Document Rp4zNMoav5bV36M1ZL0e7d6Vn

REPORT NO. 2215 FINAL, REPORT ON AROOLOR DATA BOCK Job NO. 171-451 File No. 141-87.1 contained HEREIN IS WE PROPERTY OF THE MONSANTO CHEMICAL COMPANY. RESEARCH DEPARTMENT - PHOSPHATE DIVISION A**n*n*4is*t*o*n,**A#lab*a*m+a* Report Submitted - April 87, 1948 Chemists: A.M. Ellenburg R.R. Knight Prepared by: R.R. Knight Eighteen copies were made of this report and distributed as follows: No. 1. Research File . No. 8. R.L. Jenkins - C.B. Durgln No. 3. R.R. Cole - R.S. Weatherly No. 4. W.T. Durrett - F.P. LaBelle . No. 5. H.F. Wearer No. 6. C.A. Hochwalt ' No. 7. E.P. Rucker No. 8. Edgar E. Hardy No. 9. J.F. Reeves No. 10. J.F. Reeves . No. 11. A.11. Ellenburg No. 18. H.R. Knight No. 13. Paul Logie , No. 14. P.O. Benlgnus No. 15. No. 16. No. 17. No. 18. This is copy No. /5 0231749 HARTOLDMONOOQ4843 RESEARCH DEPARTMENT - PII03PR.TT: 017131 N0N3ANT0 CHEMICAL COMPANY Anniston, Alabama AROCLOR DATA BOOK Conoral Information on properties of Aroclora, Aroolor process data, usee of Aroclore, and physiological effects of Aroclors, F0RB.T ORD As a means of presenting the available date on Aroclors to the in terested personnel within the Konsanto organization, this looseleaf notebook is being compiled. Most of the date has resulted from work carried out within our ovm organization. Literature roference3, hovtever, will be cited in all cases throughout the compilation in order to allow more detailed infor mation to be obtained by tho user. The following detailed outlino is for facilitating the looation of. data in tho book and to assist in properly inserting new data sheets. Each Aroolor is to bo given a series number for location under the . general headings. This soheno at present is as follows! Aroolor 1221 Aroclor 1232 Aroolor 1242 aroclor 1248 Aroclor 1254 Aroolor 1260 Aroclor 1262 Aroclor 1268 Aroelotf 1270 Aroclor 1271 Other Diphenyl Aroclors 100 series 200 aeries 300 series 400 series 500 series 600 series 700 series 800 series 900 series 1000 series 1100 series Aroclor 4465 1500 series Other High Boiler Aroclors Aroclor 5442 Aroclor 5460 Aroclor 5465 , - Aroclor 5468 - 2100 series 2400 series 2500 series 2600 series 2700 series Aroclor 2565 - 3000 series Related Compounds - 4000 aerie s 0231750 w mc H'h'UHMATION HEREIN IS PROPERTY OF The MONSANTO chemical company HARTOLDMONOOQ4844 -2 - The page pertaining to the solubility of Aroclor 44G5 In various solvents would be of this type "IAJ - 1500", In oases where the Infor mation for all Aroolors can be compiled on one sheet, such as refrac tive Indices, the pare will be inserted under the general heading and will bear only the number for the first Aroclor, for example, IAh - 100. I. GENEiiAL FfiOFSiTIEl OF AROCLOR3 A. Physical Properties (a) General Physical Constants . 1. Formula and molecular weight 2. Specifications for lianufaoture (b) Density and Specific Gravity (c) Cubical Coefficients of Expansion (d) Vapor Pressure and Rate of Evaporation (e) Specific Heat and Hoat Capaolty (f) Thermal Conductivity . (g) Viscosity (h) Refractive Index t . (I) Heats of Vaporization - Other Thermodynamic Properties (J) Solubilities ` 00 Flash and Flame Points . (1) Miscellaneous B. Electrical Properties (a) Dielectric Constants (b) Power Factors (c) Dielectric Strength (d) Volume Resistivity (e) Dipole Moments (f) Miscellaneous 0Z31I`)1 HARTOLDMONOOQ4845 -3- II METHODS OF MANUFACTURE A. Monsanto Process 1. Raw Materials 2. Chlorination 3. Distillation 4. Storage and Shipping B. German Process C. Other Processes III. USES OF AR0CLCR3 # A. Electrical Field . 1. Transformers 2.' Capacitors 3. Coating for Vlre 4. Other uses B. Varnishes C. Plastlolzers D. Hydraulic Fluid S. Fire Retardants F. Heating medium 0. Miscellaneous . H. Suggestions for new Uses IV. PHYSIOLOGICAL EFFECTS 1. Skin Tests 8. Systematic Tests . . PATENTS USING AR0CL0R9 02317S2 HARTOLDMONOOQ4846 -4- THIS REPORT AND THE INFORMATION CONTAINED HEREIN IS THE PROPERTY OF THE MONSANTO CHEMICAL COMPANY. The book 1b subjeot to revision and changes as various data are located. Orapha and diagrams will be inserted when possible and new graphs drawn as information is compiled. No indices of sections is planned at this time, but later re visions may include such pages if the volume of information warrants it. Contributions of new and supplementary data are earnestly so licited. Any discrepancies in the existing data or advice as to a better meana of presenting the information will be greatfully acknow. lodged. Address all correspondence to the group leader in charge of the research on Aroclors at Phosphate Division - Research Department, Anniston, Alabama. R. R. Knight re 12/8/47 0231Tb! HARTOLDMONOOQ4847 I u] 4n 14 STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON, ALABAMA Page No. PRODUCT: GRADE: Arcelor 1221 Recylor CODE NO.: 1040-C25-7S-Q9 DATE Deconbor 4, 194B AUTHORIZED: PROD. DEPT. NO.: SUPERSEDES: tlo-.i-TontsUuo R.W.J J.F.U.J F.A.B. APPROVED BY (Initials) 12-17-46 12-10-46 12-19-40 12-10-46 Control Specification Consumer Specification Crude Aroolo? liait 3p, Or. at 65*0, Acidity, m3. HaOII/nm. ( Aroolor 1221: Color Acidity, rafji NaCIl/fp,, 3p, Or. ot 65/15.5*0, Chlorine content VlocoBity ot 100*F. 1.150-1.160 40 AF!li raax. 0,01 mas. 1.145-1.155 20,5-21.5/. 38-41 353 NOTES: Copied by tb f 4/8/40 HARTOLDMONOOQ4848 m t >< STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON, ALABAMA p** n- -- PRODUCT: GRADE: Aroolor 1252 CODE NO.: HerulayAUTHORIZED: 1040-530-75-03 DATE Deoenber 4, 1946 PROD. DEPT. NO.: _________ a SUPERSEDES; Now-TantatiTM K.L.l.} A.tl.E.J T.F.K.j F,A,B. APPROVED BY (Initials) 12-17-46 1S-18-46 13-19-46 12-19-46 Control Specification Consumer Specification 0ru4o Aroolor 113a 3p. (Jr. et 63/10,BC. Aaifilty, mj>, NeOH/pji, Aroolor 1232: Color Acidity, n". NoOH/fjn. 3p, Or. at 65/15,5*0, Chlorine oontent Vlooonlty at 100*F, 1.240-1.245 C.0.5 50 AHIa max. ,01 max. 1,235-1.240 31, ,5--3a .5 46-49 303 . NOTES: Coplea by re 4/6/48 02317^ HARTOLDMONOOQ4849 STANDARD SPECIFICATION OF MONSANTO CHEMICAL COMPANY Profluot: Chlorinated Diphenyl, fllstilled Code No. 1040-340-73-09 Grade; Aroelor 1242.......................................................Data Authorized Tune 21, 1940 Suporaedea Speoiftoatlon Dated July 3, 1934 Tolerable Limits Typloal Value Sp.-Or. at 65/15.5*C, Color, N.P.A. Acidity, Mgra NaOH/gm. Vlacoalty at 54.4*C. 1.338 to 1.348 0.5 Maximum .01 Maximum 47 to 50 Seoonds 3aybolt Universal Approved by A. B, Oarber "' Chief chemist Approved by Edw. A. 0*Neal, Tr. ~ r tforks Manager Approved by Robert S, Weatherly - "sales Manager Authorized by J, N. Carothere Chemical Director Copied by rs 4/8/48 0231766 HARTOLDMON0004850 STANDARD SPECIFICATION OF MONSANTO CHEMICAL COMPANY Product; Chlorinated Diphenyl. distilled Code No. 1040-860-75-09 Grade; Aroolor 1248 Date Authorized June 81 ,, 1940 SuperaedeB Specification Dated July 3, 1954 , Tolerable Limits Typical Value 3p. Or. at 65/15.5*0. Color, N.P.A. Acidity, Mgra HaCB/gn Visoosity at 54.4*0. 1.404 to 1.414 0.5 Maximum .01 Maximum 69 to 76 Seconds Saybolt Universal Aroolor 1262 3p. Or. at 90/15.5*0, Color, N.P.A. Acidity, Mgra NaOH/gn Viaooaity at 98.9*0. 1.572-1.583 1.0 Maximum .01 Maximum 88-100 SOS Code No. 1040-310-75-09 Approved by A. B. Qerber ........ Chief Chemist Approved by Edw. A, O'Neal. Jr, Works ifenager Approved by Robert 3. Weatherly Sales tlanager Authorized byJ. N. Carothere ' "1 ' Chemical Direotor Copied by ra 4/8/48 0231757 HARTOLDMONOOQ4851 .STANDARD SPECIFICATION . OF . Producti Aroolor 1264 MONSANTO CHEMICAL COMPANY ' ' \' ' Code No. 1040-280-75-09 grade; Dleleotrio Date Authorized I0/g/4I SuperBedes: 6/81/40 Color. AFHA seale Condition Speoltio gravity at 65/18.5*C Aoldlty, Mgm. NaOH/gm. Inorganlo Chlorides, ppm. Saybolt Vieooslty at 98.9*C, eeo. Dieleotrlo Constant at 100*C Resistivity at 100*C, ohm-om.bt 500 volts Refraotlve Index at 25*0 Distilling Range, Observed, 10$ Observed, 50$ , Observed, 90$ Pour Point Water, ppm. ' Evaporation, 6 Hra. at 100*C Corrosion Test-Change in weight Aoldlty after test InorganioCbTorldes after test Condition after test Color after test rs 6/11/48 100 Uax. Clear 1.495-1.505 .01 0.10 t&X. 44.5-47.6 4.15-4.35 Above 600 X 10* 1.6370-1.6390 350-555*0 355-368*0 368-375*0 8 to 18 36 ltex. . $0.4$ 00 0.01 0.10 Max. Clear 150 Uax. 0831758 HARTOLDMONOOQ4852 STANDARD SPECIFICATION OF MONSANTO CHEMICAL COMPANT Product: Aroolor 1260 Ore4#: Dleleefcrlo ' Coda No. 1040-890-73-09 Data Authorized 11/18/41 Supersedes: 1/30/36 Color, AMA Scale , Condition Speolfle Oravlty at 90/15.5*0 Acidity, Ugm. NaOH/gm. . Inorganic Chlorides, ppm. . SayboIt Vlaooelty at 98.9*0, seo. Dlolectrlo Constant at 100*C Resletlrlty at 100*0, ohn-om. at 500 volts Refraetlve Index at 85*C Distilling Range, Observed, 10$ ' Observed, 8055 Observed, 90$ Pour Point Water, ppm. Evaporation, 6 Hra. at 100*C Oorroelon Test-Change In weight Add ity after test Inorganic bhlorldee after test Oondition after test Color ' -- after test 100 Max. Clear ' 1,550-1.860 .01 0,10 Ifex. 73-80 36""38 Above 500 X 10 1.6433-1.6468 370-377*0 377-383*C 385-400*C 86 - 34 35 Max. 0.8 $ 0.0$ 0.01 0.10 Max. Clear 150 Max. re B/ll/M 0831759 HARTOLDMONOOQ4853 SPECIFICATIONS 7CB SOLID PISTOLED AROCLQR3 PROICCT APPEARANCE %. COLOR ACID NO. lfe.RaCB/0B COLCR 5$ TOLUENE HELTUfO pomp TOTAL CHLORINE s 1268 1269 1270 1271 VIhite to yellow crystalline ponder v/hlte to erey or ligtt yellow crystalline ponder * Uhite crystalline ponder Practically white light fluffy ponder 135-160*C. 225-255*0. 285-300*0 0.05 Max. 80 AP3A ISax. 80 AB3A Max. 304*0. ran. 69.5 70.5% Copied by rs 4/8/48 09lU Z HARTOLDMONOOQ4854 STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON, ALABAMA Page No. PRODUCT: tooolog 4465 (iicrular)_____ GRADE: _______________________________ _____ CODE NO.: 1040-430-2*3-09 DATE _____ AUTHORIZED: October it, IQaa PROD. DEPT. NO.: _______________________ ____ SUPERSEDES: Time 3. 1944 n.i.3. j n.tv;.j PL.) APPROVED BY (Initial#) 3-30-44 9^9-44 lO-g-44 10-3-44 10-4V.A__________ Control Specification Contumer Specification Appearance s Color, N.P.A.* Toftenin^ Point Acid Humber (MfjfitoOlVcra.) CryetaLllnlty clear, llybt ysllcw, brittle restn 8.0 nax. 60 - 66C. 0 - .035 Ho. spec. * Rcioinf; color limit to 2.0 noxlmum la recommended because Indication records ehmi that all lots produced In 1941 hflVfi hod n color of 1 ,,3fv. NOTES: Copied, by re 4/8/40 0231761 HARTOLDMONOOQ4855 ( STANDARD SPECIFICATION Of MONSANTO CHEMICAL COMPANY r Product: Chlorinated High Boiler Code No, 1040-480-75-09 Prado: Aroolor 8460 Date Authorized May 10, 1940 Supersedes Specification Dated Deoember 23, 1933 Tolerable Limits Typical Value Appearance Clear, light yellow, brittle resin Color, N.P.A. 2.0 maximum Crystallinity Test To pass test Softening Point, ASTEJ 100 - 105.5C. ( Acid Number mgyn NaOH/gm. 0 - .05 Chlorine 59.0-80.6$ Approved by A. B, Oerbar Chief Chemist Approved by Edw. A, O'Neal, Jr, Works Manager Copied by rs 4/8/48 Approved by Robert S. Weatherly, 5/6/40 " ' '' ' Sales Manager Authorized by T. N, Carothera, 5/10/40 SKimical Director c 023l7faZ HARTOLDMONOOQ4856 Monsanto Chemical Company Anniston, Alabama Aroolor Test Methods and Designations `'"speolflo Gravity of Aroolors Total Chlorine in Aroclore ' i Softening Point of Solid Aroolors Determination of Iron In Aroolor Flash and Flame Points Vleoosity of Liquid Aroolors Distillation Range of Aroolors Evaporation Test of Liquid Aroolors Refraotlve Index of Liquid Aroolors Resistivity of Liquid Aroolors Dieleotrlo Constant of Liquid Aroolors Aold Number of Liquid Aroolor Color of Aroolor - NPA Scale Color of Aroolor - aVBa scale Aold Number of solid Aroolors Pour Point of liquid Aroolors Inorganic Chlorides in Aroolors Viator Content of Liquid Aroolors CjdLisis ' 14-10-48 14-13-48 14-17-48 14-81-48 14-84-48 14-89-48 14-81-48 14-38-48 14-34-48 14-35-48 14-36-48 14-48-48 14-43-48 14-44-48 14-46-48 14-47-48 14-48-48 14-53-48 0Z31763 HARTOLDMONOOQ4857 Monsanto Chemical Company Anniston.method no. 14-10-46 Specific Gravity of Aroolors The temperature at which the Gravities of liquid Aroolore are taken varies with the vlsooslty of the liquid. Note the temperature at nhloh the Gravity is to be taken for the Aroelor under test and heat the sample to 10*0. above that temperature. Pour the hot sample Into the steam or hot water jacketed hydrometer jar provided for thla test. Stir well with an accurate thermometer and adjuet 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. Alloy; the-hydrometer to sink into the liquid, then read the hydrometer scale at the point of the lower meniscus and record with the temperature. Report the specific Gravity to the nearest 0.001 unit. 0231764 HARTOLDMONOOQ4858 Monsanto Chemical Company Anniston Method Mo. 14-13-48 .UBXECT; . Total Chlorine In Aroclors IT.'KJOD; Volhard Titration following Peroxide Fusion Chlorine in Aroolors may he determined by fusion of the sample with sodium peroxide in a Burgess-Parr fusion cup, extracting the fusion with water, acidifying tho 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 . Tho fusion cup used is the 3urgess-Parr Sulfur Bomb No. 3 for flame ignition. A lead gasket is used. For ignition, the bomb is sus pended through a 1-3/16" round hole in a 1/8" transits plate. This allows the fusion cup to extend through the Plate for about 5/8 inch. - Ignition is effected by strongly heating the bottom of the fusion eup with the full flame of a Meker burner for two minutes. The bomb, gaskets, and the sodium peroxide are obtained from the Parr Instrument Company, Moline, Illinois. Charge for Fusion The fusion mixture is made up of about 15 grams (one natal seoop) of sodium peroxide and 0.3 grans of finely powdered cane sugar. The reagents should be free from chlorine, or a blank run and corrected accordingly. The fusion mixture is well mixed by placing the ingre 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 email pellets. These are prepared by heating the Aroclor until a oonsietenoy is reached os will permit dropping, it from a glass stirring rod onto a tinned surface (a can top), etch drop forming a pellet. Vfhen oool 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 oup and the fusion mixture placed on top of them. Aftor tightening the lid, the charge is ready for fusion. The crystalline type Aroolora are weighed in the powdered form. ,4 grams being used. They are charged in the same manner as the non crystalline type. . 