Document YDXDOpbG8RVJnoMvO8NQ4md5K

REPORT NO. 2215 FINAL REPORT ON THIS REPORT AND THE INFORMATION CONTAINED HEREIN IS THE PROPERTY OF THE MONSANTO CHEMICAL COMPANY. AROOLOR DATA BOOK Job No. 171-451 File No. 141-27.1 RESEARCH DEPARTMENT - PHOSPHATE DIVISION Anniston, Alabama ****4************ Report Submitted - April 27, 1948 Chemists: A.M. Ellenburg R.R. Knight Prepared by: R.R. Knigit Eighteen copies were made of this report and distributed as follows: No. I. Research File No. 2. R.L.Jenkins - C.B. Durgin No. 3. R^R.Cole - R.S. Weatherly No. 4. ff.T.Durrett - F.P. La Be lie No. 5. HfF.Wearer No. 6. C.A. Hochwalt - No. 7. E.P.Rucker No. 8. Edgar E. Hardy No. 9. J.F. Reeve a No. 10. J.F. Reeves NO. 11. A.M.Ellenburg No. 12. R.R. Khlgit . Noi 13. Paul Logne No. 14. P.O. Benignus No. 15. ' No. 16. No. 17. No. 18. . This is copy No. /3 DSW 268990 STLCOPCB4054090 , RESEARCH DEPARTLSNT - HI03FHATE DI7l3IGfJ MONSANTO CHEMICAL COMPANY Anniston, Alabama AROCLOR DATA BOOK General Information on properties of Aroelors, Aroclor process data, uses of Aroelors, and physiological effects of Aroelors. FOREWORD As a means of presentlng tbe available data on Aroelors to the In terested personnel within the Monsanto organization, this looseleaf notebook Is being compiled. Most of the date has resulted from work carried out within our own organization. Literature references, however, will be cited In all cases throughout the compilation In order to allow nore detailed infor mation to be obtained by the user. . The following detailed outline is for facilitating the location of data in the book and to assist in properly inserting new data sheets. Each Aroclor is to be given u series number for location under the headings. This scheme at present is as follows: Aroclor 1221 Aroclor 1232 Aroclor 1242 -- Aroclor 1248 Aroclor 1254 Aroclor 1260 Aroclor 1262 -- Aroclor 1268 -- Aroclor 1270 -- . Aroclor 1271 Other Diphenyl Aroelors - ' Aroclor 4465 - $ Other jHigh Boiler Aroelors ' -- ' Aroclor 5442 -- Aroclor 5460 -- Aroclor 5465 Aroclor 5468 - 100 series 200 series 300 series 400 series 500 series ' 600 series 700 series 800 series 900 series 1000 series 1100 series 1500 series 2100 series 2400 Series 2500 series 2600 series 2700 series Aroclor 2565 " _ 3000 series Related Compounds - 4000 series DSW 268991 THIS REPORT AND THE INFORMATION CONTAINED HEREIN IS THE PROPERTY OF THE MONSANTO CHEMICAL COMPANY. STLCOPCB4054091 -2 - The page pertaining to the solubility of Aroclor 4465 in various solvents would be of this type "IAJ - 1500". In cases where the infor mation for all Aroelors 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, IAh - 100. I. GENERAL FR0PERTIE3 OF AROCLOR3 A. Physical Properties - (a) General Physical Constants * _ , 1. Formula and molecular weight 2. Specifications for lanufaoture (b) Density and Specific Gravity (o) Cubical Coefficients of Expansion . , (d) Vapor Pressure and Rate of Evaporation (e) Specific Jfeat and Heat Capacity - (f) Thermal Conductivity ' (g) Viscosity ^ ' {h) Refractive Index , , (i) Heats of Vaporization - Other Thermodynamic Properties (J) Solubilities (k) Flash and Flame Points (l) Miscellaneous B. Electrical Properties (a) Dieleotric Constants (b) Power Factors (c) Dielectric 3trength (d) Volume Resistivity (e) Dipole laments (f) Miscellaneous V OSNN268992 STLCOPCB4054092 . ' -3- II. METHDD3 OF MANUFACTCRE- A. Monsanto Process \ ' . 1. Raw Materials 2. Chlorination 3. Distillation 4. Storage and shipping B. German Process C. Other Processes III. OSES OF AR0CLCR3 A. Electrical Field *1. Transformers 2. Capacitors 3. Coating for 'lire 4. Other uses B. -Varnishes C. Plasticizers D. Hydraulic Fluid S. Fire Retardants F. Heating medium I 0. Miscellaneous H. . Suggestions for new Uses IV. PHYSIOLOGICAL EFFECTS . 1. Skin Tests 2. _ Systematic Tests ' . . . , PATENTS USING /iROCLORS DSW 268993 STLCOPCB4054093 THIS REPORT AND THE INFORMATION CONTAINED HEREIN IS THE PROPERTY OF THE MONSANTO CHEMICAL COMPANY. ' The hook Is subjeot to revision and changes as various data are located. Graphs and diagrams will he Inserted when possible and new graphs drawn as information is compiled. No indices of sections is planned at this time, hut 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 ledged . Address all correspondence to the group leader in charge of the research on Aroclors at Phosphate Division - Research Department, Anniston, Alabama. * R. R. Knight rs 12/2/47 A. H. Ellenburg DS\N 268994 STLCOPCB4054094 Q l> 4 STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON, ALABAMA Page No. PRODUCT: Aroclor 1221 GRADE: ____ Renular CODE NO.: i04QC2S-7S-fl3 Sfct'4-19" PROD. DEPT. NO.: ________________________ ____ SUPERSEDES: Mmg-PrtntatlTa APPROVED BY (Initial*) v.v.r.j f.a.9. is-ifiAA Control - Specification Consumer Specification t Crude Aroelor 11211 3p Or. at 65*0, Acidity, ms. Naon/ftn. Aroelor 1221: Color Acidity, mg* HaGR/pm. Op, Or. ct 65/15,5*0. Chlorine content Viscosity at 100*F. 1,150-1.160 ^0*5 40 'APHA aar, 0,01 mas. i.i45-i ass 20.5-21.5;: 38-41 303 NOTES: Copied by rs 4/8/46 DSW 268995 STLCOPCB4054095 STANDARD SPECIFICATION OF . Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON, ALABAMA PRODUCT: GRADE: Agoolor 1233 CODE NO.: 1040-330-75-09 Benila* __________ AUTHoffijjS^ 4* 1946 PROD. DEPT. NO- ' __________________ SUPERSEDES: ITmr-'rentattvo __ A ,{?, | 7(F,Rt| FA,8, APPROVED BY (Initial*) 12-17-46 12-1B-46 12-19-46 12-19-46 Control Specification Consumer Specification Crude Aroolor 1132: 3p. Or, at 65/155*C' Aeldity, uv* NaOn/cm* Aroelor 1282: Color Acidity, ro*. NcOH/jja. Ip. Or. at 65/15.5*0. Chlorine content ttacoaity at 100*7. * 1.240-1.245 <.0.5 . 50 APZLt T38X. r01 max. 1.235-1.240 31.5-33.5 46-49 3J3 NOTES: Copied by re 4/8/48 l . DSW 268996 STLCOPCB4054096 STANDARD SPECIFICATION or MONSANTO CHEMICAL COMPANY Product: Chlorinated Diphenyl, distilled Code No 1040-40-75-09 Grade: Aroclor 1242 * Date Authorized June 21, 1940 Supersedes Specification Dated Tuly 3, 1934 Tolerable Limits Typical Value Sp. Or. at 65/15.5C. Color, N.P.A. Aoidlty, Ugm NaOH/gn. Viscosity at 54.4*G. 1.538 to 1.348 0.5 Maximum .01 Maximum 47 to 50 Seconds 3aybolt Universal Approved by A. B. Qtfber ______ Chief Chemist Approved by Edw. A. 0*Neal, Jr. -- ~ ' {forks Manager Approved by Robert S, Neatherly " Sales Manager Authorized by T. N. Carothere ________ Chemical birector Copied by rs 4/8/48 DSW 268997 STLCOPCB4054097 STANDARD SPECIFICATION - OF MONSANTO CHEMICAL COMPANY Productt Chlorinated Diphenyl, distilled Code No. 1040-260-75-09 Grade: Arodor 1248 ________ ; Date Authorised June 21, 1940 . Supersedes Specification Dated July 5, 1934 Tolerable Limits Typical Value Sp. Gr. at 65/15.5*C. Color. N.P.A. Acidity, Hgm NaCE/gn Viscosity at 54.4C. 1.404 to 1.414 0.5 Maximum .01 Maximum i' 69 to 76 Seconds Saybolt Universal Aroclor 1262 Sp. Or. at 90/15.5*C. Color, N.P.A. Acidity, Hgm NaOH/gn. Viscosity at 98.9*C. . 1.572-1.583 1.0 Maximum .01 Maximum 88-100 SOS Code No. 1040-510-75-09 Approved by A. B. Gerber " Chief Chemisi Approved by Edw. A. 0*Heal, Jr. Works Manager Approved by Robert 3. Weatherly Sales Manager Authorized by J. N. Carathers . Chemical Director Copied by ra 4/8/48 DSW 268990 STLCOPCB4054098 STANDARD SPECIFICATION GT MONSANTO CHEMICAL COMPANY Product: Aroolor 1254 Grade: Dlelectrio 4 * Code No. 1040-280-75-09 Date Authorized 10/3/41 Supersedes: 6/21/40 Color, APHA Scale . Condition Specific Gravity at 65/15.5 C Acidity, Mgm. NaOH/{pu. Inorganic Chlorides, ppm. Saybolt Viscosity at 98.9*C, sec. Dielectric Constant at 100*C Resistivity at 100*C, ohm-cm. at 500 volts Refractive Index at 25#C Distilling Range, Observed, 10# Observed, 50# . Observed, 90# Pour Point . vTater, ppm. , Evaporation, 6 Hrs. at 100*C Corrosion Test-Change in weight Acidity after test Inorgan ioCJKlorides after test Condition after test Color r a?Eer test rs 5/11/48 . . 100 Max. Clear 1.495-1.505 .01 0.10 Max. 44.5-47.5 4.15-4.55 Above 500 I Kr 1.6370-1.6390 350-555*C 355-362C 362-375C 8 to 22 35 Max. 0.4# 0.0# 0.01 0.10 Max. Clear 150 Max. DSW 268999 STLCOPCB4054099 STANDARD SFBCinCATICW * OP MONSANTO CHEMICAL COMPANY 'i Product: Aroclor 1260_________________ . Code No. 1040-390-75-09 Grade: Dielectric Date Authorized 14/18/41 . Supersedes: 1/50/56 Color, AFHA scale Condition Specific Gravity at 90/15.5*C Acidity, Sign. NaOH/gm. Inorganic Chlorides, ppm. SayboIt Viscosity at 98.9*C, sec. Dielectric Constant at 100*C Resistivity at 100"C, oha-cin. at 500 volts Refractive Index at 25*C Distilling Range, Observed, 10# Observed, 50# Observed, 90# Pour Point Water, ppm. . Evaporation, 6 Hrs. at 100C Corrosion Test-Change in weight Acidity after test Inorganio Chlorides - after test Condition __ . after test Color a?ter test 100 Max. Clear 1.550-1.560 .01 0.10 Max. 75-80 5.6-3.8 Above 500 X 109 1.6455-1.6465 570-377#C 377-385*C 385-400*C 36-34 55 Max. 0.2 # o.b# 0.01 0.10 Uax. Clear 150 Uax. re 5/11/48 DSW 269000 STLCOPCB4054100 SPECIFICATIONS FOR SOLID DISTILLED AROCLORS PROOTCT APPEARANCE <- COLOR ACID no. Ife.NaOR/m COLOR 5% TOUJENE HELTHfO POINT TOTAL CHLORINE 1 1 1268 1269 1270 1271 Tthite to yellow oryatallioe powder ' './hits to grey or light yellow crystalline powder TThite crystalline powder Practically white light fluffy powder 135-160*C. 0.05 Max. 225-255*0. ' 205-300*0 - 00 AFHA Max. 80 AH9A Max. ' t. 304*C. Min. 69.5 70.5# Copied by rs 4/8/48 m l* i4 STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON, ALABAMA Page No PRODUCT: Aroolor 4468 (nemlarl CODE NO.:_jjfl40^30gS^ft3_________________ DATE GRADE: _______________________________________ AUTHORIZED: Qatow a, iqaa PROD. DEPT. NO.: ____ SUPERSEDES: Tune 3, 1944 ' n.L.J.1 HtF, ?L,| ?A.B APPROVED BY (Initials) *u2Q44 ___ift-gwu mw>-aa __________ ' Control Consumer Specification Specification Appearance s Color, R.P.A.