Document XRGZyg8vG8n3w8jBbexKO6r3J

<2 rr:n. c?.4 l ' V"^ N, * REPORT NO. 2213 FINAL RIPORT ON OC LOR _0.T BOOK Job No. 171-451 FI 1* No 141-27.1 April 27. 1948 R. R. Knlsht RESEARCH DEPARTMENT PfcoipHttc Dhrlrioa 2215 Monsanto Chemicals ____ kA____ COMPANY CONFIDENTIAL TRAN 011867 HARTOLDMON0024645 REPORT 0, E215 PIKAL RXPCRT 0 THIS RCPOfTT AND THE INFOPMATIOM CONTAINED HEREIN IS THE PROPERTY Of THE MONSANTO CHEMICAL COMPANY, AROCLOR DATA BOCK Job HO. 171-401 fll* Ho. 141-87.1 RESEARCH DCTARTITEKT - PHOSPHATE DIYISIOW - Annietoa, Alabama ***************** Rsport Submitted - April 87, 1948 Chemist: A.M. Xllsnburg B.R. Knight Prspared by: RH, Knight XI girt sen ooples were nads of this report and dlstributsd as follows: . Ho. 1. Resweroh fll Ho. 2. HI.Jenkins -O.B. Darfia Ho. 3. R.R.Cols - R.3.Hsathsrly Ho. 4. V.T.tXirrstt -F.P. La Ball* Ho. 5. H.F.VssTtr Ho. 6. C.A. Hoebwalt - Ho. 7. X.P.Rueksr Ho. 8. Xd4tar X. Hardy Bo. 9. J.T. Rsstss Bo. 10. JJ.Rsstss Bo. 11. AJ. XllsnborB Bo. IX. CJR. Eal#it . Bo; IS. Paul Lopis ~io. 14. P.0. Bsalffsas lo. 15. ' Ho. 16. Ho. 17. Ho. 18. . This is oopy Ho. /3 COMPANY CONFIDENTIAL ' TRAN 011866 HARTOLDMON0024646 SEARCH DTPARTLSltT - HTOTPll.TT: DI7I3IW MCWIANTO CHUCCAL cottvjty Anniston, Alabama AROCLOR DATA BOOK General Information on properties of Aroelora, Aroelor process data, uaa of Aroolora, and physiological effects of Aroolora. TORB-.fORD Aa a auns of presentLug the available data on Aroelora to the In terested personnel within the 1`onaanto organization, thla looaeleaf notebook la being compiled. , lost of the dote has resulted from work carried out within our onn organization. Literature references, hcnwrer, will be cited in all oases throughout the oonpllatlon in order to allow nore detailed infor mation to be obtained by the user. . The following detailed outline la for facilitating the location of data in the book and to aeslst In properly insert In" new data sheets. Each Aroolor la to be glTen a aeries number for location under the headings. Thla scheme at present la as follow*: Aroolor 1221 a> 100 series Aroolor 1232 - 200 aeries Aroolor 1242 - 300 eerie* Aroolor 1248 . 400 series Aroelor 1234 - 300 aeries Aroolor I860 - 600 series Aroelor 1262 - 700 serlss Aroelor 1263 - 900 seriss Aroelor 1270 - 900 serlss . Aroelor 1271 - 1000 series Other Dlpheuyl Aroolor a - uoo series 'a Aroolor 4465 - 1300 series 4 Other ,Hlh Boiler .'roc lora _ 2100 saris* * Aroelor 5442 - 2400 series Aroelor 3460 - 2500 series Aroelor 3463 - 2600 series Aroolor 3468 - 2700 serlss /roclor 2363 1 3000 serlss Related Compound - 4000 serlss TRAN 011869 COMPANY CONFIDENTIAL THIS REPORT AND THE INFORMATION CONTAINED HEREIN IS THE PROPERTY OF THE MONSANTO CHEMICAL COMPANY. HARTOLDMON0024647 - - Tbs peg# pertaining to the solubility of Aroelor 4463 In various solvents would be of this type "IAJ - 1300". In eases where the Infor mation for ell Aroolors ean be eortp 1 led on on# sheet, such es refreotIt# indioea, the per# will be Inserted under the general heading and sill bear 00I7 the number for the first Aroclor, for example, lAh - 100, I. czrrauL wo^iTiEi or ..roclors A. Physloal Properties (a) General Physloal Constants 1. Formula and molecular weipftt 2. Speolfloations for Innufsoturs (b) Density and Specific Gravity (e) Cubical Coeffloients of Expansion , . (d) Vapor Praasura and Rats of Preparation (e) Speolfle Heat and Heat Capeolty (f) Thermal Conductivity (g) Vlaoosity ' (h) Refractive Index , . {l) Heats of Vsporixatlon - Othsr Thermodynamic Properties (J) Solubilities (lc) Flash and Flams Points (1) Miscellaneous B. Xlsotrloal Propertlss (s) Dlslsotrlo Constants (b) Power Taotoors (s) Dlslsotrlo Strength (4) Volume Resistivity (t) Dlpols Kanents (f) tllsosllnnsous COMPANY CONFIDENTIAL TRAN 0113 70 HARTOLDMON0024648 3- ii. icm>Ds or ttsjsjTAcrrasA. Eoneanto Procaaa 1. Raw Ihtariala 2. Chlorination 3. Mat Illation A, 3toraga and TMpping B. German Process C . Oth r Proeaaaea III, U3K3 Or AR0CL3 A. Elaotrioel Tiald 1. Tranafanaara 2. Capaeitcra 3. Coating for 71ra 4. Other aaea B. Varniahaa C. Plaatlolaara D. Eydraolle Fluid 3. Tira Ratardanta r. Heating taodiuH I 3. XlteaUanaeoj H. . 