0231765 HARTOLDMONOOQ4859 Total Chlorine In Aroolors -2- LICPID AROOLORS: .80 to .50 grama ere weighed by drO-nlng from a stirring rod onto a place of thin hemlspherically shaped glass, or 1/2 gelatin capsul (Gelatin Capsules No. 00, United Drug Company, Boston - St. Louis), which has been Just previously tared, and which remains on the balance. It is necessary to beat the more viscous Aroolors to "dropping" consistency. The piece of glass then easily slides off the balanoe pan Into the fusion cup. Cover with the fusion mixture. The following quantities of e-.mple, sugar, and AgN03 are used for the reapeotlve chlorine contents: 01 Content '/eight of sample Amount Sugar AgNOg 0$ - 30$ 30$ - 45$ 45$ - 58$ 98$ - 66$ 66$ - 70$ 0.8 grams 0.3 grams 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, Procedure Place the fusion oup, whloh contains the prepared sample and fusion mixture, in the transits ignition plate and apply the full flame of the Meker 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. '.'.'hen cool remove screw cap. Thoroughly rinse the cup cover with water, collecting the rinsings in a olean 400 ml. beaker. Then piece the fusion cup on its side In the beaker and cover with a watch glass. 50-75 ml. will be In the beaker from rtnBing the eap, and this Is sufficient to decompose thg charge. Remove the oup and rinse well. Then decomposition Is complete, rinse off cover-glees and add pure HN0s, with stirring, until sold is present In excess to the extent of about 10 ml. (About 50 ml. of acid are required.) Add exaetly 50, 75, or 100 ml. of standard silver nitrate solution from a plpet (depending upon chlorine present) and stir to effect coagulation of silver nitrate precipitate. Filter with suction through an asbestos pad on a 1-1/2" perforated porcelain plate and wash beaker and filter 4 ' times with email portions of cold watar. Allow the filter to drain com pletely between washings. Transfer the filtrqte hack into the 400 ml. beaker and rinse the flask twice, adding, the rinsings to the beaker. Add 5 ml. of l'errlo Iron indicator to the solution and titrate with standard KCN3 solution until a distinct pink tint Is just obtained. 0231766 HARTOLDMON0004860 Total Chlorine In Aroolors -3- Calculation of Chlorine Content Subtract the volume of X0N3 require! from the volume of KCNS required to titrate the amount of standard AgtI03 solution used. This will give the volume of KCN3 equivalent to the chlorine in the sample. Multiply the volume so obtained by the chlorine value of each ml. of KCN3 and divide by the weight of sample taken. For example: If 50 ml. of silver nitrate solution is equivalent to 61.4 ml. of KCN3 solution and the volue of 1 ml. of KCN3 solution Is .003770 gram Cl; then If It is found that 0.3 rram of sample shows a KOMI titration of 10.4 ml. the percent of ohiurine Is: - 10.4) X .003770 X 100 . 64.0955 Cl .3 ' In ease the l'uelon mixture or other reagents contain ohlorine, the amount must Vie determined and deducted from the chlorine found. Solutions Required . Standard AgIJOs solution: Dissolve 22 grams of sliver nitrate in eaoh liter of viator. Protect the solution from light. Standard KCN3 solution: Dissolve 10 'rams of KCM3 in 1 liter of prater. Ferric Iron Indicator: Use a saturated solution of ferric ammonium alum, about 50 g. per 100 ml. of water. Pure Nitric Add: Stock acid suffices provided It Is colorless. It oaa be boiled in a beaker until colorless If neoessary using 600 ml. HMO.j and 300 ml. of HgO. , Standardization of Solutions , ,'elgh 0.3 and 0.15 gram portions of pure dry NaCl Into separate 600 ml. beakers. Add 250 ml. of distilled water to each and 10 ml. of pure 5055 nitric acid. Vihen solution la complete, add 50 ml. of standard A$)0a solution from plpet. stir well and filter through an asbestos mat on a perforated porcelain plate, using suction. Wash filter and transfer the filtrate back to the beaker In the same manner es when working with a sample. Titrate the filtrates with standard KCN3 solu tion, using ferrle Iron Indicator. The value of 50 ml. of Afd?03 solution In terms of KCN3 solution Is found by subtracting the ml. of KCNS solution In titrating the 0.3 gram of NaOl from twice the number of ml. of KCNS solution used In titrating the 0.15 gram of NaCl. onnbi HARTOLDMONOOQ4861 Total Chlorine In Aroclors -4- This value is oheoked by titrating 50 ml. ot A$TO3 solution added to 400 ml. of water and 10 ml. of pure 50# HN0S with TONS solution. This titration should agree very closely (4 0.1 ml.) with the value found from the titration of NaCl. The titration muat be made slowly to avoid drainage error. . Since pure Had eontalns 60.66# 01 by theory, the value of the XCNS in terms of ohlorlne may be found by dividing the weicht 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 TONS titrations of 13,11 and 13.13 ml. Two 0.15 gram portions of NaCl show TONS titrations of 37.88 and 37.84 ml. The TON'S equivalent to 50 ml. of AgNOg is then (37.88 * 37.84) - 13.18 or 61.4 ml. By titration of 50 ml. of AgNOs against TON'S 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 XCNS Is then, .6066 X .3 divided by 61.4 13.18 or -.003770 grams Cl per ml. of TONS. The chlorine value may also be calculated front the titration of 0.15 gram of NaCl. 0.6066 X .15 divided by 61.4 - 37.86 gives .003770 (jramB Cl, per ml. of TONS. Precautions 1. The fusion materials have explosive properties If handled Improporly; consequently care must be taken to u3e safe proportions, to seoure a good mixture free of large lumps, and to uroperly seat the cover of the fusion cup. The fusion mixture must be kept away from vreter or moist air, either of w! ioh may ignite the oharge. The fusion mixture should not be ground to reduce lumps. 8. The method as described Is not applicable to volatile organic com pounds unless precautions are taken to avoid loss of sample during weighing. Effect of Variables ' 1. On aooount of the high chlorine content of many of the Aroclors and the mall amount of sample taken, great aoeuraoy le required in weighing, transfer, end mixing of the sample. The plpet and buret for measuring tbs standard solutions must be very clean to avoid drainage errors. 73l768 HARTOLDMONOOQ4862 Total Chlorine In Aroolors -5- 8, Fusions whloh show black carbon deposltes on the cover and side of tho fusion oup may or may not five the full chlorine content. If a carbon deposit is found, a second fusion should be made using a smaller cample 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 content may be determined by making a blank fusion, that.la, without addition of sample, end titrating In the usual way. Five ml. of AgNOs may be added Instead of 50 ml. portions of AgN03 solution In like volumes of solution and nitric aoid. References , Beamish: Determination of Organic Halogens, Ind. Eng. Chom., Anal. Ed., 353 (1934). FAB:cm 1-29-45 Copied by rs 4/20/48 0231769 HARTOLDMONOOQ4863 Monsanto Chemical Company Anniston Method No. 14-17-4 SUBJECT: softening Point of Solid Aroclors METHOD: Ball and Ring This method is a modification of the A.3.T.I". standard method of test for sojftenlng point of bituminous materials, serial designation: rings are larger than..-apael^led. A two ring support is also U3ed in order that two tests may be made simultaneously. M5ia2!' ` 4* The apparatus oonsists of the following: (a) Two tapered brass rln^s, 5/8" inside dia. at bottom, JtljrflB" Inside diameter at top and l/4" deep: thiokness of wall 3jQ0M%L(b)KTwo steel balls, 3/8" diameter weighing 3.45 to 3,55 grams each. (c) A 800 ml. Griffin lov: form beaker, (d) A ring support for the two rings having a brass plate exactly one inch be low the plate supporting the ring, (e) A 600C. AiO.T.Kr-lou dtatllla-v tlcn thermometer grudaatod-4P9. (X, P S7A7 Lo^v- r-r- HA+X f .. ar Preparation of the Sample / The somple 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 oooling. Since the Aroolors shrink considerably on cooling, the ring should be -veil 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 eooled Aroolar from dropping out of the ring. .In the same way, the second ring is filled with a standard Aroolar of known'softenlng, point. The standard Aroelor should have a softening within at least 10 to 15of ths Aroelor being tested. The rings while being filled should rest on a clean can lid or on a brass plate whioh has been amalgamated to prevent the Aroolar from ad hering to it. The Aroelor In the rings should be fully cooled and hardened before proceding with the test. Procedure Add cool solution (employ water for softening point between 0-80`C, glycerin for between 80-200*0., mineral oil for above 200*0.) to the beaker until the surface of the solution is 2" above the plate holding the ringe when the ring support' is suspended in the beaker. Place the rings containing the Aroelor to be tested and the standard Aroelor on the ring support. Place a ball on ths center of the upper surface of the Aroelor in each ring. Suspend the thermometer so that ths bottom of the bulb Is level with thebottom of the rings and Just midway be- tween the two rings. '7Xo 2, / '*''`7 1 023X770 HARTOLDMONOOQ4864 Softening Point of Solid Aroclaro - z - 4 /iyM* Place beatcer and apparatus on a S-4ae& fhv a /V-. -0 , feoc>faa''Py' tne tmerraornetet ut the in3tE?nv te$ 'Arociar WoteoBhes the bottom plate la reported as the softening point. The heat- la eontlnued until both Aroolora have dropped to the bottom 'late, 1. cToherresctatinodnasrdarAeromealdoer fiosr reumneargloentg swteitmh. the sample under test In order to compensate for Variations in rate of heating, dilution of glycerin, and thermometer variations. 8. 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 aB near as possible to S*C. per minute. 3. The elyoerin may be used repeatedly for the tests after removal of the Aroelor. 4. Benzol Is used for cleaning the rings and bolls. 5, '.'ator can be U3ed Instead of glycerin for softening points up to 90*C. 6. For softening points above l8*e, well boiled glyoerln should be used. The usual glyoorin Is not satisfactory above 125 to 130*C, It boils with loss of rioter while the temperature remains practl- oally constant. It la well to have a supnly of hlgh-bolling glycerin on hand to be used only for softening points above 9e`C 7, Air bubbles on the rings and balls during the test should be avoided as far as possible. 8. The rate of rise of temperature of the glycerin shall be uniform for eaoh minute after the first 3 minutes of heating end not averaged over the period of the test. by rs 0231771 HARTOLDMONOOQ4865 Konaanto Chemical Company Anniston Method No. 14-41-45 SUBJECT: Determination of Iron In Aroalors 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 lh the combined extraets Is then determined by dlchromate titration. . Procedure Transfer 5-10 grams of sample to a dean separatory funnel of about 150 ml. capacity. Add about 50 ml. of benzol and shake until the sample is In solution. . VJhen 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 oomplete, then draw off and preserve the add extract. Add another 10 ml, of 1:1 HC1 and shake again. Draw off the add layer and combine with the first extraot. Continue until HC1 layer Is dear. Determine the Iron by usual dlchromate titration method. FAB:cm 1-31-45 (j- * by re 4 0231772 HARTOLDMONOOQ4866 I Monsanto Chemical Company Anniston Method Ho. 14-24-48 3JBJECT: Flash and Flame Points I.l'.TJIOD; Cloveland Open Cup The flush and flame points of Aroolor shall be determined In the Cleveland Open Cup Teeter, following the procedure described In A5TU D 92-33. Apparatus . The oup 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 elate there shall be a plane depression 1/32" (.079 cm) In depth, and of Just sufficient diameter to fit cup. There shall be a clroular opening 5/16" (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 thiokness, and of the same shape as the metal plate. There shall be cut In the center of the as- bestOB board a circular hole Just fittln" the cup. Heat may be supplied from any convenient source. The use of a gas burner, eleotrlo heater, or aleohol lamp Is permitted, but under no circumstances are products of com bustion 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 produoe local superheating. If a flame heater Is used. It may be protected from drafts or excessive radiation by any suitable type of shield, that does not project above the level of the upper surface of the asbestos board. The thermometer shall conform to the requirements of thermometer No. 8. (3ee A3TK 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 oup, and above a point half way between the center and baok of the eup. The cup shall be filled with oil to be tested In euoh 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 tbe filling line or outside of apparatus. The test flame shall be approximately 5/32" (.397 cm) in diameter. The teat flame shall be applied as the temperature read on the thermo meter reeohee eaoh successive 5*F mark. The flame ehall pass In a straight line, (or on the circumference of a circle having a radius of at least 6 inches.) across the center of the cup and at right angles to the diameter passing, thru the thermometer. The test flame shall, .while passing aoross the surface of the oil, be in the plane of the upper edge of the cup. The time for the paasag.e of the test flame across the cuo shall be approxi mately 1 second. 