* joftenin? Point \a3,r *N) Acid lAuOber {UgkiQn/&u) Crystallinity clear, yellow, brittle resin 2*0 nax SO - 66C, 0 - .035 \ No, spec. * Raising oolor limit to 2,0 maximum is recommended because inspection reoords show that all lota produced in 1944 hare hud a color of 1S, NOTES: Copied by rs 4/8/48 " DSW 269002 STLCOPCB4054102 STANDARD SPECIFICATION . <F MONSANTO CHEMICAL COMPANY Product: Chlorinated High Boiler Code No. 1040-400-75-09 Grade: Aroolor 5460 Date Authorized May 10, 1940 Supersedes Specification Dated December 25, 1938 % ' Tolerable Limits Typical Value Appearance Color, N.P.A. Crystallinity Test Softening Point, ASTM . Acid Number Mgm NaOH/gn. . Chlorine Clear, light yellow, brittle resin 2.0 maximum To pass test 100 - 105.5*C. 0 - .05 59.0-80.6 t Approved by A. B, Gerber Chief Chemist Approved by Bdw. A. O'Neal^ Jr. 'Jorks Manager Approved by Robert S. Weatherly, 5/6/40 ' " Sales Manager Authorized by J. N. Carothers, 5A0/40 Chemical Director Copied by rs 4/8/48 DSW 269003 STLCOPCB4054103 Monsanto Chemical Company Anniston, Alabama Aroclor Test Methods and Designations Specific Gravity of Aroclors Total Chlorine in Aroclors Softening Point of Solid Aroclors Determination of Iron in Aroclor Plash and Flame Points Viscosity of Liquid Aroclors Distillation Range of Aroclors Evaporation Test of Liquid Aroclors Refractive Index of Liquid Aroclors Resistivity of Liquid Aroclors Dielectric Constant of Liquid Afrodors Acid Number of Liquid Aroclor Color of Aroelor - NPA scale Color of Aroelor - AlHA Scale Add 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 269004 STLCOPCB4054104 Ltonaanto Chendoal Company Anniston Method No. 14-10-48 Specific Gravity of Aroolors The temperature at which the Gravities of liquid Aroclors are taken varies with the viscosity of the liquid. Note the temperature at which the gravity is to be taken for the Aroclor under test and heat the sample to 10*C. 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 thermometer 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, then reed 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. DSW 269005 STLCOPCB4054105 t .. . t Monsanto Chemical Company Anniston Method Ho. 14-13-48 3JBJSCT: Total Chlorine In Arodors IE1H0D: Volhard Titration following Peroxide Fusion Chlorine in Aroolors may be determined by fusion of the sample with sodium peroxide in a Burgess-Parr fusion cup, extractinn the fusion with water, acidifying the water extract with nitric acid, and pre cipitating the ohlorlne 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 l-s/16" round hole in a 1/8" transite 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 Keker burner for two minutes. - The bomb, gaskets, and the sodium peroxide are obtained from the Parr Instrument Company, Uollne, Illinois. Charge for Fusion The fusion mixture is made up of about 15 grams (one metal scoop) of sodium peroxide and 0-3 grams of finely powdered cane, sugar. The reagents should be free from chlorine, or a blank run and corrected accordingly. The fusion mixture is well nixed by placing the ingre dients 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. 'Hhese are prepared by heating the Aroelor until a con sistency is reached as will permit dropping it from a glass stirring, rod onto a tinned surface (a can top), each drop forming a pellet. ,/hen cool these pellets can be removed from the surface by inserting a spatula under them. .4 grams are used. The pellets are brushed into the bottom of the fusion cup and the fusion mixture placed on top of them. After tlgitening the lid, the charge is ready for fusion. The orystallihe type Aroclora are weighed in the povklered form. a4 grama being used. They are charged in the same manner as the non-- crystalline type* DSW 269006 STLCOPCB4054106 . Total Chlorine in Aroclora -2 - LI'TJID AR0CL0R3: *20 to .50 grants are weighed by dro ning from a stirring rod onto a piece of thin heraispherically shaped glass, or 1/2 .gelatin oapsul (Gelatin Capsules No. 00, United Drug Company, Boston - 3t. Louis), which has been just previously tared, and which remains on the balance. It 1b necessary to heat the more viscous Aroclors to "dropping" consistency. The piece of glass then easily slides off the b&lanoe pan into the fusion oup. Cover with the fusion mixture.. The following quantities of staple, sugar, and AgN03 are used for the respective chlorine contents: Cl Content height of Sample Amount Sugar AgNOs 0/ - 30/ 30/ - 45/ 45/ - 58$ 58/0 - 66/ 66/ - 70/ Procedure 0.3 grams 0.3 grama 0.3 grams ' 0.3 grams 0.3 grams . 0.3 g. 0.3 g. 0.3 g. 0.3 g. 0.3 g. ` . , 50 ml, 50 ml 50 ml 75 ml 100 ml Place the fusion cup, which oontains the prepared sample and fusion mixture, in the transite ignition plate and .apply the fuil flame of the Maker burner to the bottom of the fusion cun 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. 'Then cool remove screw cop. Thorou^ily 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 the charre. Remove the cup and rinse well. '.Tien decomposition is complete, rinse off cover-glass and add pure HN0S, 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 poroelaln plate and wash beaker and filter 4 times with m1 1 portions of oold 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 269007 STLCOPCB4054107 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 AgN03 solution used. This will g|.vq 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 rrara of sample shows a KCNS titration of 10.4 ml. the percent of ohlcrine is: (614 * 104) X *003770 X 100 ^ 64.0955 C1 .3 ' . .. In case the fusion mixture or other reagents contain chlorine, the amount must be determined and deducted from the chlorine found. Solutions Required Standard AgNOa Solution: Dissolve 22 grans of silver nitrate in each liter of rater. Protect the solution from light. Standard KCNS Solution: Dissolve 10 '-rams of KCN3 in 1 liter of rater. Ferric Iron Indicator: Use a saturated solution of ferric ammonium aium, about 50 g. per 100 ml. of water. Rare Nitric Acid: Stock acid suffices provided it is colorless. It can be boiled in.a beaker until colorless if necessary using 600 ml. HNO3 and 300 ml. of HgO. Standardization of Solutions Teigh 0.3 and 0.15 gram portions of pure dry NaCl into separate 600 ml. beakere. Add 250 ml. of distilled water to each and 10 ml. of . pure 50 nitric acid. '.Then solution is complete, add 50 ml. of standard A0K>3 solution from pipet. Stir well and filter through 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^IOg 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 RaCl. DSW 269C08 STLCOPCB4054108 Total Chlorine in Aroclars -4- This value is checked by titrating 50 ml. of A$T03 solution added to 400 ml. of water and 10 ml. of pure 50j HN0S with KCNS solution. This titration should agree very closely ( 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 contains 60.66# Cl by theory, the value of the XDNS in terms of chlorine 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 KENS titrations of 13.11 and 13.13 ml. ` . Two 0.15 gram portions of NaCl show KENS titrations of 37.28 and 37.24 ml. The KENS equivalent to 50 ml. of AgNOg is then (37.28 37.24) - 13.12 or 61.4 ml. By titration of 50 ml. of AgNOg against KCNi 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 XCN5 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 KENS. 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 croperly seat the cover of the fusion cup. The fusion mixture must be kept away from rater or moist air, either of wl ich may Ignite the charge. The fusion' mixture should not be ground to reduce lumps. 2. The method as described is not applicable to volatile organle cam* 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 Aroclars and the snail amount of sarnie taken, great accuraoy 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 errors. - DSW 269009 STLCOPCB4054109 Total Chlorine in Aroclors -5- 2. Fusions which show black carbon deposites on the cover and side of tho fusion cup may or may not rive 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. The temperature at which the standard solutions are standardized should be noted. In case room temperatures vary from this tem perature, appropriate volume corrections should be made. 4. The fusion mixture materials should be essentially free of Chlorine. T e chlorine oontent may be determined by making a blank fusion, that is, without addition of sample, and titrating in the usual -?ay. Five ml. of AgN0s may be added instead of 50 ml. portions of AgN0s solution in like volumes of solution and nitric acid. References Beamish: Determination of Organic Halogens, Ind. Eng. Cham., Anal. Ed., 6 352 (1934). " FAB:cm 1-29-45 Copied by rs 4/20/48 / DSW 269010 STLCOPCB4054110 Monsanto Chemical Company Anniston I'othod No. 14-17-48 SUBJECT: softening Point of Solid Aroclors HETHOD: Ball and Ring ______________ This method is a modification of the A.S.T.Ii. standard method of test for softening point of bituminous materials, seria? designation: E 28-397. The method differs from the standard method in that the rings are larger than specified. A too ring support is also used in order that two tests may be made simultaneously. Apparatus The apparatus consists of the following: (a) Two tapered brass rinrs, 5/8" inside dia. at bottom, 11/16" inside diameter at top and 1/4" deep: thickness of wall 3/32". (b) Two steel balls, 3/8" diameter weighing 3.45 to 3.55 grams each, (c) A 800 ml. (Jriffin low form Weaker. (d) A ring support for the two rings having a brass plate exactly one inch be low the plate supporting the ring, (e) A 300*C. A.S.T.K. low distilla tion thermometer graduated 1*C. Preparation of the sample The sample shall be melted and stirred thoroughly, 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 shrink 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 Aroclor from dropping out of the ring. In the same way, the second ring is filled with a standard Aroelor 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 Aro&ar from ad hering to it. !tte Aroclor in the rings should be fully cooled and hardened before proceding with the test. - Procedure m* ' Add cool solution (employ water for softening point between 0-80*C, glycerin for between 80-200*0., mineral oil for above 200*C.) 