3MBtiooi for nav Uaae it. paniOLOoiCAL irrxTa I. Skin Taata 8, ( Oyatanatie Taata . s i Pmi U3IH0 AR0CLCR9 COMPANY CONFIDENTIAL . . tr*n onm HARTOLDMON0024649 -4- THIS REPORT AND THE INFORMATION CONTAINED HEREIN IS THE PROPERTY OF THE MONSANTO CHEMICAL COMPANY. Tbs boot 1 subject to revision sad changes as various data are located, Oraphe and diagram will be inserted when possible and new graphs drawn as iafornat ic i compiled. No indloes of tactions is planned ,ut this tin, but later re visions may include such pages if the volume of taformution warrants it. Contributions of nrw end supplement try data ere aamsstly so licited. Any discrepancies La the existing date or advice aa to a better means of presenting the information will be greetfully acknow ledged. Address ell correspondence to the group leader In oherge of the research on Aroclors at Phosphate Divlrion - Reaearoh Department, Annlstoa, Alabama. R. H. Knight r 12/2/if COMPANY CONFIDENTIAL TRAN 011872 HARTOLDMON0024650 m2 &*. * STANDARD SPECIFICATION or Monsanto Chemical Company PHOSPHATE DIVISION ANHISTOM, AUBAMA P** N*. PRODUCT? _L221 GRADE; ...... ItfOiiar .. PROD. DEPT. NOj _ 3 * I. APPROVED BY (Initial*) CODE NO.? l (uo-C2fl-/ww^ .... SUPERSEDES;... rifta-rmtatip* | F .A Cornell SpedRcatioo CoDiumtr SpgteiiReiitlws Cred Arwlor U.2U ip, Op. at 08*3, Acidity, Ham/n. Aroelor 1221t Color Acidity, me* WaSi/rfB* Op, Or* ot 08/13,9*3* Chlorine oaten* Viaooaitf at 100*F 1.150-1.160 4.0.3 40 /JfU me. 0,01 ns. 1.140-1.155 20.3-21.5,; 30-41 103 NOTE& Copied fey W Vs/* a# COMPANY CONFIDENTIAL . Tran ousts HARTOLDMON0024651 .. <s , STANDARD SPECIFICATION -.. or M dcIanto CmEmcIi Com pant PHOSPHATE DIVISION AXNISTON, ALABAMA Pag No. PlODUCTs Aroo lor 12S3 GRADE nm*g PROD. DEFT. 8,U| APPROVED BY (Initial*) CODE NO.: 1040^30^5^ AUTHOWSB^!* SU PERSEDE3i-"gy-T<wtatlT<> AKSt| I*F*RJ F *A *8. Control Specification Commnm S pacification 0n4* Aro&lm LIS81 Op. Or. st S/15,S' Afiiditf, W5 KaOl/gp* Arooior 129i OoIgf Aotditj, nr, RcQH/c#, 7p, Or, fit 6S/JJ5*5^9* CTiloftn* mnPt* Tiaooaitjr t 100*F, 1,240-1 .*46 4L. 00 FILt aax, ,01 MX, 1,235-1,240 31,5-31,5 48-49 373 notes' Ctoi#i y re Vb/ COMPANY CONFIDENTIAL TRAN 01.1874 HARTOLDMON0024652 standard srec otgatich cr MONSANTO OHSnCAX COMPAQ Product; CblorlMtad Dlphmyl, distilled Cade Ho, l040-g4Q-71M)9 and i AZQOior I24S ..................... ..............Bate Author lzad June 21, 1940 3a?orsda Spe triestie Dated July 3. 1954 Tolrbis Lisdte Typi&el Value Sp. Or. st $5/18.5*0. Color, RJA. Aoldity, ReOH/gs, Tiesosity it 54,4*G. 1.538 to 1.348 0.5 Iteximu* .01 l&3EtM 47 to 50 Seeonds 3yboli Unlrere! Approved W A. B, Pertor ......... " . Chief Chen trV Approved by Idw. A. 0*8841. Tts ' "`TorEi' ] 1 BjTgjir Appro?? i lay Bobort S, R--therlr * ' 1 SCoifiEnagtir Authorise by 7. M. Oarothagu ..... ' m a tflni or Copied by r* 4/8/48 COMPANY CONFIDEN IAL TRAN 011875 HARTOLDMON0024653 TEAICAKD SFK1FICATI . 0? . KcwsAjrro ckshical coupaht Proflust: Chlorinated Dlphtsayl, distilled CM Ho. 1040-2 SO-75-Of Grade; Arcelor 1248 - Dut Authorised Tone el, 194 Supersedes Specification Sated Toly 3, 1PM Tolerable Unite Typical Talon 3p. Or. at 65/13,5*0, Color j If iP .A Acidity, Mgn NaCty'pi Ylaooalty at 54.4*0. 1.404 to 1.414 0.5 Maxima * .01 Maxima St to 76 Secossia Onybolt UniTerMl Aroolor IS62 Op. Or. at 80/15,, Color, Aeldity, Mgn NaOSt/^M. Tlsaoaity si 96.9K. 1.572-1.588 1.0 Ifeximst .01 UaxLnus OT-100 90S Cod* Ho. 1040-510-75-09 Appratwl by A. B, terMr Chiaf Ohasdai As prof#4 bsr Ms, A. O'laal. Jr. Ajyoy#4 by Robert S, laatfearly Aatherisafi by 7. I. Carat hare _ " BSiHeiT 5TS i' Coplrf If rs 4/8/48. ^ COMPANY CONFIDENTIAL TRAN 011876 HARTOLDMON0024654 STAHUPD gpgCITIC TICK MDHSAJfTQ CSSJCAL OOKPAKT Producti Areolar 1254Cod Wo. 1040-290-75-09 Qradet Dlaleotrlo_______________________ Date Authorized IQ/s/il 3upara*daa! 6/81/40 Color, AFHA 3oal Condition 9poolflo OraYity at 53/15.0*0 Acidity, Ug*. NaOH/o*.. Ioorgauilo Chloride*, ppu. 3nybolt TiaOoaity at 98.?*C, aeo. Dlaleotrlo Constant at 100*C RaairtlTity at 100*C, obo-aa. at 000 Yalta Refract Ira Index at 25*0 Distilling Ran?