0231773 HARTOLDMONOOQ4867 Flash and Flame Points -2 - The oil shall he heated at a rate not exceeding 50*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 shell be decreased and for at least the last 50F before the flesh point Is reached the rate shall be not less than 9*F. or more than 11F per minute. The flash point shall be taken as the temperature read on the thermo meter when a flash apiaara at any point on the surface of the oil. The true flash must not he confused with a' bluish halo which sometimes surrounds the test flame. After determining the flash point, tha beating shall he continued at the speolfied rate of 9*F to 11*F per minute, and application of the test flame shall be made at the specified Intervals until the oil Ignites and con tinues to burn for a poriod of at least five seconds. The method of application of the flame shall he the same as for flash point. The tem perature reud at the time of the flame application, which causes burning ( for a period of five seconds or more, shall he 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 dis cernible. Mote ' , Aroolors 1248, 1254, 1260, and higher chlorinated Aroclor3 do not have a distinct flash or flame point below their boiling temperatures. FAB:om 1-26-45 Copied by rs 4/21/48 023177" HARTOLDMONOOQ4868 M3NSANTO CH:,MICAL COMPANY Anniston, Alabama Analytical Laboratory Anniston Method Humber 14-4-53 Test Method: Viscosity -- Saybolt Universal Heferenoe: Method Ho. U,433-52 Y.GK OM 25 1. Take a scrupulously dean, dry 60 ml. viscosity receiving flask from the oven and allow it to oool to room temperature while the viscosimeter is being cleaned. (Use only receiving flasks which have been standardized and found to be within + 0.05 ml. of 60.00 ml.) ' "~ 2. Clean the viscosimeter tube as follows: A. Insert the cork, whioh should bo clean and in good condition, in place in the bottom of the tube. B. Carefully pour enough benzene into the tube so that the latter is filled and the liquid overflows lhto the gallery. Do not allow any benzene to spill down into the oil both, as the vapors will affeot later visoosities. Caution: While using benzene far cleaning the viscosimeter, be sure all oirouits of the instrument ere turned off. C. Using a thermometer fitted with a holder to prevent it touching the bottom of the tube, stir the mixture well so that any adhering material is dissolved. Be sure the entire inner surface of the tube and gallery is wet. Pull the cork to drain the tube. With a clean withdrawal tube draw the exoess liquid from the gallery-and discharge it direotly into a beaker -- not into the visoosity tube, D. Repeat steps A. -- C. inclusive. E. Permit the visoosimeter tube to drain and dry. ABSOLUTELY DO NOT INTRODUCE A CLOTH OR KLEENEX INTO TIE TUBE OR CALLERY FOR BLOTTIIO UP RESIDUAL LIQUID. F. Hush oa. 80 ml. of the well-ehaten (and heated if needed to Insure fluidity) sample to be tested through the apparatus and follow step C. above. C. Drain this out, and again flush with a fresh portion of, Sample to make oertain any last drops of previous material have been rinsed out. H. Shine a pen--light up through the orifice while looking down into the tube. The orifice should be free of fibers or any other obstruction. If these are present, they should bo removed by flushing with sanple only, not by use of wires. If flushing with sample fails, Inform the super visor. 023177b HARTOLDMONOOQ4869 ADDITIONAL PRECAUTIONS: A. See that the bath oil, then hot, ia not leas than 1/4" above the level of the overflow rim of the gallery of the tube, B, The bath oil should be a grade of light--colored mineral oil whioh has a visoosity of 40 _+ 5 Saybolt seconds at 810r and should be replaced when it displays a definite darkened color, 0. For viscosities to be run at 100F, the both oil temper ature shall not exceed 100.25F (+ 0.05CF for 10 Min,). For visoositltes determined at luC'F, the bath teinperatire shall not exoeed 130.50F (+ 0.05'? for 10 Min.), For viscosities determined at 210F, the bath shall not ex" oeed 218.0*F (+ 0.10'F for 10 Min.). D. Use only thermometers standardized to the nearest 0.01`F against a National Bureau of Standards thermometer. E. Use only the stopwatoh provided for timing purposes, whioh should be aoourate to within 0.1 per oent when tested over a 60 minute period. Electrical timers must not be used unless the available power souroe is known to be of sufficiently accurate frequency. The stopwatoh mus; be . left in the holder provided, since variations in its position can oause error. F. Never use the plunger, commonly provided, for defining the instument and never expose the viscosimeter to a draft during a determination. 3. Blot the cork dry with a lint--free cloth and insert it in the tube. Four oa. 150 ml. of sample into a scrupulously clean beekBr which has been rinsed with sample, and heat the contents to not over 7*F hotter than the temperature of test. Do not use a sample whioh has overheated, even if it is then cooled to with in the prescribed range. 4. Pour enough heated sample into the tube that it ceases to over flow into gallery. All samples must be strained through the 100 mesh soreen whioh has been carefully flushed with sample. 5. Stir the sample with the standardized thermometer (with attach ed holder) until its temperature has remained constant within 0.02F of the desired temperature for one full minute (with oonstant stirring). NOTE; Stirring is a very critioal point, especially in the case of more vlsoous liquids suoh as Aroolor 1260. Use the exact technique described as follows: 0831776 HARTOLDMON0004870 Stir the sample with the thermometer, continuously in the same direction, at a measured rate of three revolutions per seoond. Alternately sweep the thermometer against the walls of the tube far five revolutions and then stir in the center of the tube for three revolutions. Do not deviate from the prescribed rate of stirring or the practice of stirring five revolutions at tie v/olls of the tubs, three revolutions at the center, five at the walls, three at the center and so on for the one-minute period specified. Regulate the temperature of the sample while stirring, by adjusting the oil bath until the desired reading holds oonstant within _+ 0.02F throughout the required interval. Do not stir by moving the thermometer up and down unless you desire to cool the sample, and under no olroum9tances stir in this manner during the oneminute timed Interval, 6. Remove the surplus sample from the gallery, with the scrupu lously clean withdrawal tube which is inserted at one point in the gallery without touching the over-flow rim, and which removes sufficient sample that the level of sample in the gallery is below the level of sample in the oil tube proper. Do not rotate the withdrawal tube around the gallery. 7. Plaoe the receiving flask in position so that the stream of oil from the outlet tube strikes the neck of the flask. 8. Snap the cork from its position, and at the same instant start the stopwatch. 9. Stop the stopwatch at the same instant that the bottom of the meniscus of the sample reaches the mark on the neck of the receiving flask. 10. Examine the end of the cork to see if it has become moistened with sample. This would denote an incomplete seal and a pre mature seepage of sample through the orifice which would produce erroneous results. The time in seconds, after applying the proper calibration correction of the tube is the Saybolt Universal Viscosity. Different operators in different laboratories should agree within 0.5/ on all readings. Report the results to the nearest 0.1 seconds. Reference: ASTM D-88-44 OPERATION OF T1IE TAG VISCOSIMETER The visooslmeter is heating when the lamp is off. Do not go away and leave the "quiok heat" on. The 'iiuiok heat" should be turned off when the temperature of the bath is within 1 degree of the desired bath temperature. The viscosimeter should be allowed 02*1777 HARTOLDMONOOQ4871 00 minutes to oome to temperature equilibrium before making a test. This will allow the metal parts of the viaoosimeter to corns to temperature equilibrium with the bath. Note s Every non and then, trouble will be found in getting the bath to hold the proper temperature. 0Z31778 HARTOLDMONOOQ4872 Monsanto Chemical Company Anniston Method No. 14-31-48 qUBJECTi Distillation Ran>*9 of Liquid Aroelors ISSTnOD: A.5.T.M, D-20 with Modifications The apparatus, consisting of flask, condenser tube, shield, end ther mometer, Is exactly the same as described under A.3.T.I1. test D-SO "Distillation of Bituminous Materials suitable for Hoad Treatment". ?' >l' 'I Attaoh a 6 lnoh auxiliary thermometer (0 - 150*0.) to distillation ; thermometer. Plooe bulb half v.ay between top of cork and probable i' average of distillation range. Cover both thermometers with a 3/4" diameter glass tube to insure a uniform temperature correction for the exposed stem, barometric pressure and thermometer error. 1 >' The procedure Is changed only to the extent that thermometer readings are taken when specified percentages (usually 10, 50, and 90^) of Aroolor have been distilled instead of following the A.I.T.K. proce dure of weighing the distillate between specified thermometer readings. In testing liquid Aroelors, 100 gras, of sample ere 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 / "felgh out 100 grams of sample into the distilling flask. Assemble apparatus as described under A.3.T.M. D-SO.., Insert thermometer ' (A.3.T.K. high distilling 0 - 400*0.) thru oork In the neok of the 'flask so that the top of the bulb is level with the lowest point of -Junoture-of the tubulature end neck of the flask.- Apply heat to the flask supported on two sheets of 20 mesh wire gauze so that the first drop oomes over in from 5 to 15 minutes. ' Conluet distillation at rate of 50 to V0 drops per minute. Collect distillate in a S50 ml. beaker tared on a balance. Take temperature -readings at -1$,-3#,--'40/;~305; fiO/j-VOj -8OjJ,-W>0, -93, 95, 96, 9VJS, end dry. " Corrections for emergent stem and pressure are applied to the thermo meter readings if required. Ta*e correction TSadlngs nt first dropy, 40;i,-50^, .90^,-on4^dfy. Report the temperatures to the nearest 1*0. Example: /(Exposed1 stem in degrees) X (temperature difference in degrees) X 0.000158 degrees stem/orreotion The exposed stem is read from the top/of the cork. The'temperature'difference is the reading of the . thermometer minus the temperature of the auxiliary thormometer. 0231779 HARTOLDMONOOQ4873 Distillation Ranee of LIquia Aroolors - 2 - 0.00012 Tj, 4 b " barometric correction Tb normal boiling point in decrees absolute} A p ^change injjressure from 760 mm. ThpWJrreotloj/la added If'barometer is helpTM norraaVand sub/raoted If the barometer Is aboye normal.- (MacDougnll - "Thermodynamics and Chemistry" pp. 113). Corrected Temperature Observed temperature Tl t Tg. FABiera 1-29-45 Copied by re 4/22/48 0231780 HARTOLDMONOOQ4874 Monsanto Chemical Company Anniston Method No. 14-32-48 SUBJECT: Evaporation Teat Of Llould Aroclors METHOD: 6 Hours Heating at 1Q0C AST:' D6-39T - Modified Procedure V.'eish on a rough holance about 50 grams (7 .5 gm.) of the well mixed Aroolor Into an accurately tared tin box, 55 mm. dla. X 33 mm. deep (3 oz. Oill-style ointment box, deep pattern), Fisher jfl-820. Let stand until box and sample are at room temperature, then weigh accu rately. - Place the box in a ventilated convection oven maintained at 100*C. 1 1 for 6 hours. Remove, cool In desieoator to room temperature and accurately rewelgh. From the loss In weight calculate the evaporation in per oent. Report to second decimal place only. Notes 1. Be sure box Is at room temperature whenever exact weight Is taken. 2. The oven Should not contain other samples which might Interfere with evaporation. 3. Beoause the evaporation loss Is sensitive to temperature, the air bath must be closely maintained at 100*C. FAB:cm 1-29-45 Copied by rs 4/23/48 0231781 HARTOLDMONOOQ4875 Monsanto Chemise1 Company Anniston Method No 14-54-48 SUBJECT; Refractive Index of Liquid Arociors METHOD:Abbe Refractomoter Refractive Index The refractive Index of any medium la defined as the ratio of the ve locity of light In air to the velocity of light In that medium. It is measured by the ratio of the sine of the incident ancle to the sine of the angle of refraotlon. The denser the medium, the 'greater is the refraction toward the normal (higher refraotlve Index). Beoause the refraetlve 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 Arocior testing refraotlve Index pro vides a verification of composition and purity. Apparatus _ Abbe Refrootometer with accessories, Bausch and Lomb, Cat. #2550, Serial No.'577. Calibrated to read directly In terms of refraotlve Index of the D line (sodium) at a temperature of 80"C. Procedure . Operators should be familiar with the Bausoh end Lomb "Directions far Use" and praetlce the manipulation as there described before attempting determinations on Arocior. The abridged directions below provide a working outline but at the expense of omission of essential explanatory details which ere contained In the B. and L. directions. Sorew thermometer Into its socket In '.rater jacket of upper prism. Open prisms and check their condition. Clean If they are soiled, streaked, or spotted. With lower fixed prism horizontal, place on It 2 or 5 drops of the Aroolor 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 refrao- tometer. No spots on air pockets should be visible. Connect water Jacket to sour-oe of constant temperature water, usually the tap, and pass water until the thermometer has been constant to 0.2C. for at least 5 minutes at 25*C. The Aroolors flow more easily at 25"C., henoe the choice of this temperature. With prisms illuminated, rotate the prisms by means of the index arms until the border of the light and dark fields passes exaotly thru the intersection of the cross hairs. If the border line Is fringed with oolor, rotate the compensator until the color disappears. If the boun- 02^782 HARTOLDMONOOQ4876 Refractive Index of Liquid Aroolors - - dary Is not sharp, adjust mirror until a distinct half shadow Is ob tained, If the line or the cross hairs are blurred, adjust eyenlece until a bo011 focus Is obtained. Secure final fine adjustment by means of the slow motion screw. ' Read the refractive index, estimating to the fourth decimal place. If the temperature of the water jacket Is other than 25*C., correct to 25* by use of the correction factor, 0,00044 per *C. This factor is applicable only to Aroolors 1248, 1254, 1260, and 1262. It was found by careful measurement on each Aroclor thru the range 10* to S0*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 1.6432 at 15*C., the index corrected to 25*0. is 1.6422 - (10 X .00014) - 1.6370. Care and Calibration of Instrument Immediately after use, clean the prisms with swabs of pure ootton dipped In benzol, finally wiping dry with a soft cloth. The prisms, especially the upper one, tarnish end scratch easily. Consequently great core must be taken In meaning. Before use the prlsmB should always be Inspected and recleaned If necessary. '.Then not in use, the refractomotor should be kept In Its closed case. For practice or for checking erformance, distilled water is useful. .Hater has a refractive Index of 1.3330 at 20*0., 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 Aroolors - Typical Careful measurements at 25*C. have given the following typical values for Aroolors. * Aroclor 1348 Aroclor 1254 Aroolor 1260 Aroolor 1262 1.6295 1.6376 1.6460 1.6482 Substantial departures (over 0.0010) from these values should be in vestigated Immediately oe they - if correct - Indicate substantial error In the composition of the Aroclor or contamination with other materials. FAB:cm 1-27-45 Copied by re 4/23/48 . ` . . 