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 Aroclor 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 the bottom of the rings and Just midway bo- tween the two rings. DSW 269011 STLCOPCB4054111 Softening Point of Solid Aroclcr a 2 Place beaker and apparatus on a 6 inch round hot plate and heat at such a rate that the temperature is raised 5C. each minute. The temperature recorded by the thermometer at the instant .the Aroelor touches the bottom piste is reported as the softening point. The heat ing is continued until hoth Aroclors have dropned to the bottom -late. Ho corrections are made for emergent stem. ' Notes . '* ` 1. 'Die standard Aroelor is run along with the sample under test in order to compensate for variations in rate of banting, dilution of glycerin, and thermometer variations. 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 5*C. per minute. 5. The glycerin may be used repoatedly for the tests after removal of the Aroelor. . 4. Benzol is used for cleaning the riags and balls. 5. hater can be used instead of glycerin for softening points up to 90*C. 6. For softening points above 100*C# well boiled glycerin should be used. The usual glycerin is not satisfactory above 125 to 130*C, ' it boils with loss of water while the temperature remains practi cally constant. It is well to have a supnly of high-boiling glycerin on hand to be used only for softening points above 100C. 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 tbe glycerin shall be uniform for each minute after the first 3 minutes of heating and not averaged over the period of the test. FAB:cm 1-31-45 Copied by rs 4/20/48 DSW 269012 STLCOPCB4054112 Monsanto Chemical Company Anniston Method No. 14-21-45 3CTBJBCT: Determination of Iron in Aroclore Iron in Aroolors may be determined by extracting a benzol solution of the Aroelor 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 grams 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. Draw 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 1-31-45 Copied by rs . 4/21/48 DSW 269013 STLCOPCB4054113 Monsanto Chemical Company Anniston Method No. 14-24-48 SUBJECT; flash and Flame Points METHOD: Cleveland Open Cup The flash and flame points of Aroolor shall be determined In the ^ Cleveland Open Cup Tester, following the procedure described In ASTM' v' 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 olate there shall be a plane depression 1/52" (.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 hole just fitting the cup. Heat may be Supplied 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 bust ioA or free flame allowed 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 Ko. 8. (r>ee A5TM 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 1/4 in. (.635 cm) from the bottom of the cup, and above a point half way between the center and back of the oup. 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 putslde of apparatus. The teat flame shall be approximately 5/32" (.597 cm) in diameter. The test flame shall be applied as the temperature read on the thermo meter reaches each successive 5*7 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 ehall, while passing aoross 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 cuo shall be approxi mately 1 second. DSW 269014 STLCOPCB4054114 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 100*F below the probable flash point of the oil. Thereafter the rate of heating shall be decreased and for at least the last 50*F before the flash point is reached the rate shall be not less than 9*F. or'more than 11*F per minute. The flash point shall be taken as the temperature read on the thermo 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 beating shall he continued at the specified rate of 9*F to 119F per minute* and application of the test flame shall be made at the specified intervals until the oil ignites arid con tinues to burn for a period of at least five seconds. The method of 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 flame 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 sufficiently so that the flash may be readily dls- cernible. . Note Aroclors 1248, 1254, 1260, and higher chlorinated Aroclors do not have a distinct flash or flame point below their boiling temperatures. FAB:cm 1-26-45 . Copied by rs 4/21/48 DSW 269015 STLCOPCB4054115 Monsanto Chemical Company Anniston Method No. 14-29-48 jUBJSCT: Viscosity of Liquid Aroclars llKfflDD: Saybolt Universal, A3TM D 88-44 Viscosity is a measure of resistance to flow. It Is measured by the time necessary for a chosen volume to be forced thru a tube of chosen length and internal diameter. By theory the viscosity of a fluid is related to the average distance between its molecules and to their average speed and their size. ' Apparatus Viscosimeter assembly with oil tube, bath, receiver, thermometers, strainer, timer, and pipet to meet all requirements of ASTM 0 68-38. The viscosimeter now in use is made by Krebs Elee. and Ufg. Co., New . York, purchased from Emil Seiner Co., their 2-tube capacity #862. One tube - on left hand - has been certified by the Bureau of standards. Procedure The vlsoosimeter is set up in accordance with manufacturers directions using No. 20 motor oil Tor the bath. The procedure and method of reporting results are those described under A5TM D 88-44. . . Care of Apparatus Bath: At conclusion of test, open the contact points until 1 or 2 Inches apart so as not to put undue strain on thermostatic control when bath cools. Put a few drops of oil in motor cups occasionally. Keep outside of bath wiped free of oil or Aroclor. Cover with hood when not in use. Maintain proper level of oil by occasional additions thru hole in front. '-Then oil blackens, dismantle, clean heaters, tubes, and Orifices, then refill with fresh oil. - Oil Tube: While still hot, remove all possible Aroclor from gallery with pipet. When cooled to 70-80*, fill tube and gallery with benzene, drop thru orifice into beaker, drain nailery with pipet, repeat with acetone, and wipe dry with absorbent paper in such a "ay that fibers cannot fall into tube. Repeat until clean. Occasionally cover the leather plunder with sized thin paper ("copy" DSW269016 STLCOPCB4054116 Viscosity of Liquid Aroclcrs - 2 - sheets) and swab walls of tube before using cleaning fluid. This keeps walls polished. Cover oil tubes with lids when not in use. Orifice: orifice. forceps. clean. Do not pass wires, strings, pipe cleaners, etc. thru the If a hair falls acrdds orifice, remove with long handle If the orifice becomes clogged, dismantle apparatus to Calibration Cheok the timer occasionally for 60 second periods. Check bath ther mometer from time to time. Check performance of viscosimeter periodi cally by running a reference sample of Aroclor on which careful deter minations have been made. Available for calibration is also an oil standard, called "Alpha 48", of the American Petroleum Institute. The oil is obtained from the Atlantic Refining Company, Philadelphia, Pennsylvania. Because such oil standards are subject to change they are Checked annually. FAB:era 1-31-45 Copied by rs 4/21/48 DSW 269017 STLCOPCB4054117 Monsanto Chemical Company Anniston Method No. 14-31-48 'XJBJECTt distillation Ran^e of Liquid Aroclors METHOD: A.3.T.M. D-20 with Modifications The apparatus, consisting of flask, condenser tube, shield, and ther mometer, Is exactly the same as described under A.S.T.M. test D-20 "Distillation of Bituminous Materials suitable for Hoad Treatment". Attach a 6 Inch auxiliary thermometer (0 - lSO^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, barometrio pressure and thermometer error. The procedure Is changed only to the extent that thermometer readings are taken when specified percentages (usually 10, 50, and 902) of Aroclor have been distilled instead of following the A.3.T.K. proce dure of weighing the distillate between specified thermometer readings. In testing liquid Aroclors, 100 <pns. 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 ,'eigh out 100 grams of sample into the distilling flask. Assemble apparatus as described under A.3.T.H. D-20. Insert thermometer (A.3.T.M. high distilling 0 - 400*C.) thru oork in the neck of the flask so that the top of the bulb is level with the lowest point of juncture of the tubulature and neck of the flask. Apply heat to the flask supported on tiro sheets of 20 mesh wire gauze so that the first drop comes over in from 5 to 15 minutes. . Cptriuot distillation at rate of 50 to 70 drops per minute. Collect distillate in a 250 ml. beaker tared on a balance. Take temperature . readings at 12, 32. 