*, Observed, 10% Obaarred, 50% Observed, 90% Pour Point . tfater, pp. Xvaporation, 6 Hra. at 100 *C Corroaion Teat-Chanf.e in walftht Acidity after taat InoroanlT^STorldaa after taat Condition after teat Color ' ' afSer taat rs 5/u/4a 100 Uu, Clear 1.495-1,506 .01 0.10 Uaz. 44.5-47.8 4.15-4.38 Above 600 I W 1,5370-1.WTO 350-385*0 355-36**C 35*-375*C 8 to 1* 35 llaz. 0.4% 0.0% 0.01 0.10 Uaz. Clear 150 Uaz. COMPANY CONFIDENTIAL TRAN 011877 HARTOLDMON0024655 Cj STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON, ALABAMA Faf No. PRODUCT: ...Areolar 44flB tHagglas-1 ___ _____ CODE NO.: iftdQnLYwre^m DATE GRADE: _______________________ . _____ AUTHORIZED: jaetna tqaa PROD. DEPT. NOj _______________ _____ _____ n.r./.i APPROVED BY (Initial*) qj*v44 _ SUPER3EPESt__ZU&fl_IL_lMA___ P.L.J F ,B. Control SpedHcation Consumer Spedfication Appeorsaet : Color, N.PA* loftania Point U.3,r*W.) Anid irusber (L^rioon/rsu) Cry/rteJLUnity eloor, 11;^h% 7ellou, brittle renin 2,0 raax, 60 - 66*0. o - ,o V. No, *p*o. * Raising color Halt to 2,0 m&slimm 1 menaoAtS booeus# Inspection record* show that all lot* produced la 1944 hare bod a eolor of 1 NOTES: Copied by r* 4/8/4 ' COMPANY CONFIDENTIAL TRAN 0U880 HARTOLDMON0024658 Monsanto Chemical Company Anniston Method No. 14-10-46 OpeolfiO Gravity of A_roelar The temperature at shleh the creTitiee of liquid Aroolors ere taken va rles with th viscosity of the liquid. Note the temperature at which the gravity is to be taken for the Aroolor under t est and heat the sample to 10C. above .thot temperature, Pour the hot sample Into the ateen or hot water jacketed hydroneter Jar provided for this test. Stir well with an eocurate thermometer end adjust the temperature to the desired point by controlling the steam or hot toter feed to the Jacket. Continue stirring until the temperature remains eonstant for half a minute. Allow the hydroaster to sink into the liquid, then reed the hydraaster scale at the point of the lower aenlseuj end record with the teaperature. Report the specific gravity to the nearest 0.001 unit. HARTOLDMON0024661 Total Ch.lcrl.ie la Aroeicar* -3 LIX'IS AR0CL3R3: ,20 to ,50 pprems srs weighed by dro 'T-ing frca a 'Btirria^ rod onto piecg of this hsmi spherically shaped glass, av 1/2 .TSlatla oapsul (Gelatin Capsules No. 00, United Drug Company, Boston - 3t, Louii), which he been Juot nrcTiously tared, and which rsraalae os the balance. It is necessary to best the now viaooua Aroclsrs to `"dropping*' consistency. The plao# of glees than welly elides off the btlnnoe pan into the fusioa map. Cows? with the fusioa mixture.. The following quantities of s-a^ale, mm w, and AgS?03 ar# used for the respect!? ehlerlns contents: 01 C intent TeLeht of Staple Amount suar 0$ - 50$ SC# - 48% 45* - 58* 58,1 - 6&% 6$ TOfS Procedure O.S grams 0.3 rr&m 0,3 grans ' O.S rxamM O.S grams 0.8 g. 0.3 B, o.s e* 0.5 c 0.5 g, ' . 50 ml 50 1 50 al 75 ml 100 ml Pine the fusioa map, which contains the trtpcred twaole and fusion mixture, in the irsasit# ignition plat and apply the full flame of the Maker burner to the bottom of the fusion eun for z minutes. . (CAUTIOH: Do not stand too near the fusion durLnr lmition. Tbs ua of a sufety shield ie recommended.) Then refflo th# flame sad cool under the tep. "Tie cool remov# oerew oop. Thoroughly rinse the oup over with water, collecting the rinsingt in a clean 400 si. beaker. Then' place the fusion cup on its side is the beaker and cover with s jssteh class. 50-7 1 will b in the boater from rinsing, the asp, and this is sufficient to decompose the cher", Rc tot* the cup and rinse well, .hen decomposition is complete, rinse off oo?ergLss and add pur WO*, with stirring, until acid is present in excess to the extent of etaat 10 ml. (About 50 ml, of eold ere required.) Add sioetly SO, W, or 100 al. of standard silver nitrat solution from pipet (depending opera ohlarine pruatel) and etix to effect e*ofil8tloa of si Iyer aitrefc# prteipitat#, filter with aictica through an sb#to p*d b e 1-1/Zm perforated porcelain plate end bsalnir and filter 4 time with aftftll portions f soli water, All@ the filter to dim la m~ pletely between waehines. Transfer th filtrate beck into the 400 si. b@aker mad rinw. the fli t twimt addla.- th rlaainns to th beeker. Add 5 al. of fsrrle Ire* indicator to th solution and titrate with standard B7M3 eolutloa until s distinct pink tint is Just obtained. CO^C^A/y TRAN 01186 5 . FIDntial HARTOLDMON0024663 Total Chlorine la Axoolora 3- Calculation of Chlorine Content _ Subtract the volume of ECTr3 required from the to lume of KC7J3 required to titrate the amount of standard AgflOj solution used. This will the volume of KEHS equlTalent to the ohlorlne la the sample. Multiply the to lone so obtained by the eiilor Lae value of each ml. of KCTH and divide by the weight of sample takcen. For eiajsple; If 50 ml. of silver nitrate solution la equivalent to 61,4 ml. of KOlfO solution and the value of 1 ml. of KDNC eolutlon Is .003770 gram 01; then if it Is found that 0.3 i-rara of sample show* a KQn titration of 10.4 ml. the percent of ohlorlne i; (61.4 - 10.4) I .003770 X 100 a 3 C1 In case the fusion mixture or other reap;ants contain oh lor ins, the amount met he determined and deducted frea the chlorine found. 