared tin box, 55mm. dla. X 35 mm. deep (3 oz. Gill--8t$J.e ointment box, deep pattern) Fisher #1-520. Let stand until box and sample are at room temperature, then weigh accu rately. . - - :. . . - - - - . . : -- Place the box in a ventilated convection oven maintained at 100* o/ 1 for 6 hours. Remove* cool in desicoator to room temperature and , accurately rewelgh. From the loss in weight calculate the evaporation In per cent. Report to second decimal plaoe only. No'fc88 . 1. Be sure box is at room temperature whenever exact weight is taken. 2. The oven should not contain other samples which might Interfere with evaporation. ' 3. Because the evaporation loss Is sensitive to temperature, the air bath must be olosely maintained st 100* 0. ; FABicm ' ; 1-29-45 i ! i Copied by af U/l/51 - T:: -' ". ' . ; . '. ... - . DSW 331868 STLCOPCB4078443