52, 102, 202, 302, 402, 502, 60, 70f.t 802, 90, 932, 952, 962, 972,. and dry. Corrections for emergent stem and pressure are applied to the thermo meter readings if required. Take correction readings at first drop, 102, 502, 902, 611(1 dry. Report the temperatures to the nearest 1*C. Example: (Exposed stem in degrees) X (temperature difference in degrees) X 0.000158 - degrees stem correction T^. The exposed stem is read from the top of the oork. The temperature difference is the reading of the thermometer minus the temperature of the auxiliary thermometer. DSW 269018 STLCOPCB4054118 Distillation Range of Liquid Aroelors - 2 - 0.00012 Tj, Ah barometric correction Ifc T& " normal boiling point In degrees absolute; A p m change in pressure from 760 ran. Hg. The correction is added if barometer is below normal and subtracted if the barometer is above normal. (UacDougall - "Thermodynamics and Chemistry" pp. 113). Corrected Temperature * Observed temperature *1 ! tfe. ' TAB: cm 1-39-45 Copied by ra 4/22/48 ' ' DSW 269019 STLCOPCB4054119 Monsanto Chemical Company Anniston Method No. 14-32-48 3UBJ1CT: Evaporation,Test of Liquid Aroclors METHOD: 6 Houra Heating at 100C. ASTM D6-39T - Modified Procedure ./eigh on a rouftfi balance about 50 grams (7 5 gs.) of the well mixed Axoclor Into an accurately tared tin box, 55 nrn. dla. X 35 m. deep (3 oz. QiU-style ointment box, deep pattern), Fisher #-1-520. Let stand until box and sample are ot 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. 4 ' ' ' 3. Because the evaporation loss is sensitive to temperature, the air bath roust be closely maintained at 100*C. ' FAB:cm 1-29-45 Copied by rs 4/23/48 DSW 269020 STLCOPCB4054120 Monsanto Chemical Company Anniston Method No. 14-54-48 . \ JitiJiiCTi Refractive Index of Liquid Aroclora Ma'IHOD: Abbe Refractometer 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 hy the ratio of the sine of the incident angle to the sine of the angle of refraction. The denser the medium, the greater 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 some quantitative analy ses of mixtures. As applied to Aroclor testing refractive index pro vides a verification of composition and purity. Apparatus Abbe Refractometer with accessories, Bausch and Lomb, Cat. #2550, Serial No. 377. Calibrated to read directly in terms of refraotive index of the D line (sodium) at a temperature of 20*C. Procedure Operators should be familiar with the Bausch and Lomb "Directions far 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. e Screw thermometer into its socket in water jaoket 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 0,2*C. for at least 5 minutes at 25*C. The Aroclors flow more easily at 25"C., hence the choice of this temperature. - With prisms illuminated, rotate the primus by means of the index arms until the border of the light and dark fields passes exactly thru the intersection of the cross hairs. If the border line is frinred with oolor, rotate the compensator until the color disappears. If the boun- DSW 269021 STLCOPCB4054121 Refractive Index of Liquid Aroclars - 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 ilace. If the temperature of the water jacket is other than 25*C., correct to 25* by use of the,correction factor, 0.00044 per *C. This factor is applicable only to Aroclors 1248, 1254, 1260, and 1262. It was found by careful measurement on each Aroclor thru the range 10* to 50*C. The correction is subtracted when the working temperature is below 25*C. and added when above 25*C. ' Example: If the refractive index is found to be 1.6422 at 15*C., the index corrected to 25*C. is 1.6422 - (10 X .00044) - 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 softdoth. 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. '.Then not in use, the refractometer should be kept in its closed case. For practice or for checking erformance, distilled itater is useful. Tatar has a refractive index of 1.3330 at 20*C., 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 25*C. have given the following typical values for Aroclors. Aroclor 1248 Aroolor 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 ss they -- ^.f. oorrect -- 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 qS'JM 269022 STLCOPCB4054122 Monsanto Chemical Company Anniston Method No. 14-35-48 GCBJECT: Resistivity of Liquid Arodors METHOD; Resistance Measurements between Conductors Apparatus Megohm Bridge: General Radio Company Type 544B, AC operated - 500 volts, serial No, 171, This is a direct-current Theatatone 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-positlon 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. Ibe 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 oonstapt supplied by General Electric Company is used. For the electrodes now in use, the cell constant was given as 815. . Glass Plate: Pyrex, 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 por celain tubes for lead vires. Holes must avoid oven heating elements which occupy 2" paths vertically and horizontally intersecting at the center of the oircular wall. / Lead 7ires: Provide 300 ohm Amphenol twin conductor cable to connect tlie electrodes in oven to the posts of the bridge. Hie nortions exposed to oven temperature are hared and then covered with oorcelain heads. Provide also a flexible lead to ground the bridge to a water pipe. Clean the leads, beads, and porcelain tubes oeriodlcally. Assembly of Test Cell The grooved glass piate ia placed in an 800 cc. beaker* The clean elec trodes are plaoed in the grooves of the glass olate with the connector posts directly opposite in order to give the widest possible spacing to reduce surface conductivity. The cylinders should be very clone to equidistant. The apparatus should be dried for 2 hours at 100*C. before use. . Heat the sample to be tested to about 110*C. on a hot plate and pour . into the eleotrode assembly until the level of the liquid is 1/4 to 1/2" above the eleotrodes. Care must be used to make aire that the ' DSW 269023 STLCOPCB4054123 SUBJECT; Resistivity of Liquid Aroclars - Page 2 METHOD: Resistance Measurements between Conductors lip of the container, froni which the liquid is poured, is clean. Tilt the beaker in such manner that all air bubbles in the Aroclor will rise to the surface. Air cool to 103-104*C. then without removing thermometer, transfer to the oven which is maintained at 100C. and connect the electrodes to the two flexible wires which lead to the megohm bridge. `Then the Aroclor comes to temperature (100C.), remove thermometer, check cen tering of electrodes, and procede to measurements. Measurement with Megohm Bridge ', Connect the two lead wires to the megohm bridge with the lead from the outer electrode-to the LOU unknown post of the bridge; the inner elec trode to the unknown post. Connect the "ROUND post on the left side to a water pipe. Diving the spring connector, pivoted on the "C" post, to the LOU post. Connect the attachment cord to the 110 Y power supply. . 7ith the Aroclor at 10CC., turn the control knob (CIIECK-OPUIL'iTE-OirJlGE) to the CHCCK position. Throw all 3 switches at the rear of the Panel to ON. After 2 minutes bring the galvanometer pointer to zero by means of the ZERO ADJUST knob. Then turn the control knob to CILVRGE for one minute. Turn the knob tc OPERATE and return the galvanometer pointer to zero by adjustment of the MULTIPLY 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 5.4 X 815 - 4.4 X 10$ meg. ohm cm - 440 X 109 ohm cm - Values for resistivity are qualified by designation of temperature and voltage. These are 100*C. and 500 volts for the test above. Like con ditions are used at Plant B. . 0S\N 269024 STLCOPCB4054124 SUBJECT: Resistivity of Liquid Aroclors - Pace 3 tUTHOD; Resistance rieasurements between Conductors Caro of Apparatus The "Operating In struct Iona", General Radio 'Form 458-3, which accompany the megohm bridge, recite details of installation, measurements, uses, and construction, illustrated by figures and circuit and firing diagramsNo attempt is made to reproduce such information here. The operator should acquaint himself with 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 and stored in cabinet. Cleaning Electrodes - After the measurements are made the electrodes are removed from the tested liquid, end allowed to drain until the liquid stops running from the electrodes. '.Thile still hot they are placed in a beaker filled with benzene under a well venileted hood and allowed to cool. Then cools the electrodes are removed from the benzene and scrubbed with powdered tri sodium phosphate end a benzene carbontetrachloride mixture (50-50 by volume). This scrubbing can be done with either a brush or the hands. The eleotrodes are then rinsed with acetone, followed by tap water and then distilled water. The eleotrodes should not he touched by the hands after the acetone wash. After final rinsing the electrodes are placed in an oven at 120*C. for one hour or until they are used again. The glass spacer plates are cleaned and handled in the same manner as the electrodes except that they are wrapped in lense paper before being placed 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 kept on hand for periodic or emergency verification Of the meter itself. rs 8/3/48 0s* tf#*6 STLCOPCB4054125 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 Variable Air Condenser 1500 cc. Pyrex Beaker General Radio Co., Type 716-AM General Radio Co., Type 707-A General Radio Co., Type 606-A Cenco-DeKhotinsky #95050 General Radio Co., Type 334-F Procedure Electrode and beaker must be cleaned as directed under "Cleaning Appa ratus for Dielectric Constant", and be at 100*C. Heat Aroclor in the can to 105*C. Pour over electrode until plates and ceramic insulation are covered. Connect leads. Stir with thermometer outside oven until temperature reaches 101*; place in oven which has been carefully adjusted to 100*C. At the time sample is placed in oven its temperature ebould not have fallen below 90*C. Connect leads to capacitance bridge, observing that the lead from insu lated side of condenser goes to insulated terminal on bridge. Balance 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 100*C., maintain bridge balance until no pronounced shift is evident. Record reading, of capacitance scale multiplied by multiplier setting. Dielectric Constant. Capacitance in Aroclor at 100*C. Capacitance in air at 100*C. Balancing Capacitance Bridge Condensed procedure. Operator should read operating instruction for NUll Detector for complete details. 