3olotlons Required `tt.aDdard AgNOg 'Solution: Dissolve ZZ nyans of silver nltrnte la eaoh liter of rater. Protect the solution from light. Standard FCN3 Solution! Dissolve 10 ''rams of KCN3 In 1 liter of -rater. Ferric Iron Indicator! Use a saturoted solution of ferric aamonlum aiua, about 50 g. per 100 ml. of water. Pure Nitric Acid: .Stock acid suffices provided It Is colorless. It can be boiled ln.a beaker until colorless'if necessarr using 600 ml. HN03 and 300 ml. of HgO. Standardization of Solutions ,'etgh 0.3 and 0.13 pyam portions of pure dry NsCl into separate 600 ml. beakers. Add 200 ml. of distilled mater to each and 10 ml. of pura 30> nitric acid. '.Than solution is complete, add 30 ml. of otandard A^IOg solution rraa plpet, 9tlr well ami filter through an asbestos sut os a perforated porcelain plate, using suction. Wash filter and transfer Mas filtrate back to the beaker in the same manner as. whan working with a sum'Is. Titrate the filtrates with standard IGK3 eola tion, mim ferric Iron, indicator. The value of 30 ml. of k$BQ% eolation in terms of ICN3 solution is found by subtracting the ml. of KGS3 solution im titrating the 0.3 gram of HaGl from twice the number of ml. of ICIT3 eolutlon used 1b titrating the 0.13 gram of Had. HARTOLDMON0024664 Total CWffiiw la Aroclcrs -4- This value la checked by titrating 30 ml. of A^IO, eolutico added to 400 ad. of water pd 10 ml. of pure 50> W09 with KCTC3 solution. This titration ghould agree very closely (1 0.1 ml.) with tha ralu* found from tha titration of NeCl. Tha titration mu at be made aloviljr to arold drainage error. 3Lnoe para NaCl aontalaa S0.66ii Cl by theory, the ralua of the SONS In terms of chlorine nay be found by dividing the weight of chlorine In the fteCl taken by the ml. of KCR3 equivalent to the silver nitrate required. Examplet Two 0.3 gram portlona of NeCl eherw KENS titrations of 13.11 and 13.13 ml. ' . Two 0,15 gram portion* of RaCl show HONS titrations of 57.28 and 37.24 ml. The KENS equivalent to 50 ml. of AgNO> is then (37.28 37.24) - 13.12 or 61.4 al. By titration of 30 ml. of Agfl0# against KCWT solution. It is found thnt 61.36 ml. are required. This agrees within .04 ml. of the value obtained from the NeCl titrations. The ehlorlne value of the KCNS is then, .6066 X .3 divided by 61.4 13.12 or .003770 pmms Cl per ml. of KCN3. The ehlorlne value nay also be calculated from the titrationof 0.15 gram of H01. 0.6066 X .15 divided by 61.4 - 37.26 rives .003770 gnm 01, per ml. of KCN3. Precautions 1. The fusion raatsrials havs axploslva properties if handlsd improperly; oonssqusntly ears mat be taken to us# safe pro.oortlons, to secure a good alxturs free of large lump#, and to croperly neat the cover of the fusion sap. Tbs fusion mixturs anat be kept away from -ater or moist sir. either of ml ioh nay ignite the charge. The fusion mixture should not bs ground to reduoe lumps. 2. Tbs method as donor lb ed la not applicable to volatile organ le com pounds unless prsoautlons are taken to avoid loss of sample during weighlag. Ifftot of Tarlobles . 1. On account of the high chlorine content of s^ny of tha Aroclara and tha Mll mount of samole taken, great accuracy la required in weighing, transfer, and mixing or the sample. Tha plpat and buret for momiriar the standard solutions mast be very damn to avoid drainage errors. COMPANY TRAN 011887 CONFIDENTIAL HARTOLDMON0024665 Total Chlorine In Aroolors -5 2. Fusions whiob show blaolc oarbon denositei on the cover and aid of tho fusion oup may or may not "ife tha full chlorine content. If a carbon deposit la found, a second fusion should be made uslnp a mailer sample or reducing the amount of sugar In the ehar^e or both, 3. Tbs temperature at which the standard solutions are standardised should bs noted. In csss rooa temperature* rary from this tem perature , appropriate Tolune corrections should be .made. 4. The fusion mixture materials should be essentially free of ahlorln#, T e chlorine oontent may be