0231783 f L, HARTOLDMONOOQ4877 Monsanto Chemical Company Anniaton Method Mo. 14-35-48 'JJBJECT; Resistivity of Liquid Aroclars METOOD; Resistance Measurements between Conductors Apparatus ' Megohm Bridge: General Radio Company Type 544B, AC operated - 500 volts, serial Mo. 171. ' This is a direot-current '/heatstone bridge for measuring high resistances, bridge balance being obtained thru use of a vacuum tube voltmeter. Range: 0.1 megohm to 10,000 megohms, covered by a dial and 5-position multiplier switch. A resistance of 1,000,000 megohms can be detected. . .. Test Electrodes: Two concentric nickel cylinders (or brass, nicksl plated) with feet. Obtained from General Electric Company. The inner eleotrode hae outside diemeter of 2.8" and height of 3.25", with area of 184 sq. cm. The outer electrode has inside diameter of 3" and like height of 3.25", with area of 198 sq. cm. The distance between electrodes is therefore 0.1 inoh or 0.254 cm. By theory the electrode constant, area/ length, is 191/0.254 or 752 where 191 is the overage area. In practice the cell oonstant supplied by General Electric Company is used. For the , / electrodes now in use, the cell constant lvas given as 815. - Glass Plate: Pyrex, about 3-1/2" diameter with concentric grooves to assist in spacing the electrodes. Obtained from General Electrio Company. Oven: Cenoo-DeKhoteneky drying oven with two holes in back wall for por celain tubes for lead v.lrea. Holes must avoid oven heating elements which occupy 2" paths vertically and horizontally intersecting at the center of the circular well. Lead "Vires: Provide 300 ohm Amphenol twin conductor cable to connect the eleotrodee in oven to the posts of the bridge. The portions exposed to oven temperature ore bared and then oovered with porcelain beads. Provide nl80 a flexible lead to ground the bridge tp a water pipe. Clean the leads, heads, and porcelain tubes Periodically. Assembly of Test Cell The grooved glass plate is placed in an 800 cc. beaker. The clean elec trodes are placed in the grooves of the glass olate with the connector posts dlreotly opposite in order to give the widest possible spacing to reduce surfaoe conductivity. The cylinders should be very clone to equidistant. The apparatus should be dried for 2 hours at 100*C. before use. . Heat the eample 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 electrodes. Care must be used to make sure tbnt the - 0231784 HARTOLDMONOOQ4878 SUBJECT: Resistivity of Liquid Aroolnra - Page ,, METHOD:___ Resistance Measurements betwoen Conductors lip of tho container, from which the liquid is poured, is clean. Tilt the booker in ouoh manner that all air bubbles in the Aroclor will rise to the purfuco. Air oool to 10S--104*C. then without removin'', thermometer, transfer to the oven which is maintained et 100*0. and connect the electrodes to tho two flexible wires which lead to the megohm bridge. '/lion the Aroclor comes to tempsrature (100*0.), remove thermometer, check cartaring of electrodes, end proceab to measurements. Measurement with Megohm Bridge Connect the two lead ivires to the megohm bridge with the lead from the outer electrode to the LO'J unknown post of tho bridge; the inner elec trode to tho unknown post. Connect the "ROUND post on the left side to a water pipe. Swing tho spring connector, pivoted on the "3TM post, to the L0 / post. Connoot the attachment cord to the 110 V power supply.' /1th the Aroclor ot 10C*C., turn the control knob (CUEOK-OPUR i'E-'U'iU'iG'.;- to the CHUCK position. Thro-; all 3 switches at the roar of the Panel i. ON. After 3 minutes bring the galvanometer pointer to zero by msaaa oi the ZERO iuXTUST knob. " Then turn tho control knob to CIIARCJE for one minute. Turn the knob to OPERATE and teturn the galvanometer pointer to zero by adjustment of the MULTIPLY BY switch and tho megohm dial. Read after one minute, Re peat the CHARGE and OPERATE positions for verifioetiou. The resistivity of the Aroclor is the product of the "multiply by" reading times tho dial reading times the electrode constant. Report in units of 10 ohm ora, rounded off to two significant figures. Example: , "Multiply by" reeding: 100 . Megohm dial reading 5.4 meg. ohms Electrode Constant 815 cm Resistivity 100 X 5.4 X 815 , > *> 4,4 X 10^ mag. ohm cm ' 440 X 10 ohm cm Values for reaistivity are roe lifted by designation of temperature end voltage. These are 100*0. ana 500 volts for the test above. Like con ditions are used at Plant B. 0231785 HARTOLDMONOOQ4879 SUBJECT;....Resistivity. of Llgulfl Aroclora - Po.p.e 3 I.r?moD: Resistance Measurements between Conauetors Caro of Apparatus The "Operatin'', Instructions", Central Radio Form 458-B, which accompany the megohm bridge, recite details of installation, measurements, uses, and construction, illustrated by figures and circuit and wirin'?, diagrams No attempt is made to reproduce such information here. The operator should acquaint himself vilth the contents of the O.R. manual and refer to It for maintenance of tubes and parts, .`hen not in U3e the megohm bridge should be closed and stored in cabinet. Clean Inc Electrodes . After the measurements are made the electrodes are removed from the tested liquid, and alloyed to drain, until the liquid stops running from the electrodes. V.'hile still hot they are placed in a beaker filled with benzeno under a well venlleted hood and allO'jcd to cool. 7hen cool., the electrodes are removed fron the benzene and scrubbed with povjdored tri sodium phosphate and a benzene carbontetrachlurlde mixture (50-50 by volume). This scrubbing cun bo done with either, a brush or the hands. The eloctrodes arc then rinsed with acetone, followed by tap viator and thin distilled mater. The electrodes should not be touchod by thi hands? after the acetone wash. after final rinsing the electrodes are placed in an oven at 120*C. for one hour or until thoy are used again. The glee8 spacer plates are cleaned and handlod in the sane manner as the electrodea except that they are wrapped in Ionso paper before being placed in the oven. Calibration For a rough check on the condition of the bridge, one or more cartridgotypo resistances of known approximate value should be kept on hand for periodic or emergency verification of the meter itself. rs 8/3/48 02il7b HARTOLDMON0004880 Monsanto Chemical Company Anniston Method No. 14-56-52 METHOD: Cleaning Dielectric Testing Cells The following mothod Is currently In use In Monsanto laboratories, for calls for the dlelectrlo testing of Aroolors, particularly the SB resis tivity cells. All steps up to (7) are performed with the oell assembled and in the beaker used In tests. ' (1) Drain cell while hot. (2) Fill with hot trloblorobenzene (TCB); heat for 10-15 minutes. (3) Dlsoard TCB from (2), fill with unheated TCB; let stand a few minutes, drain. (4) Rinse at least twloe with methanol, and twice with top water. (5) Fill with hot 10 to 12$ trlsodlum phosphate (TSP) solution, heat for 10-15 minutes, drain. (6) Rinse thoroughly with tap water. (7) Disassemble the oell, rinse the members thoroughly with distilled water. Dry at 120-130*0. for at least one hour. (6) If oell Is left In oven over 8 hours, It must be reoloaned Immediately before use. NOTES The TSP solution should be cheated to about 100*. The TCB should be heated to about 100 to 140*. I Hot TCB Is neoessary to cut Aroolor 1260o Other solvents, e.g., benzene oan be used on lower Aroolors. These suffer the handioap of flamablllty and lower boiling point. The second filling of TCB, from (3), may be saved for re-use in (2), provided the sample In the previous test was not too badly contaminated. The TSP solution should be made up fresh about every two days If In continuous use. If a thermometer Is to be used In stirring the Aroolor while heating, it shouli be oleaned by the method outlined above. Developed by: R. I. Good 9/84/52 0231787 HARTOLDMONOOQ4881 Monsanto Chemical Company Anniston Method No. 14-36-48 SUBJECT; Dielectric Constant of Liquid Aroclor METHOD: Measured at 100*0. and 1000 eyolsB 300PS This method applies to mineral oils and oil sahstltute used for Insu lating purposes. Apparatus Oapaoltanoe Bridge Cathode Ray Null Detector Osolllator Oonstant Temperature Oven -Jteslel!ltfttr--Ciiiiifrrnisi 1800 oo. Fyrez Beaker Renerel Radio Co., Type 716-AM ` General Radio Co., Type 707-A General Radio Co., Type 606-A ^ Ceneo-DoKhotlnslcr #95050 -/i . . ...Jlmisist^wmirCqTy^ypc Procedure Eleotrode and heaker mist be cleaned as dlreoted under "Cleaning Appa ratus for Dleleotrlo Constant", and be at 100C. Jt Heat Aroolor In the eaaeto 10S*C/ff Pour over electrode until plates and--- oaraml o-inenlatton are oovered. ( Cgmoot-leada^^stlr with thermometer outside oven until temperature reaches 101*1; plaoe in oven whleh-has been nn-nfnJ4y .ii-|.iua-a^t.n . At the time sample Is plaosd In oven its temperature should not have fallen below 90"C. Connect leads to capacitance bridge, observing that the lead from Insu lated side of oondenser goes to Insulated terminal on bridge. Balanoe. bridge oarefully eooordlng to direction under "Balancing Capecltanee Bridge". Until Aroolor and oven temperaturea have heoome Identical the bridge balance will constantly shift. After oven temperature reaohes 100*C., maintain bridge balanoe until no pronounced Shift Is evident. Record reading of capacitance aoale multiplied by multiplier setting. Dleleotrlo Constant Oapaoltance in Aroclor at 100C. Capeeltanee In air at 100*C. Balsnolng Oapaoltanoe Bridge Condensed procedure. Operator should read operating instruction for Null Detector for eomplete details. 1. Oonnset to power supply leads to osolllator and null detector. Ground the oscillator. 8. Turn on oscillator by pushing 5000 ohm, 10 multiplier, 100 oyole frequency buttons. Adjust harmonic control until oscillation begins as shown by eloslng of scoter in cathode ray tube. 023178B HARTOLDMONOOQ4882 Page #2 Dielectric Constant of liquid Aroolor - Test 14-36-48 1 . .. ,,, 3. On null detector turn brilliance knob to extreme left{ the focus knob to extreme right, gain control to extreme left, sweep amplitude et mid-scale position, the sweep frequency switch on line side. 1 4. Turn on power switch, lighting pilot light. ' 5. Visit fifteen seconds, turn brilliance knob to extreme right., ;"f (tS-l/t* U> l'-v- 'j: " . 6. Adjust foous and brillianee knobs until sharp fine line. 7. Connoot external terminals on detector to output terminals on osoillator. Switeh sweep frequency to external side. 8. Connect detector terminals of bridge to incut terminals of deteotor, taking care that the black wire (ground wire) of the lead goes to grounded terminal on both ends of lead. 9. Set gain oontrel at mld-sesle and selectivity to extreme left. Turn sweep amplitude to extreme left, Obtaining vertical line. :Uith 10. With turning oontrol knob obtain the maximum length of this ' line, keeping it always under 1/4. inch with gain knob. - . a 11. Set sweep amplitude to extreme left. ' / - . / ' J ' , / ` 12. Set gain oontrol to give vertical straight lino of about 3/8 lnoh. 13. Balanoe bridge by adjusting power factor and oapacltanoe dials until only a dot remains on the screen vhan the gain oontrol 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 elOBee into a straight line inclined to the horizontal. 16. Bring power-factor dial back to balanoe position, wbloh should restore the horizontal strolfftt line. Displace this control the same amount in the opposite direotlon. This should again tilt the straight line but in the opposite direction. Adjust phase oontrol 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 *3i7g9 HARTOLDMONOOQ4883 Page J)3 Dleleetric Constant of Liould Aroclor - Test 14-36-W8 oapeoitance Dial) must be in balance position. If the ellipse grad ually opens when the line is horizontal it nay be brought back to the line again by making slight changes in this oontrol. 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 oontrol will tilt the line which does not open apprecia ble thru an angle of 30 to the horizontal both ways; an alteration of the capacitance dial opens the ellipse but does not change the inclination of the major axis. The apparatus may be left this balanced condition, turned off by switching off first the brilliance knob of the detector, then the power switch, then turning off the oscillator. For successive measurements the controls are not changed, the apparatus left in adjustment. Then the following steps define the procedure: ' 1. Conneot all lends as previously directed including that from null detector to bridge. 3. 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 oxtreme left and adjust brilliance to Obtain a fine vertloal line on screen. 4. Briif this line to e dot by adjusting the two bridge controls. Initial adjustment is facilitated by having "Gain" control to left. Yihen final adjustment is obtained this knob must be at extreme right. 5. This dot remaining unchanged shows condition of bridge balance. Cleaning Apparatus for Dielectric Constant The condenser is removed from the tested dleleetrlo end allowed to drain while still in the oven at 100C. The condenser is then plaocd, while etill hot, in e beaker of benzene under a well ventilated hood and allowed to cool. It is then thoroughly washed with powdered trleodium phosphate and a 50-50 mixture of benzene end earbon tetraohlorlde 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 elean paper in an oven at 120*C for at least one hour or until it is again used. awb 3/1/46 0231790 m HARTOLDMONOOQ4884 Monsanto Chemical Company Anniston Method Mo. 14-42-48 ^OBJECT; Acid Number of Liquid Aroclors 1CTH0D: Titration with Alkali using Phenol Bed 3oope ( The Aoid Number Is the wolcht in milligrams of sodium hydroxide re quired to neutralize ono gram of Aroolor to pH 7.6, It thus includes any hydroohlorlo acid, ferric chloride, and other Inorganic or organic constituents having sold characteristics. It corresponds to the Neu tralization Number of ASTI.I Designation D188 except that the latter is expressed in terms of KOH Instead of NaOH and has a somewhat higher (phenolphthaleln) end point. Procedure To 100 ml. of adjusted (pH 7.6) solvent containing Indicator slowly add 0.1 N NaOH dropwlse until the color corresponds approximately to pH 7.6 when compered against a suitable reference solution. Readjust if necessary to maintain pH 7.6. Add SO grams (tig.) of Liquid Aroolor and mix well. Titrate from micro buret with 0.01 N NaOH until the original red oolor of the solvent is restored. A portion of solvent in a similar container is a useful reference in determining the end point. The mateh is governed by estimation of the Intensity of red because the hue is not exaotly reproduced on account of the yellow oolor Introduced by the Aroolor, 1 ml. of 0.01 N NaOH 0.4 Kgn. NaCH. Calculate in terms of Hon. NaCH per n. of. sample.- Report to 4 decimal places. PjL OrOQ-NaOH.