1. Connect to power supply leads to osolllator 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 269026 STLCOPCB4054126 i Pago #2 . /. Dielectric Constant of Liquid Aroclor - Test 14-36-48 3,, On null detector turn brilliance knob to extreme left, the focus knob to extreme right, gain control to extreme left, sweep amplitude at raid-scale position, the sweep frequency switch on line side. 4. Turn on power switch, lighting pilot light. 5. "'ait fifteen seconds, turn brilliance knob to extreme right. 6. Adjust focus and brilliance knobs until sharp fine line. 7. Connect external terminals on deteotor to output terminals on oscillator. Switch sweep frequency to external side. 8. Connect detector terminals of bridge to imut 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 pain control at mid-scale and selectivity to extreme left. Turn sweep amplitude to extreme left, obtaining vertical line. :7ith 10. With turning control knob obtain the maximum length of this line, keeping it always under l/4 inch with gain knob. 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 v-han the gain control is at extreme right. 14. Set sweep amplitude beyond mid-point, and slightly`displace the power-faotor dial to obtain a tilted ellpse. 15. Adjust phase control until this ellipse closes into a straight line Inclined to the horizontal. , .i 16. Bring power-faotor 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 line to open up when it is swung 30 degrees from horizontal in both directions. 17. Throughout these adjustments the other bridge control (the DSW 269027 STLCOPCB4054127 Paf;e #3 Dielectric Constant of Liculd Aroclor - Test lrf-36-*8 capacitance Dial) must be in balance position. If the ellipse grad ually opens when the line is horizontal it nay be brou-iit back to the line again by making slight changes in this control. If confusion results, balance both controls again as in (13) and repeat the suc ceeding adjustments, , This is the position of bridge balance: An alteration of the power-factor oostrol 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 in 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 and adjust brilliance to obtain a fine vertical line on screen. 4, Brinr 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 extrema right. 5, This dot remaining unchanged shows condition of bridge balance. Cleaning Apparatus for Dielectric Constant The oondenser 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 allowed 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. sorb 3/1/48 DSW 269028 STLCOPCB4054128 Monsanto Chemical Company Anniston Method Mo. 14-42-48 SUBJECT: Acid Humber of Liquid Aroclors METHOD: Titration with Alkali using Phenol Red 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 haying acid characteristics. It corresponds to the Neu tralization Number of ASTU 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 NaGH 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 Aroolor 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 llgn. NaCE. Calculate in terms of Hga. NaCH per gn. of sample. Report to 4 decimal places. 0. Hga. NaOH/gm. . g. of sample Example: If titration is 0.08 ml. for 50 g. of Aroclor, the Acid Number is 0.08 X 0.4/50 0.00064 I%n. NaOH/gm. Report as 0.0006. Solutions Required 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 gn. of dry indicator in a small bealcer add exactly 2.0 ml. of 0.1409 N NaOH. Stir to dissolve and dilute with 3-A alcohol to 50 ml. Reference Buffer pH 7.6: Dissolve 0.41 g. ffenaP04 and 0.59 gm. NaaHP04 (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 LaMotte pH 7.6 color standard is not available. DSW 269029 STLCOPCB4054129 Acid Number of Liquid Aroclars - 2 - Standard 0.01 N NaQH: 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. aoetone in solvent instead of 200 ml. a 100 gm. sample of 1254 may be taken for analysis. FAB:am 1-30-45 Copied by rs 4/23/48, DSW 269030 w& w STLCOPCB4054130 Monsanto Chemical Company Anniston Method No. 14-43-48 SUBJECT: Color of Aroclor on N.P.A. icale LTZTIIQD: Helllge Pocket Comparator Scope The method is applicable to Aroclors 4465 , 5460, or others haring 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 Helliga Pocket Comparator, Model 605, xrtth 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. ASTK color numbers coincide with National Petroleum Association color number (1915). The relation of the N.P.A. color numbers to other color scales is tabulated below: NPA Color NOS. (1915) NPA Names Union Petro leum Co. A8TM Color Nos. Lovlbond Analysis Red Yellow Blue 200 510 1180 1/4 1/2 3/4 1 1-1/2 2 2-1/2 3 3 -3/2 4 4-1/2 5 6 7 8 - - *. Lily white Cream white Extra pale Extra lemon pale Lemon pelt) Extra orange - Orange pale * Pele Light Red Dark Red Claret Red mm ' -- G H 1 J K L II 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 mm mm .55 .55 .55 1.80 - FAB:cm 1-26-45 Copied by rs 4/27/48 OSVJ2690^ STLCOPCB4054131 Monsanto Chemical Company ' Anniston Method No. 14-44--48 3PBJECT: Color of "Hater Thite" Aroclora METHOD: Comparison against A.P.S.A. Ocala Scope . The method Is applicable to Aroclors 1254, 1260, or others having color less than N.P.A. #1 ("V/ater V.Tiifce"). A.P.H.A. Standards These color standards are acid solutions of potassium chloroplatlnate and cobaltous chloride. The unit of color Is that produced by 1 mg. of platinum per liter. The ratio of oobalt 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 chloroplatlnate (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, 3 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 Hater 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 downward through the tubes upon a white or mirrored surface placed at such an angle that light la reflected upward through the column of liquid. A color tube support (Fisher #7-065, 50 ml.) is convenient. Inaanuoh as the proportions of the standard color solution in the compari son tubes are such as to represent an aliquot part of a liter, the readings are dlreot as ports 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, 5), and thB color obtained to nearest 10 by multiplying by the dilution ratio. FAB:am 1-30-45 Copied by rs 4/27/40 ' DSW 269032 STLCOPCB4054132 Monsanto Chemical Company ' Anniston Method No. 14-46-46 ``STBJBCT: Acid Number of Tolld Aroclars and Heavy Llnuld Aroclors METHOD: Titration with Alkali using Phenolphthaleln Procedure Dissolve 50 grams of the Aroelor 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% phenolphthaleln solution, and titrate, In the case of the distilled Aroclars 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 NaOH, Acid No. - ml. titration X 0.4/sample weight For 50 gm. ~ Acid 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 Apparatua 10 ml. burette in .05 divisions. Conversions 1. To obtain Neutralization Number in terms of XOH, multiply the Acid Number in terms of NaOH by 1.402. Inverse factor is 0.713. 2. Multiply the Aoid Number by 1000 to obtain the parts of NaOH re quired to neutralize one million parts of Aroclar. Thus Acid Nujriber of 0.0006 is equivalent to 0.6 parts of NaOH per million parts of Aroelor. 3. The large amount of water used causes sharper separation of the aqueous layer from the non-aqueous layer, thereby making the endpoint more easily 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 email amounts, also consumes NaOH in neu tralization to phenolphthalein. It therefore follows that an Aroelor of very low acid number rust be also extremely lor; in ferric chloride. FAB:em 1-26-45 . Copied by rs - 4/27/48 DSW 269033 STLCOPCB4054133 Monsanto Chemical Company Anniston Method No. 14-47-48 SUBJECT: Pour Point of Liquid Aroclora LETTED: A.3.T.M. D-97-39 The pour point of an Aroclor i s the lowegt temperature at which the material will flow when it is chilled under certain prescribed condi tions listed in A3TM D 97-39. Apparatus Apparatus consists of test Jar, thermometer, cork, jacket, disk, gasket, and bath as described under A.3.T.M.-method D97-39. The thermometer is the A.3.T.M. Cloud and Pour Test, range -38 to 50C. Present apparatus is the Emil Greiner Co. #GR 2234 single unit with Gr2242 test Jar. Procedure for Aroclor Follow D97-39 in all respects except that the centigrade scale is sub stituted. Only on 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, '.'arm the Aroclor without stirring to 46C. irf a bath at 46-48C. Cool to 32*C. in air or water bath at 25*C. Trans fer the Jar to the jacket of the cooling bath which is maintained at 0 to 3*C. Beginning ut a temperature 8 to 10 degrees above the pour point, at each interval of 2*C., remove the test jar from the jacket and tilt just enough to detennine if there is movement of the Aroclor. This inspection should not require more than 3 seconds, '/hen movement is not promptly apparent, the test jar should be held 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*C. 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 whlcfT the liquid will flow or pour under the test conditions. Technicians must familiarize themselves with D97-39 which Hives complete details of apparatus and procedure, reproducibility of results, effects of thermal history, etc. 