determined by natcinr a blank fusion, that Is, without addition of sample, end titrating in the usual may. Fife al. of AgNOg 'may be added instead of 30 ml, portion* of A^05 solution in like volumes of solution and nitric aoid, Heferences Beamliria: Determination of Organic Halopens, Ind. Eng. Chem., Anal. Ed., _6 332 (1934). r.vB: os 1-29-45 Copied by r 4/20/48 COMPANY TRAN 011888 HARTOLDMON0024666 Uonisste Chemical Company Anniston liethod Ho, 14-17-40 mi-SST; ^ETHD l noftanla^ Point of Tolld Aroolam Ball and Rjjmr This method la a modification of ths A.I.T.Ii. standard "method of teat tar softening point of bituminous materials, seria? designation: B 28-397, Tfe method differs from the standard rasthod In that the rings are larger than apeolfled. A two ring support Is also used In order that two tests nay be mede simultaneously. Apparatus The apparatus oonalsts of the following: (a) Two ta pared brass rlrvi, 3/8" inside dia. at bottom, 11/16" lnaide diameter at top und 1/4" deep: thickness of wall 3/32". (b) Two steel balls, 3/8" diameter '.'eight:**, 3.45 to 3.35 grans eaoh. (e) A 800 ml. Qrlffln lor: form Weaker. (d) A rinc support for the two rings ha Tine a brass olate exactly one Inch be low the plate supporting tha ring, (a) A 300*C. A.3.T.K. low distilla tion thermos ter graduated 1*C . Preparation of tha ^aapla The sample shall be melted and stirred thoroughly, avoiding overheating or incorporating sir bubbles in the ness end then ooured Into the ring so as to leaTe a slight excess os cooling. 31nce the Aroolars shrink considerably on cooling, the rlnr should be 'tell filled, nearly to over flowing. A little of the excess should be drawn over the top of the ring at several points so aa to prevent tha oooled Aroclcr rroa dropring out of tha ring. In tha same way, tbs second ring. Is filled with e standard Aroclcr of known softening point, Tha standard Aroolor should have a softening within at laaat 10 to 15of tha Aroolor being tasted. The rings while being filled should rest on a clean can lid or on a brass plate which has been amalgam ted to prevent tha Aroclcr from ad hering to it. The Aroolor in the rings should be fully oooled and hardened before preceding with the test. Procedure 0 1 Add wool solution (esploy water for softenlag point between 0-80*C, glycerin for between 00-200*0., mineral oil for above 300*0.) to the beekar until the surface of the solution Is 8" above the plate holding the rings when the rinc support ie buspended In the beaker. Place the ring containing the Aroolor to be tested end th standard Aroolor on the ring support. Plaoa a bell on tha oester of the upper surface of tha Aroolor in each ring. 3aepemt the thsrnoaeter so that the bottoa of the bulb 1 lev si with tbs bottom of the ring Just midway be tween the two rings. COMPANY CONFIDENTIAL r(u,< on... HARTOLDMON0024667 Softening Point of Tolld Aroolcr* 2 Pl*Oi beaker and apparatus on a 6 laoh round hot nlute and heat t uoh a rate that the temperature la raised 5C. each minute. The temperature recorded by the thermometer at the 1113tent the Aroelar touohee the bottom plote is reported ee the softening point. The heat ing la continued until both Aroclors hate dropped to the bottom -lete, Ifo oorreatlons are made for merge nt stem. Rotes 1. The artandord Aroclor Is run along with the sample under test in order to compensate for variations In rate of hBr.ting, dilution of glyoerln, and thermometer variation*. 2. The soften inn point of the standard sanols is determined by making seTersl determinations using fresh elyoerln and oarsfully cheeking the rise in temperature of the Glycerin so that it Is as near as possible to 5*C. per minute. 3. The Glycerin nay be used repeatedly for the testa after removal of the Aroclor. 4. Benzol la used for cleaning the rings and bells. 6. .ater can be used Instead of glyoerin for softening points up to 90 *C. . 6. Tar softening point# ebore 100*C, -ell boiled glycerin should be used. The usual glycerin la not satisfactory above 125 to 130*C, ' It bolls with lots of water while the tsraoerature remains practi cally constant. It Is well to hare a supmly of hlcb-bolliag glyosrln on hand to be used only for softening points above 100*0. 7. Air bubbles on the rings and balls during the test should be avoided as fax as possible. 