*,.A . Ugn. NaOH/gm. g. of sample Example: If titration Is 0.08 ml. for 50 g. of Aroolor, the Acid Number is 0.08 X 0.4/50 0.00064 Kgra. NaOH/gm. Report as 0.0006. Solutions Required Solvent: Mix 600 ml. of benzol, 200 ml. of 5-A alcohol and 200 ml. of aoetone. Add 5 ml. of 0.2'/ phenol red solution. Phenol Red Solution, 0.255: To 0.1 gm. of dry indicator in a small, boulter add exactly 2.0 ml. of 0.1409 N NaOH. Stir to dissolve and dilute with 3-A alcohol to 50 ml. Reference Buffer pn 7.6: Dissolve 0.41 g. NanaP04 and 0.59 n. NaaHF04 (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 oolor standard is not available. 0231791 HARTOLDMONOOQ4885 Aoia Number of LIquia Aroolorg - 8 - Standard 0,01 N NaOR: 5 ml, of .5 N NaOB to 850 ml. vol. of 3-A aloohol. ProteeT at all times from atmospheric C0g. Note By using 250 ml. aoetone In solvent Instead of 800 ml. a 100 gm. sample of 1854 may be takes for analysis. FABiam 1-30-46 Copied by ra 4/83/48 i 02317 HARTOLDMONOOQ4886 Monsanto Chemleal Company ' Anniston Method No. 14-43-48 ' SPBJSOTt Color of Aroclor on N.P.A. 3cale LGTHOD: Helllge Pocket Comparator 3oope ' . The method la applicable to Aroclora 4465. 5460, or others having N.P.A. oolore In the range 1 to 5. Procedure . ." '.'.'arm the Aroolor la necessary to obtain pouring oonslstenoy. rill the test oup of the Helllgs Pocket Comparator, Model 605, with Aroolor, Insert oup In the comparator, and oompara against the oolor disc (No. 820C-50, Lubrtouting 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 oup with a mixture of CCI4 and benzol, with final rinse of benzol. ASTO! color numbers eolnelde with National Petroleum Association color nuiriber (1915). The relation of the N.P.A. oolor numbers to other color scales is tabulated below: NPA Color Nos. (1915) 1/4 1/8 3/4 1 1-1/8 8 8-1/8 3 3 -]/* 4 . 4-1/8 5 6 7 8 NPA Names s Lily white Cream white Extra pale Extra lemon pale Lemon.pelw Extra orange Orange pale Pale Light Red Dark Red Claret Red - Onion Petroleum Co. ^. - a H 1 j K L .K N 0 P c R A3TM Color Nos. -. 1 1.5 8 8.5 3 3.5 4 4.5 5 6 7 8 Lovlbond Analysis Red Tellow .Blue 200 510 1180 *> .* 0.18 0.60 8.5 4.6 6.9 9.4 14.0 81.0 35.0 60.0 60.0 166.0 0.6 1.1 1.7 2.4 8.0 86.0 87.0 38.0 45.0 50.0 56.0 1 93.0 60.0 106.0 64.0 m m ''- am .55 .55 .55 1.80 FABtom 1-86-43 Copied by rs 4/27/48 - HARTOLDMONOOQ4887 Monsanto Chemical Company t Anniston Method No. 14-44-48 SUBJECT! Color of "'.later Hhlte" Aroolors METHOD: Comparison against A.P.H.A, Scale 3oope The method is applicable to Aroclors 1254, 1260, or others having color less than N.P.A. #1 ("Vfeter White"). A.P.H.A. Standards '' Theso eolor standards are aeld solutions of potassium cbloroplatlnate and oobaltous ohlorlde. The unit of color is that produced by 1 mg. of platinum per liter. The ratio of oobalt to platinum may be varied if neoessary to match the hue. Because the hue of Aroelor 1254 and 1260 seems best matehed without'oobalt, this has been omitted In the prepara tion described. Dissolve 1.245 g, of potassium chloroplatlnate (KgPt01#) containing 0.5 g. of platinum In water with 100 ml. of concentrated hydrochloric acid, end 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 Tilth 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 Water and Sewage" eighth edition (1936) for details of standards containing oobalt. Published by American Public Health Association, 1790 Broadway, New York. Procedure 7111 a matching Nessler tube with Aroelor 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 surfaoe placed at suob an angle that light is reflected upward through the column of liquid. A color tube support (Fisher #7-065, 60 ml.) is convenient. Inasrmioh 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 parts per million. Colors up to 100 are recorded to tbs nearest 5. Dlreot comparisons are satisfactory up to 100. Above this the sample should be diluted with Carbon tetraohloride (maximum A.P.H.A. color, 6), and the oolor obtained to nearest 10 by multiplying by the dilution ratio. ( FABtem 1-30-45 " ` ' by re 0231794 HARTOLDMONOOQ4888 Monsanto Chemical Company Anniston Method Ho. 14-46-46 > SUBJECT; Acid Humber of Solid Aroclars and Heavy Liquid Aroclors UBTHOD: Titration with Alkali using Phenolphthaleln Procedure Dissolve SO grams of the Aroolor In SO 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, phenolphthaleln solution, and titrate, In the case of the distilled Aroolors with 0.01 N sodium hy droxide solution, to a faint pink color whloh 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 es milligrams of sodium hydroxide required per gram sample. Calculations Using 0.01 H HaOH, Add Ho. ml. titration X 0.4/sample weight For SO gm. ~ Acid Ho. >(.111. tit. ml. blank) X 0.008 Using 0.1 H HaOH, Acid Ho. ml. titration X 4.0/sample weight For 50 n. Acid Ho. (ml. tit. - ml, blank) X 0.08 Apparatus 10 ml. burette In .05 divisions. Conversions 1. To obtain neutralization Humber in terms of KOH, multiply the Add Nurfber In terms of HaQH by 1.402. Inverse factor Is 0.713. 2. Multiply the Add Humbor by 1000 to obtain the parts of NaOH re quired to neutralize ono million parts of Aroolor. Thus Add Number of 0.0006 Is equivalent to 0.6 parts of HaOH per million parts of Aroolor. 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 oarried 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 HaOH consumption, ferric ohlorlde whloh Is usually present In small amounts, also consumes NaOII in neu tralization to phenolphthaleln. It therefore.follows that an Aroolor of very low add number must be also extremely low in ferric ohlorlde. FABtom 1-26-45 Copied by rs - 4/27/48 07317^ HARTOLDMONOOQ4889 Monsanto Chemical Company Anniston Method No. 14-47-48 SUBJECT: Pour Point of Liquid Aroclore METHODl A.3.T.M, D-97-39 __________ The pour point of an Aroolor Is the lowest temperature at which the material will flow when it Is ehllled under oertaln. prescribed condi tions .listed In A3TM D 97-39. . Apparatus - ' Apparatus oonsists of test jar, thermometer, cork, Jacket, disk, gasket, end bath as described under A.s.T.M. method D97-39. The thermometer Is the A.S.T.M. Cloud and Pohr Test, range -38 to 50*C. Present apparatus is the Emil Greiner Co. #G8 8834 single unit with Or2242 test jar. Procedure for Aroolor Follow D97-39 In all respeots except that the centigrade seals Is sub stituted. Only on outline follows: Add 40 ml. of Aroolor to test Jar. Adjust thermometer to center of Jar with beginning of capillary 1/8 inch below surface of the Aroolor. '..'arm the Aroolor without stirring to 46*C. In a bath at iB-iB'C. Cool to 32'C. In air or water bath at 25*0. Trans fer the jar to the jacket of the cooling bath which Is maintained at 0 to 3*0. Beginning at a temperature 8 to 10 degrees above the pour point, at each Interval of 2*C., romovt the test jar from the Jacket and tilt just enough to detemlne If there Is movement of the Aroclor. This Inspection should not require more than 3 seconds. '.Then 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 8*C. lower. Continue the test In steps of even degrees centigrade (14,12,10, etc.) until the Aroolor shows no movement when the test jar Is held horizontally for exactly 3 seoonds. 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 wKIcET the liquid will flow or pour under the test conditions. Technicians must familiarize themselves with D97-39 which gives complete details of apparatus and procedure, reproducibility of results, effects of thermal history, etb. The directions above are inadequate except as a working outline. The bath temperature Is controlled by adding dry Ice to acetone for pour points below 0*C. FABtcm _ 1-30-45 Copied by re - 4/27/48 Ogj, 6 HARTOLDMON0004890 Monsanto Chemloal Company . Anniston Method No. 14-46-48 SUBJECT: The Testing of Aroolors for Inorganic Chlorides METHOD:_______ __________ _________ Solutions Reoulred Standard Chloride Solution: Dlssolvo 0.660 grams of pure sodium chloride In sufficient water to measure exactly 500 ml.} 1 ml. then contains 800 mlorograms Cl. Pipette 85 ml. of this solution to a 500 ml. flask and make to the mark to give a*0.00115 M NaCl solution, 1 ml. of whloh con tains 40 mlcro&'ams of Cl. Preserve In a Pyrex bottle. Caution: The water used in preparation must be chloride free by the Tyndall Beam test; the 0.00113 M solution should not bs kept over 1 month. Silver Nitrate Solution 10$: Dissolve 5 grams of sliver nitrate orystals In 40 ml. of water and add 10 ml. of concentrated nitric acid. Chloride free distilled ''ater. Apparatus Required Lalfotte 10 ml. oolor tubes (13 mm, X 100 mm). Test tube raok with a blaok surface at the base for uniform comparison (Note: we are using blaok 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 oolor tubes. It la just high 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 aocomodate at least seven tubes. Method Clean all flasks, tubes, and pipettes to be used. Then rinse with dilute nitric add then with chloride free distilled water. ./ ' Add 50 ml. chloride free water to a 850 ml,'iErlenmeyer flask, heat to boiling, add 800 gram of the Aroelor to be tested, which has been heated to 100C, shake vlgorouely for 1 minute, cool in cooling pen. Carefully decant some of the water extract to a separatory funnel. Wash with pure ethyl ether (ohlorlde free). Transfer 10 ml. of the ether washed extract to a 10 ml. Lelbtte color tube after rinsing tubs with portion of extract. Prepare standards by diluting exactly 5 ml. of the 0.00133 M NaOl solution to 100 ml. In a HARTOLDMONOOQ4891 The Teat lag of Aroolors for Inorganic Chlorides - 2 - volumetrio flask. One ml. then oonteins 2 mlorograms of Cl. Transfer 1, 8, and 3 ml. portions to 10 ml. tubes, Kake to the 10 ml. mark with Cl free HgO. Place standards and sample In light free box from whloh only the top of tubes are exposed add 0.5 ml. of the silver nitrate to eaoh tube compare In a specially prenared test tube raok. The comparison is to be made quickly and from a oonstant source of light, preferably day 11edit from a window away from the sunlight. Comparison le. easier when other sources of light are shielded from the comparison ' raok. Look dlreotly into the top of the tubes and compere. Rote the known solution which most nearly mutches the rater extract estimating to the nearest whole mlorogram. The extract blank and the distilled water should show no turbidity. Calculation' Divide the chloride content In micrograms of the known solution whloh matohes the extraot by the weight of the Aroelor represented by the extraot to obtain the chloride content of the Aroelor In p.p.m. In the procedure described, the 10 ml. extraot represents 40 grams of Aroolor (1/6 of 200 g. taken). The three knowhs contain 2, 4, and 6 mlorograms of Cl, thus representing 0.05, 0.10, and 0.15 p.p.m. respec tively. Values should be reported to the nearest 0.025 ppm. Precautions , Because of the sensitivity of this tost, serious errors may result through very slight contamination or inattention to details. All equip ment must be scrupulously cleansed, the distilled water absolutely ohlorlde free and testing done away from fumes of HC1 or ehlorlne fumes. 4/27/48 0231798 HARTOLDMONOOQ4892 Monsanto Chemical Company Anniston Method No, 14-53-48 SUBJECT: V.'ater Content of Liquid Aroolora METHOD: Titration with Karl Flsoher Reagent Outline "" t The Aroolor la dissolves In a mixture of benzene and methanol which has been titrates with Flsoher reagent to the characteristic end point. Flsoher reagent is a solution of Iodine, sulfur dioxide, and pyridine. Iodine is oonsumed as long as any water Is present. The solution Is again titrates to Obtain the water content Introduced by the Aroolor. Solutions and Apparatus Karl Flsoher Reagent: flelgi Into a flask 864 grams of pyridine, Barrett 8-A or Eastman 214-H, and add 51 grams of liquid or gaseous sulfur dioxide. Add the liquid sulfur dioxide directly from the inverted oyllnder by attaching to the outlet valve a glass tube extending Into the pyridine. Sulfur dioxide gas can be bubbled into the pyridine until proper amount Is added. Store In a glass stoppered bottle. . Transfer 65.6 grams of the pyrIdine-SO mixture and 134 ml of absolute methanol to a 1 liter Florence flask. Cool thoroughly in an ioe water bath. Add 16,9 giems of Iodine, stopper, eool 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 84 hours before using. When fresh, one ml of reagent Is equivalent to about 0.0033 gras, of water. Aroolor Solvent: Mix 8 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 XOp to come over. Keep In glass stoppered bottles with minimum exposure to air. Kloro Buret: 10 ml. x 0.05 ml. Koch automatic with glass stoppered reservoir. Eek and Krebs #8460. Equip reservoir with a moisture guard tube containing Drlerlte or a similar dehydrating agent. Procedure Heat a clean 500 ml. narrow mouth Erlenmeyer flask In an oven or on hot plate until thoroughly dry. Sweep out for 10 minutes or until cool with air which has been thoroughly dried by pesBlng thru tubes containing 6 mesh Drlerlte. Disengage the flask from the aspirating train and imme diately close with a paper oap held by a rubber band. 0231799 HARTOLDMONOOQ4893 Water Content of Liquid Aroolore - 2 - Without delay, transfer 100 ml, of the benzene-methanol solvent to the flask thru a email hole punctured into the paper cap. Cover again with paper. Titrate at once with Karl ?lsoher reagent to dlstlnot red-brown end point which does not fade after swirling several times. The Fischer reagent la dispensed from the mloroburet the tip of which projects Into the flask thru the puneture In the paper cap. At the end point any water content of the solvent has been reacted. Superimpose a fresh paper cap . immediately. ' Obtain weight of the solvent and well-covered flask on a Torsion balance or equivalent. Qplokly lntroduoe with a dry pipette about 100 grams of the slightly warmed Aroolor to be tested. Cover at once and weigh again to obtBln the weight of Aroolor to nearest gram. Shake until the Aroolor la dissolved. . If the mixture is Cloudy, warm sllehtly. If cloudiness persists another mixture should he prepared. Punoture a small hole In the paper cap for the insertion of the buret tip and titrate with Fischer reagent to the first definite brown oolor, agitating with a gentle swirling motion. The end point should persist through several swlrle. The end point may slowly fade through slow acoess of stmospherlo moisture In whloh ease it la restored by a drop or two of reagent. If not so restored, the end point may have been a false one or the eloaure Is faulty. A definite end point Is impossible If humid air Is not well exoluded. From the amount of reagent required and the weight of Aroolor used, cal culate the water content In p.p.m. Calibration of Fleoher Reagent and Standard 'Jeter Solution Standard water solution In methanol: Transfer exactly 0.40 ml. of water from a micro buret or a 1 ml. measuring pipet to a 100 ml. volumetric flask. Fill to the mark at onoe with anhydrous methanol and mix. One mi. of solution then contains 4000 mloro-rams of rater In addition to any water Whloh may be present In tbe methanol. - Transfer exactly S ml. of the above standard water solution (equivalent to 0.02 grams of water) to a 2B0 ml. Erlenneyer flask which has been dried and swept with dry air. Close with paper cap and titrate with Fleoher reagent In the same manner as the sample. The end point Is sharp. A methanol blank, found by titrating 5 ml. of the methanol used In making up the standard water solution to a like end point, must always be subtreoted from this titration. Divide the eraount of water taken by the -net Fischer reagent required to obtain the titer of tbe Fischer reagent in terns of water. Example: A 5 ml. aliquot of standard solution, equivalent to 20,000 mlorograms of water, required 6,61 ml. of Fischer reagent while 5 ml. *3l800 HARTOLDMONOOQ4894 Water^Content of Liquid Aroolors - 3 - of the methanol retired O.SS of Fischer reagent. 