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 269034 Copied by rs - 4/2.7/48 STLCOPCB4054134 Monsanto Chemical Company Anniston Method No. 14-48-48 ^OBJECT: The Testing of Aroolors 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 in a Pyrex hottle. Caution: The water used in preparation -mist 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 crystals in 40 ml. of water and add 10 ml. of concentrated nitric acid. Chloride fl*ee distilled **ater. Apparatus Required LaMotte 10 ml. color tubes (13 mm. X 100 mm). 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 higi enough to allow 1/4" of test tube to extend through the holes in the top. The box should be painted a flat blaok on the inside and on top and should contain enough holes to accomodate at least seven 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 Tree water to a 250 ml. Erlenmeyer flask, heat to boiling, add 200 gram of the Aroclor to be tested, tdiich he3 been heated to 100*C, shake vigorously for 1 minute, cool in coollug pan. Carefully decant some of the water extract to a separatory funnel. Wash with pure ethyl ether (ohloride free). Transfer 10 ml. of the ether washed extract to a 10 ml. Lalbtte 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 DSW 269035 STLCOPCB4054135 The Testing of Aroclors for Inorganic Chlorides - 2 - volumetrio flask. One ml. then contains 2 micrograms of Cl. Transfer 1, 2, and 3 ml. portions to 10 ml. tubes, Eake to the 10 ml. mark with Cl free H20. 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 oompare in a specially prepared 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 the sunlight. Comparison is easier when other sources of ligit 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 ater extract estimating to the nearest whole microgram. The extract blank and the distilled mater should show no turbidity. Calculation Divide the chloride content in aicrograras of the known solution which mutches the extraot by the weight of the Aroclor represented by the extract to obtain the chloride content of the Aroclor in p.pjn. . In the procedure described, the 10 ml. extract represents 40 grams of Aroolor (1/5 of 200 g. taken). The three knowns contain 2, 4, and 6 mlcrograms of Cl, thus representing 0.05, 0.10, end 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 through very elicit contamination .or Inattention to details. All equip ment must be scrupulously cleansed, the distilled water absolutely chloride free and testing done away from fumes of HC1 or dhlorine fumes. rs 4/27/48 DSW 269036 STLCOPCB4054136 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 point* Fischer reagent is a solution of iodine, sulfur dioxide, and pyridine. Iodine is consumed as long as any water is uresent. Bie solution is again titrated to obtain the water content Introduced by the Aroclor. Solutions and Apparatus Earl Fischer Reagent: Welgi into a flask 264 grams of pyridine, Barrett 2-A or Eastman 214^1, 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. p* Transfer 65.6 grams of the pyridlne-SO mixture and 134 ml of absolute methanol to a 1 liter Florence flask. Cool thoroughly in an ice water bath. Add 16.9 grams of iodine, stopper, cool again before shaking. Alternately cool and swirl until the iodine is in solution. Makes 200 ml of reagent. Store in glass stoppered bottle. Let stand 24 hours before using. '.Then fresh, one ml of reagent is equivalent to about 0.0033 gms. of water. Aroclor Solvent: Mix 2 parts dry benzol with 1 part anhydrous methanol. The dry benzol is prepared by shaking the commercial grade with anhydrous calcium chloride, decanting into a flask and distilling, rejecting the first 10i' 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 haa been thoroughly dried by passing thru tubes containing 8 me& Drierite. Disengage the flask from the aspirating train and imme diately close with a paper cap held by a rubber band. DSW 269037 STLCOPCB4054137 I :/ater Content of Li quid Aroelors - 2 - without 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 Fischer reagent to distinct red-brown end point which does not fade after swirling several times. The Fischer reagent is dispensed from the microburet the tip 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 reaoted. 9uperimpose a fresh paper can immediately. __ Obtain weight of the solvent and well-covered flask on a Torsion balance or equivalent. Quickly introduce with a dry pipette about 100 srams of the sllgitly 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 slightly. If oloudiness persists another mixture should be prepared. Puncture a small hole in the paper cap for the insertion of the buret tip and titrate with Fischer reagent to the first definite brown color, agitating with a gentle swirling motion. The end point should persist through several swirls. The end point may slowly fade through slow aocess of atmospheric moisture in which case it is restored 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.m. Calibration of Flecher Reagent and Standard 'Veter Solution Standard water solution in methanol: Transfer exactly 0.40 ml. of water from a micro buret or a 1 ml. measuring plpet to a 100 ml. volumetric flask. Fill to the mark at once with anhydrous methanol and mix. One ml. of solution then contains 4000 microTama 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 {prams of water) to a 250 ml. Erlenmeyer flask which has been dried and swept with dry air. Close with paper cap and titrate with Fischer reagent in the same manner as the sample. The end T>oint 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 alvmys be subtracted from this titration. Divide the amount of water 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 micrograma of water, required 6.61 ml. of Fischer reagent while 5 ml. sw 269038 STLCOPCB4054138 !7ater Content of Liquid Aroelors - 3 - of the methanol retired 0.55 of Fischer reagent. 20,000/(6.61 - 0.55} 20,000/6.06 3300 raicrograms vjater/ral. Reoallbratlons: Because the Fischer rea-ent deteriorates rapidly, Its titer must he 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). The total water is the produot 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 3300 * 21813 raicrograms. If on recalibration 7.37 ml. of Fischer reagent is 21813/7.37 2960 micrograms 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 H^O 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 .4 by A - B factor grams of H20/ml. l&iltiply factor X B giving gras, of HgO 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 269039 STLCOPCB4054139 0 ` . From . PROPERTIES OF BASIC "HALOTIAX" PRODUCTS Letter to vr.C.TL/M.ToBolaer (Halowax Products Div,,yUnion Carbide and Carbon Corp,,, 30 E. Forty-Second St., N.Y. 17,, N.Y.). letter dated Feb. 27, 1948. : HiiTLHIAL HUMBER * i Ho. 1000 No. 1001 No. 1013 No. 1014 Colors Flow Point ("tod, ASTU Softening Point) deg. F. White to Pale Straw White to Pale Yellow! Pale Yellow Liquid 194-201 ' ! 247-252 . Pala Yellow E77-883 i S.dCific Gravity at 77 deg. F. 1.19 - 1.25 1.53-1.59 1.65-1.71 , 1.75-1.PI Penetration (Pod. ASTI!) 200-g. load at 77 dee. F 10-15 5-8 5-8 Videosity (Saybolt Universal Seconds) Didtillation Renee (ASTT) dee. F. . 33-37 at 77 dee. F. 33-37 at 266 dee. F. 31-35 at 266 deg.F. 33-37 at 302 deg.F/ 480-590 600-650 615^^55 Tfiash Point (ASTil Cleveland Open Cup) dee. F. 203 .284 356 392 Fire Point (AST!! Cleveland Onen Cup) dee. F. Pr/ner Factor at 1,000 cycles at 106 cycles 338 None to boiling None to boiling None to _ Less than 0.2*/ Less than 0.2f. boiling less than 0.8 0,43?! 0.70?! 0,70$ 1l' eiectrio Constant at 1,000 cycles at 10^ cycles ---------------------------- --' 5-6 5-6 Over 107 - 108 4-5 4-5 Over 107 - 108 4-5 4-5 Over 107~108 STLCOPCB4054140 Copied by mwb 4/2/48 DSW 269040 . l I-A-B-4000 From - Halcyi.Tai Products DiTisiom Union Carbide and Carbon Corporation 30 East 42nd 3treet Hew York 17, New York Letter - TV.C,M./J.IT. Cole, Tech. Rep. 2/16/48 Zyrox 3009 (11-313) GENERAL INFORMATION Color 3p. Gravity ' Softening Pt. Stormer Viscosity Saybolt Furol Viscosity Penetration at 50*0. Penetration at 25C. 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 at 25*C. - Brown - 1.40-1.45 at 25 C. - 79-83C. - 59-89 at 130C. - 79-180 at 130*C. - Approx. 15 (200 gra. load) - Less than 3 (200 gm. load) - Approx. 590*F. - None to 600* F0 - ".'ill not support combustion - Conchoidal - Excellent - Excellent - Average for 24 hours at 130*C. Less than 0.10 mg./s^.cm./hr. - Approx. .001 - Approx. 2.96 - Over 10 raeg. cms. Copied by rs 4/2/48 DSW 269041 STLCOPCB4054141 From - Halowax Products Division Union Carbide and Carbon Corporation 30 East 42nd Street New York 17 , New York Letter - 7J.C.U./J.!;. 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 deg- C. Flash P$. Fire Pt. Combustibility Fracture Acid Resistance Alkali Resistance ,, Volatility P.F. at 25 deg. C. (1000 cycles) Diel. Constant at 25 deg. C. (1000 cycles) DC Resistivity at 25 deg. C. - Brown - 1.29 - 1.32 at 25 deg. C. - 65 - 70 deg. C. - 20-27 at 130 dee. C. - 20-30 at 130 deg. C. - Approx. 75 (50 g. load) - Less than 3 (200 g. load) - Approx. 530 deg. F. - None to 600 deg. F. - Till not support combustion - Conchoidal - Excellent - Excellent - Average for 24 hrs. at 130 deg. C. O.So mg./sq.cm./hr. - Approx. .004 - Approx. 3.0 - Over 10 meg. cms. Copied by rs 4/2/48 0S\N 269042 STLCOPCB4054142 I-A-b-40 STLCOPCB4054143 n h\ d--400 DSW 269044 ( 009-P-V-I r o . Nl o un oo<CDN 5 Vo) o STLCOPCB4054145 From: B.I.O.G. Final Rept. No* 893 . APPENDIX. II. FHT3ICAL AND CHEMICAL PROPERTIES OF CLOFHFN OILS Item Nos. 1, 7, 22, & 31 Pages 108 - 109 (a s quoted in I. G. Farben' s sales sheets) Property Clophen A30 Clophen A40 Clophen A50 Clophen A60 Clophen A70 Clophen A80 Form ............................................. G o Xomr o o * oo o 9 0 Specific Gravity at 20*0 .. 