8. The rate of rise of temperate* of the glycerin shall be uniform for each minute after the first 3 minutes of heating end not averaged over the period of the test. TAB:ea 1-81-48 Copied by re 4/20/48 TRAN 011890 HARTOLDMON0024668 Uoneento Chanlcel Company Anniston Method Ro, 14-21-48 aDBJTSCTi Da tend nation of Iron In Aroolors Iron in Aroolors nay be determined by extraetinc a benzol solution of the Aroelor with dilute hydroohlorio eold until further extractions show do appreetable iron content. The iron in the combined extracts is then -determined by dlohrcraate titration. Procedure Transfer 3-10 grans of eaaole to a dean separatory funnel of ebout 150 ad. oopeolty. Add ebout 30 ml. of benzol and shake until the sample la in solution. TThen solution is oomplete, add 10 ml. of 1:1 iron-free 301 and shake for about 2 minutes. Let stand until separation of the two layers is complete, then drew off and preserve the eeld extract. Add another 10 ml. of 1:1 3C1 end shake again. Draw off tha acid layer and eonbine with the first extrnot. Continue until HC1 layer is clear. Determine the iron by usual dlohronate titration method. FAB tom 1-31-48 Copied by ri 4/21/48 TRAN 011891 HARTOLDMON0024669 Monsanto Chealoal Coespany Anniston U&thcA Uo, 14-24-48 0UBJ3CT; Flash and Flame Points M/TUDDi CleTeland Open Cup rh flush and flams points of Axoolor shall b determined in the . Cleveland Open Cup Tester, following; the prooedure described in ASTti' v D 92"S3. Apparatus The oup shall be supported by a metal plate 1/4" {.633 era) in thioknees and 6 inches (13.24 on) in width. The plats shall bs of brass, oast iron, rrroagfat iron, or steel. In the center or the lists there shall be a plans depression 1/88" (.079 on) in depth, end of Just 'sufficient diameter to fit oup. Thera shall be a circular opening 2 3/16" (5.30 era) in dlametor, out thru the plate, oanterinr with the oenter of the above mentioned depression. The plats shall bs covered with a sheet of hard asbestos board 1/4" in thickness, and of the mrm shape as the astal plate. There shell bs cut in the center of the as bestos board a circular hole just fitting the sup. Heat may be supplied from any convenient source. The use erf a ras burner, electric heater, or alcohol lamp is permitted, but under no olrcuastanees are products of cobbustlod or free flame allowed to oorae up around the cup. The source of heat shall be centered under the opening in the plate and shall be of a type that will not produce looal superheating. If a flame heater is used, it may be protected from drafts or ezoessive radiation by any suitable type of shield, that does not project above the level of the upper surface of the asbestos board. Tha thermometer shell conform to the requIrenaats of thermometer Ho. 8. (Tee A3TM table of thermometers). Procedure The therraooeter shall be suspended or held in vertical cosltlon by any suitable device, the bottom of the bulb shell be 1/4 in. (.635 oa) from the bottom of the cup, and above a point half uay bstwsan the center and back of the cup. The oup shell bs filled with oil to be tested in such s Banner that the top of the meniscus is exactly at the filling line at roan temperature. The surface of the oil shall bs free from babbles. There shall be no oil above the fiUlnr. line or outside of apparatus. The test flame shall be approximately 6/S" (.897 cm) in diameter. The test flame shall be applied is the tesperature read cm the tberaometer reach seh successive 5*F mark. The florae shall pass in e straight line, (or es the oircuafarena* of a olrcle having a radius of at least 6 inches.) across the oemter of the oup and at right angles to the diameter passing thru the thsrraoaster. The test flans shall, while passing across tbs surface of tb oil, be in ths plan of tha upper edge of the oup. The time for the passage of tbs test flame aoroes the cue shall b ipvcil- aately 1 second. COMPANY CONFIDENTIAL TRAN 011892 HARTOLDMON0024670 Flash and Flag# Folate Z- The oil shall be heated at a rate not exeeedinr 30aF car minute terar>art3ture rise till a point Is reached approximately 100*F below the probable flesh point of the oil. Thereafter the irate of heating shall be deoreased and for at least the loot 50F before the fleeh point Ib reaohed the rot shall be not lees than 9T. or more than lleF per minute. < The flash point shall be taken us the temperature read on the thermo meter when a flash ap'eura at any point on the surface of the oil. The