20,000/(6.61 - 0.55) - 20,000/6.06 . . ' m 3300 micrograms water/ml, - Reoallbratlons: Because the Fischer reagent deteriorates rapidly, Its titer must he determined for each days use. If the same standard inter solution Is used In reeallbratlon as in the Initial calibration, the titer of the Flsoher reagent must be calculated from Its total water oontent (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 micrograms. If on reoallbfatlon 7,37 ml. of Flsoher reagent is 21813/7.37 2960 ralcrograras of water per ml. Two or more calibrations should be made with agreement within 0.025 ml. Calculation of HgO sample . Standardization of Standard HgO sol. Titrate 5 ml. mixture HgO sol. Titrate 5 ml. of methanol Tit of 5 ml. mixture A Tit of 5 ml. methanol B . A - B - ml. reagent for HgO added - 5/100 of .4 Divide 5/100 X .4 by A - B faotor grams of HgO/ml. Hultlply faotor X B giving gms. of Hs0 In 5 ml. of methanol. Add this wt. of HgO to .02 already added glvlis HgO in 5 ml. (Total) Factor _T HgO St'd Titration 1 T^ X sample Titration Ts Tg X 1,000,000 ppn HgO wt. sample FAB: cm 1-27-45 Copied by rs 4/27/48 0231601 HARTOLDMONOOQ4895 JlVToPIAL HOUSER From 1 FR0PMITIE5 OF BASIC "HAIXTAY" FHOOCCTS Letter to U.C.:.T./*J.T.Bolaer (Halowax Products Div..Union Carbide and Carbon Corp,,, 30 C. Forty-Second St., N.F. 17, HoY.)o Letter dated Feb. 27, 1948. Ho. 1000 Ho. 1001 j Ho. 1013 . vqa 1014 . C<>lOPS P'.ow Point ('fed, ASTII Softening Point) de<*. F. S.acifio Gravity at 77 dee, F. White to Pale Straw Ohite to Pale Felloe Pale Fellow Linu Id 194-201 247-252 1.19 - 1.25 1.53-1.59 1.65-1.71 Pale Fsllo* 277-283 1.75--1.PI Penetration (Pod. AST2T) 200-e. load at 77 dee. F= 10-15 5-8 5-8 Viscosity (Saybolt-Universal Seconds) Dltit illation Renee (AST:;) dee. F, 7`eeh Point (AST!! Cleveland Open Cup) dee. F, 33-37 at 77 derr* F* 33-37 at 266 de*. F. 31-35 at 266 deg.F,. 33-37 at 302 de^.F.' 480-590 600-650 615-655. 6P0-730 203 284 356 392 File Point (ASTU Cleveland Onen Cup) der. F. p-iwer Factor at 1,000 cycles at 10 cycles r ilectric Constant at 1,000 cycles et 10 cycles 0 C, Resistivity (nep;. cm.) at 30 deft, C. 338 ' --- --- _ -- -- None to boiling Less than 0.8? 0.43 Hone to boilino: Less than 0.3? 0.70? Hone to boll in*' 1 Less than 0.1 j 0-70 5-6 5-6 Owr 107 - 10 4-5 4-5 4-5 4-5 _ Over 107 - 108 Over 1C7-108 ... Copied by swb 4/2/48 0231802 HARTOLDMONOOQ4896 From - Halowax Products Division Union Cartolfle and Carton Corporation 30 Hast 42nd Street New York 17, New York Letter - V/.C.M./J'.M. Cole, Tech. Sep. e/16/48 Zyrox 3009 (11-313) GENERAL INFORMATION Color 3p. Gravity Softening Pt. Stonier Viscosity SaytoIt Furol Viscosity Penetration at 50*C. Penetration at 25*C. Flash Pt.' Fire Pt. Combustibility Fracture Acid Resistance Alkali Resistance ' Volatility ' P.F. at 25*C. (1000 cycles) Dial. Constant at 25*0. (1000 cycles) DO Resistivity at .25*0.- - Brown - 1.40-1.45 at 25*C. - 79-83C. - 59-89 at 130*C. - 79-180 at 130*C. - Approx. 15 (200 gm. load) - Less than 3 (200 gm. load) - Approx. 590*F. - None to 600* F,, - "Jill not support combustion - Conchoidal - Excellent - Excellent - Average for 24 hours at 130*C. Less than 0.10 mg./s^.om./hr. - Approx. .001 - Approx. 2.96 - Over 108 meg. ems. Copied by rs 4/2/48 0231603 HARTOLDMONOOQ4897 From - Halcwax Products Division Onion Carbide and Carbon Corporation 30 Fast 42nd Street New York 17, New York , ' Letter - ;,C.tl./J.!I, Cole, Teoh. Rep. 2/16/48 Zyrox 3007 (11-308) GENERAL INFORMATION Color Sp. Gravity 3oftenlng Pt. Stormer Viscosity Saybolt Furol Viscosity Penetration at SO doc. C. Penetration at 25 dee. C. Flash Pt. Fire Pt. Combustibility Fracture Acid Resistance Alkali Resistance Volatility P.F. at 25 deg. 0. (1000 cycles) Dlel. Constant at 25 deg. C. (1000 eycles) ' DO Resistivity at 25 deg. C. - Brown - 1.29 - 1.32 at 25 dee. C. - 65 - 70 deg. C. . - 20-27 at 130 deg. C. - 20-30 at 130 deg. C. - Approx. 75 (50 g. load) - Less than 3 (200 g. load) - Approx. 530 deg. F. - None to 600 deg. F. - .'ill not support combustion - Concholdal - Excellent - Excellent - Average for 24 lire, at 130 deg. C. tf.TSO mg./sq.cm./hr. - Approx. .004 - Approx. 3.0 - Over 10 meg. cms. Copied by rs 4/2/48 HARTOLDMONOOQ4898 HARTOLDMONOOQ4899 HARTOLDMON0004900 HARTOLDMON0004901 .' , From: B.1.0.3. Final Rapt. APPENDIX II . PHYSICAL AND CHEKtCAL PROPERTIES OF CL01WM OILS Item Nbs. 1, 7, 22, & 31 . Pages 108 - 109 (as quoted in I, 0. Farben* s sales sheets) Property Clophen A30 Clophen A40 Clophen A50 Clophen A60 Clophen A70 Clophen A80 Form .. .. .. .. .. .. .. Colour.......................... .. .. .. Specific Gravity at 20*C .. .. Solidifying Point .. .. .. .. Flash Point* .................................. Shrinkage: 100* - 20*C .. .. 50* - 20*C .. .. Viscosity at 100*C ........................ . Soiling Point Limit at 12am. of ISercury .. .......................... Loss during Evaporation (after 6 hours at 100*0} .. Liquid Liquid Nearly colourless Nearly colourless 1.36 1.48 -18*C -5*C 166* 193* (Pensky -- Kartons) 6J5 3$ 1.1*5 6$ 1.2 *E 165 - 195* 180 - 215* 0.05$ 0.03$ Volatility at 20*C .. .................. (1mm. of Kercury for 100 hours) Heat Conductivity at 40*0 (in Calories per metre per hour per *C). Saponification No............................ .. <0.009$ 0.095 0.0 <0.009$ 0.091 0.0 Liquid Liquid Nearly Nearly colourless colourless 1.55 1.68 12*C 30*C 222* 236* In an open crucible 6$ 3$ 1.5*5 ' 6$ - 8$ 1.9*5 Firm Nearly colourless Firm, crystalline Thite 1.7 1.72 - 1.77 50*C >160*C 240* 290* or over (Pensky - itartens) 5-6$ 355 . -- 4*5 - * 190 - 230* 195 - 250* 200 - 255* 210 - 260* 0.02$ <0.009$ <0.01$ <0.009$ 0.01$ <0.009$ 0.0 (2 hra. at 125*) <0.009$ 0.087 0.086 - - ' 0.0 0.0 0.0 0.0 Ash . ................................ .. .. Permittivity at 20*C .. .. .. Power Factor .. .. .. .. .. Breakdown Strength .......................... Insulation Resistance in Ohm .cm. V. small 6.0 <0.001 . 200kV/em. 1 X 1013 V. small 5.4 <0.001 200kV/era. 1 X 1018 V. small 5.0 <0.001 )F200KV/ora. 1 X 1014 V. small 4 - 4.5 V. small 3.0 <0.001 <0.001 > 200kV/om. - >11 1014 >1 X 1014 V. mail 3.0 - >1 X 1014 Clophens ere not combustible and do not support combustion of materials into which they are impregnated. oi-a-v-i 0231606 HARTOLDMON0004902 H4HLE i Pron - United 'States Patent 2,070,368 Patented February 9, 1937 Pass 2 1-------2 .-------3-------4-------- 5-------6-------- Hydrocarbon compositions Di phenyl Dis tilled high bo 111ns com pounds Percent 0 0 80 80 50 50 Percent 100 100 20 20 50 50 Properties of dielectric Chlo-- . rine content Percent 23.9 40.3 41.2 52.2 42.0 36.4 Viscosity see. laybolt at 210* F. Seeclfie grarlty at 65*/65* C. 63 290 35.7 47.5 48.8 40.8 1.251 1.405 1.352 ' 1.490 1.383 1.324 Dielectric constant K at 100* C. (1,000 cycles) 4.35 4,98 4.87 4.56 4.84 4.89 Properties of chlorinated diphenyl MH <71 Ul ^ u 00 -a 7-------8-------- 100 100 0 54.0 0 42.0 46.0 34.0 1.523 1.380 4.30 4.80 o u> Copied by rs 2 2/2/48 -I-A. (b) (g) B (a) 300, 2100 HARTOLDMON0004903 I-A (j) - 500 Stability of Grade P Hycar end Teflon In Aroclor 1254 at 130*0 and 45*C 3hort Form Report No. 8179 File No. 141-87.1 December 89, 1947 Notebook references: Smith 45137 Grade P Hjroar and Teflon Immersed In Aroclor 1854 Material Temp, Hours 5? Oeln In 7t. Gain In Thickness Grade P Hycar Grade P Hyoer Teflon Teflon 130*0 45*0 130*0 45*0 885 885 885 285 68.6 86.3 Negligible Negligible 86 6 Negligible Negligible rs 1/14/48 023181 HARTOLDMON0004904 I-A-l - 500 ( From - Memo P.O.B./R.L.J. 3/S2/48 Aerovox Corporation New Bedford, Massachusetts Determining Fluorescence In Aroclar "The ultraviolet light we use for determining fluorescence In ' Aroolor Is manufactured by George :!. Gatos end Company, Franklin Square, lone Island, Hew York. It Is a CB 4, 100 Watt, G. E. Mazda lamp with filter. . "Our procedure la to pour a small amount of Aroclor Into a 5" watch glass or a 5" Pyrex evaporating dish and observe for the degree of fluorescenoe 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 fluorescenoe around the meniscus of pure Aroolor Is not to be confused with the fluorescenoe resulting from contamination. ( "This test Is qualitative and, as such, Is based on the experi ence of the person performing It. We keep a standard sample for comparison. If there are any further questions please feel free to contact us". Copied by rs 4/3/48 ( ^3181! HARTOLDMON0004905 TB - 100 ( December 2, 1947 ELSOmiCAL DATA ON AROCDOR3 Introduction Time baa not permitted us to oerry 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 oonstant, loss factor, and dlreot current resistivity measurements over, a temperature range for a lov> chlorinated and highly chlorinated biphenyl; also one sample each of the terphenyl and the . mixed biphenyl and terphenyl series would represent the electrloal be havior of Aroolora. The trend of the eleotrlcal properties of the samples not measured can be estimated; l.e. as the viscosity of the Aroclors of a particu lar series Increases, the loss factor will decrease and the loss faotor maximum (If within the temperature range meusured) will be shifted to higher temperatures. An Increase In vleeoslty will Increase the resls- . tlvlty of the Apoclor. The dielectric constant of a material is a measure of Its polarizability. Therefore, any change In the structure of the noleoule which will Increase Its polarizability will cause an <' increase In dielectric constent. Accuracy cf Data The accuracy of the alternating current data Is dependent on the dissipation factor of the dleleotric at a particular frequency and a particular temperature. The dielectric oonstant values are acourate within .2$ provided the dissipation factor Is less than 10$. The error la greater with Increasing dissipation faotor. The eccuraoy of loss faotor (dleleotric constant X dissipation faotor) Is also dependent on dissipation faotor. Aroclor 5442 was the only sample which had a dis sipation faotor neater than 10$ and that ocourred at the following conditions: 41*0, 500 cycles 41*C, 750 cycles 35*C, 500 cyoles It will be noted that the dielectric constants extrapolated to 100*0. oheck satisfactorily with the values listed In your letter to Dr. Bump. The direct ourrent resistivity values have a 30$ error for the greatest resistance readings on our Instrument. For lower resistance values the error decreases. Aroclors 1221, 1254 showed an increase In resistance with time which Is Indicative of polarization effects. For these materials then, resistance wes read after the voltage was applied end then at the end of one minute - an emplrioal method used for talcing a readable value. Aroclors 4465 and 5442 did not show noticeable pola- 0231812 HARTOLDMON0004906 -8 - IB - 100 December 2, 1947 rlzetlon effects, even at the higi temperatures. Data The dleleotrio oonstant of Aroolor 1221 and 1254 la Independent of frequency. The dlelectrlo oonstant of Aroclor 4465 and 5442 Is also Independent of frequency at the high temperatures. The llquld-llke properties of 4465 and 5442 disappear at the lower temperatures where a dispersion region becomes evident. It will be notloed that the dielectric constant curves (at the lower tempera tures) have the same order as those of the corresponding loss faotor , curves and the Inflection regions occur at the loss faotor maxima tem peratures . ' The loss factor curves of 5442 at the higher temperatures show a sharp up-swlng, Indicative of a large conductance component In the loss faotor. Similarly, the loss faotor curves of 1221 and 1254 seem to be In the conductance region. Aroolor 1221 showed an unusual sensitivity In changing loss faotor values and as great an Insensitivity to change In dlelectrlo oonstant. It was found that a sample measured Initially at room temperature end 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 faotor, probably volatilizing the more Conducting or the hlgi loss substances In the Aroclor. Below 5000 cycles this effect was very noticeable, the diffe rences Increasing with decreasing frequency. It may be mentioned here that loss factor measurements at low frequencies might possibly be used as an analytical tool or as a control method of Indicating volatile sub stances contained In the Aroolor 1200 series. The log resistivity versus 1/T graph Is useful as an Indication of the change that occurs In resistivity with temperature - or what Is related, the change In vlsooslty 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 Aroclora have a muoh larger vlsooslty-temperature coefficient than the other two plots. It is hoped that the enolosed -rephs will summarize the dielectric properties of the Aroelors measured, llore complete Information or any questions concerning the data will be sent on request. aom/ . Copied by re 1/15/48 R. Levreault Monsanto Chemical Company Plastics Division Springfield, Uassachusetts ' . 0231813 HARTOLDMON0004907 *0 DATA ON AROCLOR 12*2 FKXX FOUND AFTER TALKING WITH YOU. f o- RESISTIVITY 50 DECREE C. *200 X 10* 100 DECREE C. 2*00 X 10* 150 DECREE C. 1800 X 10* "O A N ELLENBURC " MONSANTO " ST LOUIS *C 023181* 0 I HARTOLDMON0004908 i! 