0 Solidifying Point .. . .. e P1qah Point* #o o * o 9 0 Shrinkage: 100* - 20*0 50* - 20*0 .. .. Viscosity at 100*C ,. .. .. Boiling Point Limit at 12mm. Of LlGPCljLX^V Off* oo oo o Loss during Tftacoratlon (after 6 Lours at 100C) 00 99 0 0 90 Volatility at 20*0 oo #o *o (1mm. of Mercury for 100 hours) Heat Conductivity at 40*0 (in Calories per metre per hour per *C). Saponification Ho 0o .. o o Afiil o oo oo oo oo oo oo e o Permittivity at 20*0 .* .. 0 o Pcv:er Factor .. . o .. Bxeokdcwn. Strength .. .. .. o Insulation Re si stance in Ohm o'cm. Liquid Liquid Nearly colourless Nearly colourless 1.35 1.49 -10 *C -5*C 166* 193* (Pensky - Martens) 6$ 6$ 3>t 3$ 1.1"E 1.2E 165 - 195* 180 - 215* 0.05$ 0,03/1 <0.009$ <0.009$ 0.095 0.0 V. small 6.0 <0.001 200kV/cm. 1 X 1013 0.091 0.0 V. small 5.4 <0.001 200kV/cm. 1 X 1013 Liquid Liquid Nearly Nearly colourless colourless 1.55 1,60 +12 *0 +30*C 222* 236 In an open crucible 6$ 3$ lo5*E 6$ 3$ 1.9*E Firm Firm, Nearly crystalline 'vhite colourless 1.7 1.72 - 1.77 +50*0 >160*C 240* 290* or -over . (Pensky - Martens) 5 - 6$ - 3$ 4*E ' ** 190 - 230* 195 - 250* 200 - 255* 210 - 260* 0.02$ <0.009/5 <0.01?: <0.00955 0.01J5 <0.009$ 0.0 (2 hr3. at 125 <0.009$ 0.08? 0.086 0.0 0.0 0.0 V. small V. small V. small 5.0 ^ 4 - 4.5 3.0 <0.001 <0.001 <0.001 >200kV/om. > 200kV/cm. 1 X 1014 >1X 1014 >1 X 1014 0.0 V. small 3.0 - > 1 X 1014 . Clonhens are not combustible and do not. support combustion of materials into which they are impregnated. I-A-B-10 DSW 269046 TABLE I From - United Itates Patent 2,070,268 Patented February 9, 1937 Page 2 2--------3-------4 --5 --- 7-------8-------- Hydrocarbon compositions . Di phenyl Dis tilled high boiling com pounds Percent 0 0 80 80 50 50 Percent 100 10C 20 20 50 50 Properties of dielectric -- Chlo rine content Viscosity sec. lay . bolt at 210* F. Soecifie gravity at 65*/65* C. Dielectric constant K at 100 C. (1,000 cycles) Percent 23,9 40.3 41.2 52.2 42,0 36.4 63 290 35.7 47.5 4e.o 40.8 1.251 1.405 1.352 1.490 1.383 . 1.324 4.35 4.98 4.87 4.56 4.84 4.89 Properties of chlorinated diphenyl 100 0 100 ______1 54,0 42 :,0 46.0 34.0 1,523 1380 4,30 4.80 D Copied by tb 0} 2/2/48 fO ay o nj StxJ IT I Ol 8 M 8o STLCOPCB4054147 I--A ( 3) *"* 500 Stability of Grade P Hycar and Teflon in Aroclor 1254 at 130*C and 45C Short Form Report No. 2179 File No. 141-27.1 . December 29, 1947 Notebook references: Smith 45137 Grade P Hycar and Teflon Immersed in Aroclor 1254 Material Temp. Hours % Gain in ".rt. $ Gain in Thickness Grade P Hycar Grade P Hycar Teflon Teflon 130*C 45C 130 C 45C 285 285 285 285 68.6 26.5 Negligible Negligible 26 6 Negligible Negligible r8 1/14/48 DSW 269048 STLCOPCB4054148 I-A-l - 500 From - I.'erao P.G.B./R.L.T, 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 -7. Grates and Company, Franklin Square, Lone Island, Hew York. It is a CH 4, 100 77att, 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 and 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 ands as such5 is based on the experi ence of the person performing it, '7 keep a standard sample for comparison. If there are any further auestions please feel free to contact us". Cooied by rs 4/2/48 DSW 269049 STLCOPCB4054149 13 - ICC December 2, 1947 ELECTRICAL DATA ON AROCLORS Introduction Time has not permitted us 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 temperatures The dielectric constant values are accurate within .2$ provided the dissipation factor is less than 10$. The error is greater with increasing dissipation factor. The accuracy of loss factor (dielectric constant X dissipation factor) is also dependent on dissipation factor. Aroclor 5442 was the only sample which had a dis sipation factor greater than 10$ and that occurred at the following conditions: 41*C, 500 cycles . 41C, 750 cycles 35C, 500 cycles It will bo 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 50$ 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 269050 STLCOPCB4054150 13 - 100 2 ~ ' December 2, 1947 rizetion effects, even at the high 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. 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 compared 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 high loss substances in the Aroclor. Below 5000 cycles this effect was very noticeable, the diffe rences inrreasing 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 viBC03ity 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 Aroclors have a much larger viscosity-temperature coefficient than the other two plot3. It is hoped that the enclosed -raphs will summarize the dielectric properties of the Aroclors measured. More complete information or any questions concerning the data will he sent on request. acm/ Copied by rs 1/15/48 R. Levreault Monsanto Chemical Company Plastics Division Springfield, Massachusetts DSW 269051 STLCOPCB4054151 K n g rn v in tj 7 X 10 i:i. STLCOPCB4054152 STLCOPCB4054153 DSW 269054 STLCOPCB4054154 II-B From - B.I.0.3, Final Report No, 893 Item Nos. 1, 7, 22, and 31 Pages 12, 13, 14, 15, 16, & 17 III. CHLORINATED DIPHENYLc 1. General. Chlorinated dipbenyl 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 igaxes. 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 n A60 132 tt 1943 tt A50 170 tt tt AGO 506 tt The cost of the material in Germany is:- Type A50 III. 50pfg. to 111. 60pfg. per Kilogram " T64 Bio 20pfg. per Kilogram. The following is a list of the principal prewar consumers of Clophen Giemens-Gchuckert, Berlin. A.E.G. (Hydrawerk), Berlin. TIicafil (Brown Boveri), Zurich, Switzerland. Alsthom, Paris. Ducati, Milan, Italy. It was stated that no German capacitor manufacturer uses Clophen for the manufacture of small capacitors lor radio and telephone purposes and where these have been used by the Ger man fighting services they were supplied by the Italian firm, Ducati. 2, Manufacture, (1) The synthesis of diphenyl from benzene. Diphenyl is synthesised from benzene as shown in the figure, following:- ` DSW 269055 STLCOPCB4054155 -vwv---- * Condenser Distilling Column 500-650aC< J 200*C < Two-stage \ Heat Exchanger Reaction . Coil > 800*C> Synthesis of Diphenyl from Benzene L The synthesis occurs in the vapour phase, at 800"C. and atmospheric pressure, in an electrically heated reaction coil of copper-manganese alloy. No catalyst is required. The apparatus, apart from the reaction coil, is of iron, and operates at the temperatures shown above. About 10/, 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 0,3 to 0.5/ of paraffins but little definite information could be obtained regarding any undesirable impurities or the mechanism by vjhich 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 pre' ise 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.: 0.876 Distilling range: First 5/ within 0.25*0. 5/ - 95/ " 0.25*0. 95/ - end " 0.25O. Solidification point: Not less than 5C. Bromine consumption: Not more than 0.5 gm. bromine per 100 c.c. Sulphuric acid test: Not more than 0.15 gu. K-2^^2^7 Carbon disulphide: Shall be free from C$2. DSW 269056 STLCOPCB4054156 Difficulty in the synthesis wa3 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* but 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 month0 No use is made of chlorterphenyls as paper impregnants, since the materials are resinous and tend to crack; moreover the permittivities axe lower than those of the chlordiphenylso The crude diphenyl is next purified by distillation. During this 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 vacuer yielding 1-4 terphenyl with melting point of 208*Cc 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*C. (2) Chlorination of diphenyl. For the chlorination of diphenyl a lead lined vessel of 10,000 litres capacity is used. It is charged xvith 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 130-155 kg/hour during which time the tem perature is raised gradually from 110*C. to 130*C0 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 1/25! of solid sodium hydroxide* heated and agitated. The sodium hydroxide is allov/ed to settle out and the Clophen drawn off from the top, transferred to another vessel to which Fuller's earth and soda are added and the liquid redistilled. The stills for this process are gas heated. DSW 269057 STLCOPCB4054157 So Properties. ' . (1) Capacitor Impregnating grades,,- A summary of the physical and chemical properties of the capacitor impregnating grades of Clophen is given in Appendix II. Thar are siz grades of capacitor iffipregnante A30,, A40e etc. up to ASO, the 3, 4g 5,, etc. indi cating the number of chlorine radicals combined with the diphenyl. Each grade contains a proportion of the adja cent homologues not exceeding 20^. Grade A30 has the highest value of permittivity,. Theoretically the highest value obtainable with a chlorinated diphenyl is 9,,0B 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 AGO is considered by I.G. to possess the optimum combination of non-inflammability,, stability and viscosity. As with Nibren,, it is considered that no addi tives are required since the substances are stable in U3B provided that the capacitors are efficiently sealed against the air. Kicafil of Zurich are the only users of A30 and A40. The following table shows tho variation in capacitance and power factor with temperature for a Clophen impregna ted paper capacitor. . The impregnant is A50,, the dielectric is Schoeller and . Hbesch "A" finish rag tissue (density 1.2 - 1.25) with a thickness of 10 u? frequency of measurement is 800 c/s. Power factor shows a maximum value of 0.052 at about +4C c while capacitance falls off by some 20% at temperatures below this critical value. Variation in capacitance and power-factcr with temperature for a Clophen-Impregnated capacitor. Temuerature (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 Pactor 0.035 0,024 0.013 0.048 0.052 (max.) 0.006 0.005 0.004 0.005 No 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 269058 STLCOPCB4054158 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 whole 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)P 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. The principal users of this product are A.E.G. and Siemens, but it is understood that, as with other chlorinated com pounds, 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 vras said to be very important to avoid con tamination of Clophen T64 which may occur in transit and for this reason the use of leather for gaskets must be avoided. 