true flash roust not hs confused with s bluish halo which sometimes surrounde the test flame. After determlnlnc the flesh point, the heating shall bo continued at the specified rate of 9*7 to il*F per alnote, and application of the tast flags shall be made at the speolfled intervale until the oil irpaltes arid con tinues to burn for a period of at least five seoonds. The method of application of the flame shall be the same as for flash point. The tem perature read at the time of the flame application, which causes burning for a period of five seconds or more, shall be raoorded as the fl&ae point. The flash point and flame point testa shall be made in a room or com portment free from sir drafts. The operator shell avoid breathing over the surface of the oil. It is desirable that the room or ecrapert- Burnt nay be darkened sufficiently so that the flash nay be readily die-, oernible. . Note Aroolora 1248, 1854, 1260, and hl~her ohlorlnatad Aroclors do not hava a dlstinot flash or flam# point below their boiling temperatures. 1-26-45 Copied by re 4/21/48 COMPANY TRAN 011893 HARTOLDMON0024671 Moas&st Chsmiaal Coapajjy Axmlstoe ?isthod No. 14-29-48 lUBJlKTi ITETaOD: Tlsooslty of Liquid At emigre Saybolt Universal, A.3TM D 8B-44 Tlacosity la a measure of resistance to flow. It Is measured by tha tin necessary for s ofaoaen volume to be foroad thru tub* of chooen lsacth and Internal dlane ter. By theory the viscosity of a fluid la related to the average distance beV.teen its noleoulee end to their arereee epeed end their size. Apparatus 71 eoofloater assembly with oil tube, beth, reoeiver, thermometers, strainer, tlaer, and plpet to meet all requirements of ASTBJ D 88-38. The viscosimeter now in ass Is asds by Krebs Klee, and Hfg. So., New York, purchased froa FJtil Qrelnsr Co., their 2-tube capacity $&, One tube - on left hand - has been certified by the Bureau of Ttanderde. Procedure The viscosimeter is set up in accordance with manufacturers directions using No. 20 motor oil for the beth. The procedure end method of reporting results ere those described under A3TM D 88-44. Care of Apparatus Both; At conclusion of test, open the contact points until 1 or TnoEee apart so as not to put undue strain oa thermostatic control whan bath cools. Put a few drops of oil in motor cups occasionally. Keep outside of btts wiped free of oil or Areolar. Cover with hood when not in use. Usintain proper level of oil by oeoaslonsl additions thru hole in front. Then oil blackens, dismantle, clean heaters, tubes, and rifloes, than refill with fresh oil. Oil Tuba*, Sfclle rttll hot, renove all possible Aroclor fresa gallery with plpet. Then ooled to 70-80*, fill tub end allery with beaisas, drop thru orifice into besker, drain -allery with plpet, repast with eeefcon, and wipe dry with absorbent paper in such a ay that fibers cannot fall into taab. Repeat until clean. Occasionally cover the leather plunrer with aired thin paper ("copy" C0iVi fany CONFIDENTIAL TRAN 01189<* HARTOLDMON0024672 Kaaaanto Chemical CotEpany Annlatom Dethod No. 14-31-45 t3XBJ~TCTi Distillation ft&nra of Liquid troolore METHOD: A.n.T.U, D-2Q with Modifier11 oaa The apparatus, oonelatinc of flask, condenser tabs, shield, ead ther mometer, la exactly the sane as described under A.9.TJ1. test D-80 "Distillation of Bituminous Material# suitable for Hoed Treatment". Attaah e 6 lnoh uuxlllery thermometer (0 - 130"C.) to distillation thermometer. Pine bulb half naj between top of oork end nrobeble average of distillation range. Cover both thermometers with e 3/4" diameter glens tube to Insure a uniform temperature correction for the exposed stem, baronetrlo pressure and thermometer error. The procedure la chanced only to the extent that thermometer readings are taken when specified percentages (usually 10, SO, and 90*) of Aroolor hive been distilled instead of following the A 8.T JK. proce dure of weighing the distillate between specifled thermometer readings. In testing liquid Aroolcrs, 100 rpxa. of sample ere welched into the distilling flask and distillate received in a tared flask or beaker resting on pen of a Torsion belanoe with 100 gram seels. Pro cedars 7elgh out 100 grams of sample into the distilling flask. Assemble apparatus as described under A.5.T.M. D-80. Insert thermometer (A.D.T.M. high distilling 0 - 400*0.) thru cork in the neek of the flask eo that the top of the bulb le level with the lowest point of juncture of the tabula tore end neck of the flask. Apply beet to tha flask supported on two sheets of SO mesh wire gauss so that the first drop comes over In from 3 to 13 minutes. . Conduct distillation at ruts of 30 to 70 drops pear mlante. Collect distillate in a 890 ml. beaker tared on a balance. Take temperature readings *t 1*. %, &*, 10*, 20*, SO*. 