'Tfesis-f-itify A* IM.i .co s ,co*>& HARTOLDMON0004909 HARTOLDMONOOQ4910 0231816.01 /r,p(:rW<,re HARTOLDMON0004911 HARTOLDMONOOQ4912 II-B From - B.I.O.S. Final Report No. 893 Item Nos. 1, 7, 22, and 31 Pages 12, 13, 14, 15, 16, A 17 III. CHLORINATED DIPHENYL. ' 1. General. Chlorineted diphenyl is manufactured by I.O, Farben under the trade name of Clophen, Some types are liquid and otbers solid at normal temperatures. They are used as lmpregnants as alternatives to hydrocarbon oils and waxes. Clophen shares with other chlorinated materials a high permittivity and has the same dangers in handling, due to noxious properties. In addition to the grades suited to capacitor impregnation, a grade known as T64 is made by I.G. Farben, suitable for trans former cooling. The total output of Clophen A50 and A60 for the years 1938 and 1943 was:- 1938 Type A50 81 tons " A60 132 " 1943 " A50 170 " " A60 506 " The cost of the material in Germany iss- Type A50 1M, 50pfg.to 1M, 60pfg. per Kilogram " T64 ill. 20pfg. per Kilogram. The following is a list of the principal prewar consumers of Clophen:- Siemens-Schuekert, Berlin. A.E.O. (Hydrawerk), Berlin. THoafll (Brown Boveri), Zurich, Switzerland. Alsthom, Paris. Duoatl, Milan, Italy. ; *. It was stated that no German capacitor manufacturer uses Clophen for the manufacture of small capacitors for radio and telephone purposes and where these have been used by the Ger man fighting services they were supplied by the Italian firm, Duoatl. ' 2. Manufacture. (1) The synthesis of diphenyl from benzene. Diphenyl is synthesised from benzene as shown in the figure, following: - 0231816 HARTOLDMONOOQ4913 St -VWV-- Condenser Distilling < '4 Column > 500-650*0 , 800*0 < Two-stage S Heat Exchanger Reaotion Coil . 800*C Synthesis of Diphenyl from Benzene The synthesis occurs In the vapour phase, at 800*C. and atmospheric pressure, in an electrically heated reaction coil of copper-manganese alloy. No catalyst is required. The apparatus, apart from tbo reaction ooll, Is of iron, and operates at the temperutures shpvm above. About 10$ of the benzene vapour Is converted Into diphenyl In one passage through the reaction coll. The purity of the benzene Is of Importance for the elec trical quality of the ultimate ohlorlnated produots and a specification Is attached overleaf. The benzene used was believed to contain 0.2 to 0.3$ of paraffins but little definite Information could be obtained regarding any undesirable Impurities or tho mechanism by whioh they cause poor electrloal performance. Thiophene was stated to be definitely harmful, and vague reference was made to "nitro-oompounda", to "aliphatic hydrocarbons" and to "substances which could not be chlorinated". The precise nature of these materials was not known, but their absence was ensured by obtaining benzene always from suppliers whose product was known to be satisfactory. Analytical Specification for Pure Benzene Appearance! Clear and colourless. Density at 20*0.; 0.876 Distilling range: First 5$ within 0.25*0. 5$ - 95$ " 0.25*C. 95$ - end " 0.25*0. Solidification point: Not less than 5*C. Bromine consumption: Not more than 0.5 gm. bromine per 100 c.e. Sulphuric acid test: Not more than 0.15 gt, KeCrgO^ Carbon disulphide: Shall he free from CSg. 0231819 HARTOLDMONOOQ4914 Difficulty in the synthesis wao still being experienced, due to rapid corrosion of the copper-manganese reaction coll, operatin'! at 800*U. A small scale experimental apparatus using a fused silica coll had been made, but bad not been developed for production use. In addition to diphenyl, about 5# each of 1-3 and 1-4 terpbenyls are produced by the process. These are se parated, chlorinated and used in sealing varnishes; present production is about 4 tons per month. Ho use Is made of chlorterphenyls as paper lmpregnants, since the materials are resinous and tend to crack; moreover the permittivities are lower than those of the chlordlphenyls. 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 vaoue, yielding 1-4 terphenyl with melting point of 208*0. The 1-3 isomer, remaining In solution In benzene. Is more difficult to Isolate. The solution Is clarified with activated char coal, filtered, and the benzene evaporated. The residue Is distilled to yield 1-3 terphenyl with melting point 80-84*0. (2) Chlorination of diphenyl. For the chlorination of diphenyl a lead lined vessel of 10,000 litres capacity is used. It is charged with 6000 kg. of diphenyl and 15 kg. of ferric chloride. The mix ture Is heated to 110*0., agitated and chlorine passed in. The addition of chlorine Is continued for 100 hours at a rate of 130-135 kg/hour during which time the tem perature Is raised gradually from 110*C. to 150*0. The end point of the chlorination is determined by measuring the density of the product. To remove hydrogen chloride formed In the process, dry air Is blown through the liquid for 2 hours and this hy drogen chloride le recovered. The product is transferred to another vessel and treated with 1/2# of solid sodium hydroxide, heated end agitated. The sodium hydroxide is allowed 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 procsss are gas heated. 0231820 HARTOLDMONOOQ4915 Propart lea, (1) Capacitor lmpropjatiir> grades. A summary of the physical end chemical properties of the capacitor Impregnating grades of Clophen Is given In Appendix n. There are six grades of capacitor lmpregnont, A30, A40, etc. up to A80, the 3, 4, 5, etc. indi cating the number of chlorine radicals combined with the diphenyl. Each grade contains a proportion of the adja cent homologuas not exceeding 20$. Grade A30 has the highest value of permittivity. Theoretically the highest value obtainable -with a chlorinated diphenyl is 9,0, and a grade having a permittivity of 7.0 has been prepared, but is chemically unstable, and very sensitive to moisture and Impurities. The most commonly used grades are A50 and A60; A90 Is the most stable grade and has the lowest dielec tric loss. Grade A60 Is considered by 1.0. to possess the . optimum combination of non-lnflammabllity, stability and viscosity. As with Nlbren, It Is considered that no addi tives are required since the substances are stable In use, provided that the capacitors are efficiently sealed against the air. Klcufil of Zurich are the only users of A30 and A40. The following table shows the variation In eapaoltanoe and power factor with temperature for a Clophen Impreca ted paper capacitor. The lmpregnant Is A50, the dloleotrlc Is Schoeller and Eoesch "A" finish rag tissue (density 1.2 - 1.25) with a thickness of 10 u; frequency of measurement Is 800 e/s. Power factor shows a maximum value of 0.052 at about +4*0, while eapaoltanoe falls off by soma 20# at temperatures below this orltlcal value. Variation In capacitance and powcr-factcr with temperature for a Clophen-impregnated capacitor. ' Temperature (C.) -60 -40 -20 0 4 +20 +40 60 80 RelativeCapacltanoe 0.87 0.91 ' 0.94 . 1.02 1.06 1.10 1.10 . 1.10 1.11 Power Tactor 0.035 0,024 0.013 0.048 0.052 1 0.006 0.005 0.004 0.005 Ko 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. 0231021 HARTOLDMONOOQ4916 The method adopted fop evaluating the water content in oils such as Clophen Is described in Appendix III, It is also applicable to 3uch solids as Nlbren, Engelhardt stated that no source of failure had been ex perienced during the vhole 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, (8) Transformer-cooling grade (Clophen T64). No detailed information was sought on this material, since it is unsuitable as a capacitor impregnant and is onlyused as a coolant tor transformers and phase shlfterso A summary of its physical and chemical properties is given in Appendix 17. It has a low vlseoslty, is moderately stable under electrical stresses and has the distinct ad vantage over mineral oils of being non-inflammable. The principal users of this produot are A.E.G. and Siemens, but it is understood that, as with other chlorinated eastpounds, conservatism and prejudice among customers have prevented its wider use. No 8tahllisera are added to the material as their function of absorbing hydrochloric acid would be defeated by the * formation of "chloride salts", which in turn beoome elec trolysed. It was said to bo very important to avoid contamlnatlon 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.O. for the construction of test-specimens of Clo-. phan-impregnated capacitor. This was partly censed by the non appearance, after the first day, of Engelhardt, but it la not considered likely that any novel processes are Involved. Tor Information on the precautions necessary in the nee of Clophen, see Section II, 5, above. rs U/19/47 023182 2 HARTOLDMONOOQ4917  III-A-b - 500 ''rom - B. 1.0,3. Final Tteport No. 893 Item Nos. 1, 7, 22 an9 31 Pace xiv Clophen is made in several grades, which correspond olosely with their U.3. counterparts, A.50 being the "rode most commonly used for oopacitors. Except for very rare use by Siemens and Ho lake for special orders, Clophen has not been used in Germany for email capacitors of the tele communication type, but it hes been used extensively by 31enens~3ohuckert for power oapacltors. It is interesting to note that the German forces used Clophen impregnated and filled tubular capacitors made by Ducatl, of Milan, who obtained the impregnant from I.O. The prejudice against Clophon was, however, being gradually overcome and several manufacturers were contemplating an extended use of this material, some of them con sidered it to bo equal to or possibly better than mineral oil for opera tion at power frequencies. rs 11/24/4? 0231823 HARTOLDMONOOQ4918 III-A-b-50 From - B.I.O.S. Final Report No, 893 Item Nos. 1, 7, 22, and 31 Pages 98, 99 (2) Clophen The only ohlorlnated impregnant used by llenonaSchuokert Is Clophen, supplied by I.O, In power factor correction and high voltage applications it Is consider ed practically Ideal.- The only type of Clophen used in bulk Is A.50, pentachlordlphenyl, (corresponding to Aroolor 1254). a.an and A.40 have been tried and found unstable. A.60, A.70 end A,80 ure too vlicouiT^o'allow rSfROofl "Impregnation and have lower permittivities. Although the viscosity of A.50 at room temperature Is much greater than that of oil, the viscosity at Impregnation temperature Is sufficiently low to give no trouble in attaining 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.0. over e period of years, the acid content had gra dually diminished, and it is now possible without chalk treatment to work to the same rejection limit of resis tivity as for oil, viz. 101 ohm.em. at 20*C. Drums of Clophen falling to pass the conductivity test ere returned to I.G., unless urgently needed, A certain elasticity Is permissible In view of the hlgi standard set. Apert from conductivity, further acceptance ohecks 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 costa about 1 K. 60 pfg./kg., and Is therefore much dearer than oil (30 pfg./Eg.). 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 lmpregnant Is that Is has a similar permittivity to paper (viz. 5). Other lmpregnants studied. As Clophen Is considered nearly Ideal, no serious attempts have been made to find superior materials or addi tives to Improve its performance. This attitude Is sup ported by service experience. In which no failures have been reported. It is realised, however, that on freezing .discharges may ooour In the contraction voids, which may result In decomposition of the Clophen and failure of the 0231824 HARTOLDMONOOQ4919 dielectric. Tests were performed (see Section XT, 2, (5)) to check whether this depredation does In fact occur, end no failure was noted. Nevertheless, 1.0. supplied small samples resembling Clophen A.50 but having a lower melting point so that this possible source of failure could be Investigated. De pression of the temperature at which the dipoles beecme Immobile should raise the maximum usable frequency and hence broaden the range of applications by Introducing those for audio-frequency furnaces. Two of these 1.0,. samples, with references A.162K and A.16BN, are, like Clophen, made from benzene, but have a lower chlorine content because of the presence of an additional alkyl group (CflHen+l), and hence e layer density. Their advantage over Clophen A.50 Is that the setting point (l.e. temperature of maximum dispersion end of capacitance diminution) is lowered from -8*C. to -17*0. The permit tivity, viscosity and non-lnflammablllty 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 XXXV. ( 11/19/47 ( 0231825 HARTOLDMON0004920 IU-B-2500 December 22, 1947 TO: FH03PU.YTE DIVISION SALESMEN 30BJ: Aroclor 5460 aa Deed In F.thylcellulone Lacquer RE: Federation of Paint and Varnish Production Clubs Official Digest (October, 1947). Aroolors used aa plasticizers and resins Impart excellent qualities to ethylcellulose. Ethylcellulose Is used In lacquers of various types, the ethylcelluloso 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 whloh may develop In nitrocellulose laoquers on heat sealing Is not permissible; linoleum lacquers whero alkali resistance Is essential; textile printing; printing Inks, particularly In multicolor designs where hydrocarbon solvent does not soften or blood Into previously printed designs; alroraft lacquer for resistance to both heat end cold and to quick temperature changes; record lacquers, especially for home recorders; and In wood sealers where good sanding and flexibility ere essential. A good pigmented ethylcellulose lacquer has been made, based on the following formula: Ingredients Ethylcellulose N-22 Aroclor 5460 T108 Menthylphenol Toluene Ethanol Parts (by weight) 6.4 6.4 4.2 0.06 67.0 16.0 100.06 Benignus Copied by rs 2/2/48 HARTOLDMONOOQ4921 XI1-3-300 From - Memo G.Y. Frankle/P.O. Benlgnus Maroh 11, 1948 Soil-Poison Concentrate As described below, tbrne materials are formulated Into a water emulelflable soll-polson ccooontrate carrying almost 80 per cent by weight of aotlve Ingredients. Aroclor 1242 Trlohlorobenzene (Klxed Isomers) Pentaohlorophenol Isopropyl alcohol Toluene or Xylene Sterox SE* Santomerse 3 Paste 33.55: 33.5 10.0 3.3 16.7 1.5 -A&. 