4. 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 phen-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 lection II, 5, above. ra 11/19/47 DSW 269059 STLCOPCB4054159 in-A-fc - 500 From - B.I.O.S., Final Report No. 895 Item Nos. 1, 7, 22 and 51 Pa^e xiv Clophen is made in several grades, which correspond closely with their U.S. counterparts, A.50 being the grade most commonly used for capacitora. , Except for very rare use by Siemens and Halske for special ordors, Clophen has not been used in Germany for small capacitors of the tele communication type, but it has been used extensively by Sienens-lchuckert for pov/er capacitors. It is interesting to note that the German forces used Clophen impregnated and filled tubular capacitors made by Ducati, of IJilant who obtained the impregnant from I.G. The prejudice against Clophen was, however, being gradually overcome and several manufacturers were contemplating an extended use of this material. Some of them con sidered it to be equal to or possibly better than mineral oil for opera tion at power frequencies. rs 11/24/47 DSW 269060 STLCOPCB4054160 III-A-b-50 From - B.1,0,3. Final Report No, 893 Item Nos, lg 7, 22, and 31 Page s- 98* 99 (2) Clophen The only chlorinated impregnant used by "SiemensSchuckert is Clophen, supplied by I,,G, In power factor correction and high voltage applications it is consider ed practically idealc The only type of Clophen used in bulk is A,50* pentachlordlphenyl, (corresponding to Aroclor 1254), A,30 and A.40 have been tried and found unstable, .4.60, A,70 and A.80 are too viscous to allow for good impregnation and have lower permittivities. Although the viscosity of A.50 at room temperature is much creater than that of oil, the viscosity at impregnation temperature is sufficiently low to give no trouble in attaining thorough impregnation. A routine check on conductivity is made on each drum of 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 a3 for oil, viz, 10^ ohm.cm, at 20C 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 higjk standard set. Apart from conductivity, further acceptance checks 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 E. 60 pfg./kg., and is therefore much dearer than oil (30 pfg./kg.). 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 (vis. 5). Other impregaants studied. As Clophen is considered nearly ideal, no serious attempts have been made to find aiperior 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 269061 STLCOPCB4054161 dielectric. Tests were performed (see Section 17, 2fl (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 but having a lower melting point so that this possible source of failure e mid 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 for audio-frequency furnaces. Two of these I.Gr,. samples, with references A.162K and A.1621?, are, like Clophen, made from benzene, but have a lower chlorine content because of the presence of an additional alkyl group (CjjH^+l) 8 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 -8C. to -17*C. The permit tivity, viscosity and non-inflammability 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. re 11/19/47 DSW 269062 STLCOPCB4054162 III-B-2500 December 22, 1947 TO: fHOlPIIATE DIVISION T.ALE3FEN 3JBJ: Aroelor 5460 as Used in Ethylcellulose Lacquer RE: Federation of Paint and Varnish Production Clubs Official Digest (October, 1947). Aroclors used as plasticizers and resins impart excellent qualities to ethylcellulose. Ethylcellulose is used in lacquers of various types, the ethylcellulose 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 ouick 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 Aroelor 5460 Ti02 Menthylphenol Toluene Ethanol Parts (by weight) 6.4 6.4 4.2 0.06 67.0 16.0 100.06 rh Copied by rs 2/2/48 Benignus DSVJ 269063 STLCOPCB4054163 II1-0-500 From - Memo G.Y. Frankle/P.G. Benignus March 11, 1948 Soil-Poison Concentrate As described below, the~e materials are formulated into a water emulsifiable soil-poison concentrate carrying almost 80 per cent by weight of active ingredients. Aroclor 1242 Trichlorobenzene (Mixed isomers) Penta chlorophenol Isopropyl alcohol Toluene or Xylene Sterox 3E* 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 NE or Span and Tween can be used to replace the Sterox 3E. Copied by rs 4/2/48 DSW 269064 STLCOPCB4054164 Chemical Abstracts POSSIBLE USE OF AR0CLCR3 Vol. 41 Page 6867 III-H-10 U.S.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 - 80a Cla. Particularly good for use with 11 castings. rs 12/2/47 DSW 269065 STLCOPCB4054165 IV-10 From - B.I.0.3. Final Report ?7o. 895 Iton -Nos. 1, 7, 22 and 51 Pa^es - 10 and 11 Much loss trouble has been experienced with chlordiohenyl than with chlornaphthalene, probably because the former, being liquid, in volves loss physical dontact in disposal, (2) Prevention, Very thorough washing of all areas of the skin likely to be * contaminated with solid, liquid^ or fumes has always been the basic principle in prevention of skin troubles, and is still looked upc-n a o-fundamental0 'Vhen 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 *CTJII.'TBOn, made at Trommersdorf, This has now been replaced, for lack of supplies, by an alternative mads by I.G,, named "MITIGAL", which is considered inferior to cuimbo but satisfactory. The Fissan first put up a special powder named "SCH'TJFEL^ KJLVFRW to act as a harrier, 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 3erlin, 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. lines superfatted soaps have ceased to be available, e cleansing composition containing uichlor-methane 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 ehloracne 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 8 few mild cases of ehloracne have been met. These have been treated with a solution of acetic and salicylic acids in methylated spirits. DSW 269066 STLCOPCB4054166 -2 - {4) Conclusions and Recommendationsa I,,Grt consider that nelthor toxicity nor skin, affection need now be any deterrent to th use of chlorinated nenhthalene,, and that chlordiphenyl is if anything less trouble soft!, Certain people,, notably those with fair skins, show distinct allergyt 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) i3 essen tial and needs strict enforcement. `.lashing with hot water and good soap is sufficient, so long as the soap is superfatted,, since th 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 use of protective clothing and gloves where possible. Areas of the skin which ere contacted by fumes only, and particularly those chafed by clothing (e.g. the nock adjacent to the edge of the clothing) need protection by a suitable soothing powder. ','here fumes are generated, they should be drawn away from the 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 one overhead, with exhaust In two directions simultaneously. In case th precautions are being evaded, or lest there should be Berm idiosyncrasyf monthly medical inspection is desirable. rs 11/24/47 DSW 269067 STLCOPCB4054167 I7-B-100 From - The Journal of Industrial Hygiene and Toxicology Volume 20, Number 2 February, 1938 MORPHOLOGICAL CHANGES IN TIE' LIVERS OF ILVP3 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 electrical 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) v:as 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 experiment (employing an average air con centration of 0.93 mens, par 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 microscopic 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 chlorinated hydrocarbons tested, chlorinated di phenyl gave evidence of being the mo9t"toxic. vJhen administered by inhalation in very low concentrations (average 0.57 to 0.93 mgms. 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). 3ucli cellular alterations t?ere essentially unchanged after a 2 month recovery period. In these animals email eublethal doses of carbon tetrachloride and alcohol uni formly produced extensive liver necrosis and was highly fatal to them (figs. 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 III). However, animals removed from exposure before beinr futally DSW 289068 STLCOPCB4054168 2 - poisoned, subsequently developed hyaline degeneration of liver cells similar to that produced by prolonged administration of small doses of this compoundo Thus the results of the present study,, as well as certain field studies that have been made (1) safest 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 damageo 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 diohenyl than for tricolor- naphthalenes if a safe environment far 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 diphenyl5 its U3e as a sol vent for these compounds would appear to be very hazardous. rs 2/3/43 DSW 269069 STLCOPCB4054169