100 .OfC * Other non-lonle type emulsifying agents such as Triton HE or Span and Tween oan be used to replace the Sterox SB. Copied by rs 4/2/48 HARTOLDMONOOQ4922 ( m-H-io Chemical Abstracts POSSIBLE U9E OF AR0CLCK3 . Vol. 41 Page 6867 U.S.P. ,425,978 to Anderson and Coalehan, (Hercules Powder Company). Foundry cores sprayed with 15 solution of chlorinated naphthalene In hydrocarbon solvent show greater scratch resis tance than untreated oores. Cl2 content remains from 40 - 80;' Cl*. Particularly good for use with A1 castings. rs ( 12/2/47 ( 0231828 HARTOLDMONOOQ4923 From - B.1.0.3. Final Report Ho. 893 Item Nos. 1, ?, 28 and 51 Papes - 10 and 11 Huoh less trouble has been experienced with cblordlphenyl than with ohlornaphthalene, probably because the former, being, liquid, in volves less physical Contact in disposal. (2) Prevention, ' Very thorough washing of all areas of the skin likely to be contaminated with solid, liquid, or fumes has always been the basio prinoiple In prevention of skin troubles, and is still looked upon as fundamental. - :Vhen fatty soaps ceased to be available, because of the di version of fats to food, it became essential to insist upon the uso of barrier creams, of which the best was one named "QPiraO", made at Tromraersdorf. This has now been replaced, for lack of supplies, by an alternative made by I.O., named "MITIQAL*, which is considered inferior to rulmbo but satisfactory. . The Flssan firm put up a special powder named "3CH"SFELKJLV'rR" to act as a barrier, but this was found to be inefficient except to allay irritation on skin areas exposed to fumes only. For this purpose it still finds use at Leverkusen and at the Hydrawerke factory at Berlin. A special point is made of fume extraction,' and the minimum air speed away from the operator is 1 metro 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 ehlorlnatpd hydrocarbons, and slnoe the enforcement of the precautions, no deaths or symptoms of internal Injury have occurred. Since superfatted soaps have ceased to be available, a cleansing composition containing dlehlor-methahe hes 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 chloraene end Internal sickness were encountered, in the early years, when the properties of ohlorlnated 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 e few mild cases of chloraene have been met. These have been treated with a solution of acetic and salloyllc acids in methylated spirits, 0231829 HARTOLDMONOOQ4924 (4) Conclusions and Recommendations. 1.0. ooasider that neither toxicity nor skin affection need now be any deterrent to the use of chlorinated naphthalene, and that ehlordlphenyl la If anything less troublesome. . Certain people, notably those with fair skins, show dlstlnet allergy, and are best diverted to other work not Involving oontact. Scrupulous cleanliness of the skin (Including the face, neck, and arms) and of the olothlng (especially undergarments) Is essen tial and needs strict enforcement. '.Joshing with hot water and good soap Is sufficient, so long as the soap Is superfatted, since the skin bcoomes sensitive to irritation by alkali. Barrier cream should be used on those parts of the skin whloh 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 are contacted by fumes only, and particularly those chafed by clothing (e.g. the neck adjaoent to the edge of the clothing) need protection by a suitable soothing powder. . v.'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 the precautions are being evaded, or lest there should be some Idiosyncrasy, monthly medical Inspection Is desirable. ra 11/24/4' 0231830 HARTOLDMONOOQ4925 rv-B-ioo From - The Journal of Industrial Hygiene and Toxicology Volume SO, Humber S February, 1938 MORPHOLOGICAL CHANGES IN TIE LIVERS OF RATS RESULTING FROM EXPOSURE TO CERTAIN CHLORINATED HYDROCARBONS * Chlorinated hydrocarbons, particularly chlorinated naohthalenes and chlorinated diphenyl, have been used extensively In certain In dustries. Their U3S 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 rots that had been exposed to various chlorinated naphthalene com pounds and to chlorinated diphenyl. Compound G (chlorinated diphenyl) was administered to two croons of animals in low concentrations. An average concentration of 0.57 mgms. per eu. m. was employed 16 hours daily for 154 days In the first experiment. In the second experiment (employing an overage air con centration of 0.93 mens, por eu. n.) the animals mere exposed 8 hours dally for 143 days. The pronent experiments demonstrate that chlorinated naphthalene compounds and chlorinated diphenyl are capable of producing marked liver damage In the white rut without demonstrable microscopic changes appearing In the other org..ns. 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, chlorine.ted di phenyl gave evidence of being the most toxic. '.Then administered by Inhalation In very low concentrations (overage 0.57 to 0.93 ragma. per ou. m.) liver cell changes were very pronounced after the first exposure period. The most striking change was the hyalintzetion of t the oell cytoplasm (see fig. 6, plate III). 3uch cellular alterations were essentially unchanged after a 2 month recovery period. In these animals small sublethal doBes of oerbon tetrachloride and alcohol uni formly produced extenelve liver necroslo and was highly fBtul to them (firs. 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 oells and active regeneration (see fig. 4, plate III). However, animals removed from exposure before being futally 0231831 HARTOLDMONOOQ4926 -2 poisoned, subsequently developed hyaline degeneration of liver oelle similar to that produced by prolonged administration of small doses of this compound. ThUB the results of the -resent study, as well as certain field studies that have been made (1) surest that the solution of the In dustrial hazard Involved Is dependent largely on a reduction of the air concentration of these compounds to a level that will not produce liver damage. The present experiments Indicate that loner air con centrations must be obtained In the case of the more highly chlori nated naphthalene compounds and chlorinated diphenyl than for trlchlornaphthalenee If a safe environment for workmen la to be assured. Be cause of the pronounced toxlo effeot of small doses of carbon tetraohiorIde on the livers of animals already Injured by exposure to chlorinated naphthalenes and chlorinated diphenyl. Its use as a sol vent for these compounds would appear to be very hazardous. rs 2/3/48 0231832 HARTOLDMONOOQ4927 January 27, 1949 Distribution: 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. `Bits Copy For^l5. 16. 17. 18. Researoh File R.L. Jenkins - C.B. Durgln J.L. Christian - R.S. Weatherly W.T. Durrett - F.P. LaBelle v H.F. Weaver C.A. Hoehwalt E.P. Rucker Edgar E. Hardy J.F. Reeves J.F. Reeves A.M. Ellenburg R.R. Knight Paul Logue P.O. Benlgnus . ' V Please Insert the attached data In your copy of Report No. 2215, "Aroolor Data Book", Issued April 27, 1948 by R. R. Knight, Researoh Department, Phosphate Division, '1 AHE:rs A. ti. Ellenburg *3i*33 HARTOLDMONOOQ4928 I-A-a-200 Oi:S: j. jl. Kmj-.& oh ; ilo Kind Report on "Evaluation of lionsanto Ilatsrials os PlEntidzere", Job Ko,, S!%>. AROCLCIR 1832 Calculated molecular woigjhi,: 283 Refractive inder*: 1.620 at 20C. 'Saponification equivalent*: none Crystallization point*: ~32,,3>C. Boillnc point*: 290-325C. at 760 nut. Acidity*: ,,01 milligrams KOH/fja, Acidity after heat: none Color (Gardner Standard): 0 Color after heat: 0 Color after llgjit: 11-12 Specific Gravity''': 1,2623 at 25/25*0. Viator solubility: .0016# at 25C. Stability to hydrolysis*: essentially none Odor: chleroeromatic Viscosity: 20*C. - 6,,2<i centlpoise 0*C. - 65 centlpoise -20*C. - 627 centlpoise Solubility: soluble in: octyl alcohol, acetone, ethyl acetate, benzene, Shellysolve C, Skellyaolre L, turpentine, castor oil, cotton seed oil. Partially soluble In: methanol, ethanol, ply- corol, linseed oil. Insoluble la: glycol ra 8-20-48 oi*v HARTOLDMONOOQ4929 I-A-b-300 TABLE I DENSITY AND SPECIFIC VOIBMS 0? AROOLORS AROCLOR 1342 Temperature (c.) 49.9 103.3 150.3 301.7 254.0 398.3 Density (g./ml.) 1.3546 1.3051 1.2587 1.2080 1.1549 1.1071 Spaeifie Volume . (ml./g.) 0.7382 0.7662 0.7945 0.8278 0.8659 0.9033 . Temperature (C.) 25.1 49.9 103.3 150.1 201.7 254.0 298.3 AROCLOR 1848 Density (g./ml.) 1.4439 1.4193 1.3673 1.3210 1.2691 1.2148 1.1664 Specific Volume (ml./g.) 0.6926 0.7046 0.7314 0.7570 0.7880 0.8232 0.8573 Temperature (c.) 35.1 49.9 102,9 150.1 301.8 205.5 298.2 Density (g./ml.) 1.5392 1.5139 1.4607 1.4127 1.3595 1.3096 1.2546 Specific Volume (ml./g.) 0.6497 0.6605 0.6846 0.7079 0.7356 0.7636 0.7971 023183^ HARTOLDMON0004930 X-A-b-300 ( TABIE X Cont'd DENSITY AND SPECIFIC VOIIJME OF AROCLORS AROCLOR 1260 Temperature (C.) 49.2 102.8 150.2 201.9 251.0 298.3 Density (g./ml.) 1.5956 1.5424 1.4931 1.4386 1.3854 1.3322 Specific Volume (ml./g.) 0.6267 0.6463 0.6698 0.6951 0.7218 0.7506 Copied by re 1-20-49 D. Ward Central Research Department December 21, 1940 ( 0231036 HARTOLDMONOOQ4931 I-A-g-400 naaosm: - ggrscT-ub mssjKB on. visrs. . o? <mgjm OHyfiKXTSp . B. B, Dow, V. Hr Tenshe mft H. -1". Morgen Tho Pennsylvania statt, Collets Industrial and Engineering Chomi stry Vol. 29,,1076-30, (1937) The following data are taken from tables in the article end should be viewed critically. Specific heat data are out of line viith our Aroolor figures. . . TABLE I Aroolor SjJ.Ht. tal^g/C'' Cent ipole Vise. so*c Viscosity Donetty Index SCO. 1848 1851 0.95 1,49 -634 -IS83 1,413 1.510 Observations wore nsede that tho ir.eroase in viscosity with preotwj was very groat with the Aroclora aafi Aroolor 3351 exhibit eae of toe highlit highest ratio of increase known'for an oil. HARTOLDMONOOQ4932 TAME II VISCOSITY VARIATION V/CTrl PRESSOR Pressure RSL 14.8 600 1000 1500 2000 2500 3000 3500 4000 5000 .6000 7000 8000 0000 100000 18,000 14,000 16,000 16,000 80,000 22,000 24,000 86,000 28,000 50,000 32,000 50*0 134-8 1354 129 Cps -- 153 -- 181 883 887 364 553 833 1270 1950 2940 2740 Ops 3140 4020 5670 8740 14300 33600 40500 ...... 75C 1846 1254 8.7 Ops -- 9.3 -- 10 -- 11 18 13 15 17 19 21 24 30 39 53 75 111 176 300 494 816 1350 2196 24 Cps -- 25 26 -- S9 -- 33 40 48 59 73 92 117 19 B 345 648 1890 8580 Copied by ra 7-12-48 ^3l838 HARTOLDMONOOQ4933 I-A-g-400 TABIE II VI3C03nT OF AROCLORS Temperature (0.) 24.80 29.10 29.41 49.9 99.4 190.2 200.4 291,8 297.7 Klnematio Viscosity (Cent1stokea) 191.0 144.7 140.2 18.27 3.04 1.297 0,777 0.933 0.412 Absolute Vlsooslty (Centipolses) 218.1 208.9 202.4 29.93 4.17 1.660 0.987 0.649 0.482 . Temperature (*c.) 24.80 23.41 49.9 90.1 98.7 130.6 200.4 230.3 231.8 297.6 Klnematlo Viscosity (Cent1stokes) 989x10 903x10 96.7 99.9 3.86 1.783 . 0.991 0.698 0.692 0.483 Absolute Viscosity (Centipolses) 901x10 ' 777x10 146.4 144.9 8.39 2.921 1.349 0.863 0.833 0.608 Copied by rs 1-20-49 D. Ward Central Research Department December 21, 1948 0231839 HARTOLDMONOOQ4934 I-A-a-300 HMWLMlliBIJE DIELECTRIC ORGANIC COEP0OiKrfl3 F. t.l. Clark - General Electric Company Industrlol and Engineering Chemistry Vole 29, 693, (1987) Oharootorljtios of Dielectric liquid Compounds Property Ponteehlor Ponteehlor Hexachloro Purtachlor- diphenyl diphenyl diphenyl- Trickier Biphenyl Oxide Ketone Ifethano Benzene Bum Point K.F. Sp. Or. (*0/15,5C.) 1.51 (65) Viscosity, SOS, *0. 45 (98) Pour Point, *C. + 10 Refr, Index (85C.) 1.6080 Dielootrio Strength, Kv. 40 DicleotrJ.o Constant (25*0.) 5.1 Ai'C formed Oasos N.E. Sludging Nona Fj oc> Acid Nor a Distillation Rungo, *C 880-400 N.F. 1.59 (100) 390 (37.0) 0 1.6220 40 5.0 n.e. None None 200-250 (15 ram) N,F. 1.45 (100) 54 (100) + 15 1,6370 40 . 8.0 N.E. None None 250-300 (25 nra) NX. 1.52 (100) 84 (100) + 20 1.6370 40 4.3 N.E. None Nona 2S0-340 (25 m) N.F. 1.46 (15) 30 (37.e) 0-10 F.P. 1.57C0 40 4.8 N.E. None Non 3 200-220 N.F. - Non-flnrtT.ablo. N.E. - Non-explosive. Moplor_1251 Viscosity - HoKlchoal - Oentlpolsaa Temperature - *C 28 01 40 50 60 70 80 90 100 Vlacoslty - cps. 6000 3000 700 180 70 33 26 19 17 Copied by ra 7-12-40 OZBIB**0 HARTOLDMONOOQ4935 St. Louis Dr. R. L. Jenkins Mr. 0. B. Durgln Anniston May 25, 1948 III-G-100 Messrs. Edgar E. Hardy - Anniston A.M. Ellcnburg - Anniston Paul Logue. T.H. Wheelock Aroolor--SilcBtio Faoto Attached are two ooplos of the Ho. 5 series about Silastic Facts. Reoently Dos Coming submitted the following Information to us: "Sllastlo is swollen quite badly When subjected to most organlo solvents such as toluene, benzene, eto. However, our laboratory has reoently submitted a report concerning the effeots of eblorl- nated diphenyl on Sllaetlo. Sllastlo lmmersod In chlorinated diphenyl for seventy hours at 150*C. The change In the physical properties were noted and the figures Indicated that sllastlo Is remarkably resistant to deteriorations from contact with the hot chlorinated diphenyl. The changes In the properties are similar to thoss produced by hot lubricating oils and can be summed up as follows: ' (1) Lowering of the hardness by about 20 points. (2) Improvement In the elasticity by aeveral points,, (3) Practically no change In tensllo strength. (4) An appreciable Increase in the ultimate elongation," Western Felt Manufacturing Company at Chicago, Illinois, quoted Silicone 180 In sheet form as follows: 8x8" shoot, 1/4" thick 20x20" sheet, 1/4" thick 24x24" sheet, 1/4" thick $11.25 63.50 89.50 Apparently the greatest drawback to the use of Silicone as a gesket material for hot Aroolors Is the high price of the plastics. rh enes Copied by rs 9-84-48 Benignus 0231841 HARTOLDMONOOQ4936 HANDLING AROCLORS III-Q-100 Gaskets - Aroolor and Pyranol . Latter F. B. Zienty to H. M. Hitchens - 9-20*48 "At a reoent meeting It vaa stated by Dr. Suita of General Eleotrio that allloona rubber gaskets wore found to hold Pyranol effectively under oondltlona where other gasket materials gave poor performance with respeot to free.dom from leaks." ' SAIES DEVELOPMENT REPORT . P. 0. Beulgnus - 2-18*48 Precision Dio Casting Company, Cleveland, Ohio "Ball-bearing swine Joints made by Chlksan Tool Company at Brea, California used on flexible connections with Aroolor Installations. "0. I. Olyptal # 8 Red Is excellent for sealing fluid on application to threaded pipe," ra 9-24-48 OZ^8*2 HARTOLDMONOOQ4937 Z -9 'J o o - H HARTOLDMONOOQ4938 * HARTOLDMONOOQ4939 3 0 : fr;6 HARTOLDMON0004940 DIRECTIONS FOR TEST NO. 14-08-48 SUBJnr.r, Evaporation Beat of Liquid Aroolora------------------------Mgrufin- 6 Hours Heating at 100* 0. ASTM D6-S9T - Modified i'- Rroosdure Weigh on a rough balanee about 50 grama ( <5 gm.) of the well mixed Aroolor Into and aoourately tare4 tin box, 55mm. die. X 05 mm. deep (3 oz. 0111-6t|}.e ointment box, deep pattern), Fisher #1-580. Let `stand until box and sample are at room temperature, then weigh aoou rately. . Plaoe the box In a van\^lated oonveotlon oven maintained at 100* 0/ X 1* for 5 hours.'Remove, oool In desleoator to room temperature and aoourately reweigh. From the loss In weight oaloulate the evaporation In per cent. Report to seoond deelmal plaoe only. Motes 1. Be sure box Is at room temperature whenever exaot weight Is taken. 8. The oven should not oontaln other samples whleh might Interfere with evaporation. < 3. Beoause the evaporation loss Is sensitive to temperature, the air bath must be elosely maintained at 100* 0. FABiom 1-89-45 ' ' ` Oopled by af UA/5l 023184b HARTOLDMONOOQ4941