40*, 90*, 60*, TO*. 00*, 90*. 95*, 93*, 96*, 97*, and dry. Corrections for ener^snt stem end pressure are applied to the thermo aster readings if required. Teke correction readings at first drop, 10*, 80*, 90*, and dry. Report the tempera tores to the nearest 1*C. trample: (Exposed stem in degress) X (temperature difference in degrees) X 0.000158 degrees stem eorreetion T^. The exposed stem is reed from the top of the ssrk. 'The temperature differemc ie the reading of the theraosaster aisaa the topers bur# of the auxiliary tbaraceeter. COiVtrA NY confidential TRAN 011896 HARTOLDMON0024674 Distillation Ran* a of Li<$aid Axoelors - 2 0.00012 4 h barosetrie oorrootion Tg normal boiling point La dogroai abaolnt* A p aha nr. La pffaaaura from 780 an. Hg. the oorraetion la addad if barcxnatar la balers normal and subtracted if tb barcsetar la aboya normal, (UaeOou/^11 - "Therraodynaraioe and Chajalatrjr" pp, US}, Correoted Temperature - Obaarred temper# tur* T1 t Tb. * FABta 1-29-4a Copiad by r* 4/22/42 CCr^rM.vjy" CONFIDENTIAL TRAN 011897 HARTOLDMONOQ24675 Monsanto Cheoloal Gaspsny Anniston Bethod No. 14-32-iS OutiJUaTi Evaporation Teat of Liquid Aroolara METHOD: 6 Hours Heating ot 100C . ATT.' D6-39T - Modified Procedure './#lgh on a rough balance about 50 grama {* ,5 gm.) of the wall mixed Aroolor Into an eoeurotely tarad tin box, 35 cm, dla. X 35 on. deep (3 ox. 0111-style ointment box, deep pattern), flabor tf1-620. Let etand until box and sample are ,,t room temperature, then melgh eoeuretely, place the box in a ventilated oonTeotlon oven maintained at 100*C. 1 1* for 6 hour*. Remove, cool In deslooator to rooa temperature and accurately reweigh. From the lose In wight eeleulate the evaporation In per oect. Report to aeoond deolmal place only. Notea 1. Be mire box la at room temperature whenever exact weight la taken. . 2. The oven aboulfl not oontaln other samolea which might interfere with evaporation. * 3. Beeauee the evaporation lose la aeneitlve to temperature, the air bath met be closely maintained at 100*C. FAB:ora 1-29-45 Copied by ra 4/2 3/ CGiVIPaiVY CONFIDENTIAL TRAN 011898 HARTOLDMON0024676 Refraotivg Index of Liquid Aroelars 2 dary is not sharp, adjust mirror itnti 1 a distinct half ahado-j is ob~ talned. If the 11m or the cross hairs are blurred, adjust eyeMeoe until a good focus is obtained. Secure final fine dJust.sent by mean of the slew motion seres. Head the refract ive index, estijratlnc to the fourth decimal -ilaoe. If the temperature of the water Jacket Is other than 25*C., correct to 25 by use at the,correction feotor, * 0.00044 per C. This footer la applicable only to Arodors 1248, 1254, L260, and 1262. It we found by careful aeasuremect on each Aroelcr thru the ran(?e 10* to 50C. The correction is subtracted when the work Lao t apara tor Is below 25C. and added when above 5*0, ' Example: If ti e refractive Index is found to be 1.6422 at 15*0., the index corrected to 25*C. Is 1.6422 - (10 I .00014) - 1.6578. Care and Calibration of Instrument Immediately after uoa, clean tbs prisms with swabs of pure cotton dipped In benzol, finally wiping dry with a soft doth. The orlsma, especially the upper one, tarnish end scratch easily. Consequently great care must be taken in deaninc. Before use the orlsms should always be inspected and recleaned if necessary. 'Then not In use, the refreetonetar should be kept in Its closed oese. For practice or for cheeking erformanoe, distilled water io useful, (star has a refractive index of 1.3330 at 20C., with temperature co efficient of 0.0001. A test niece of eceoial rises of known refractive index ie supplied with the instrument for calibration and adjustment If neoasaery of the position of the index era. Refractlva Index of Aroclors - Typical ' Careful moasurernente at 25C. have given the following typical values for Axoclors. Aroclor 1848 Arodor 1254 Aroclor 1260 Aroclor 1262 1.6295 1.6376 1.6460 1.648 Substantial departures (over 0.0010) from thee values should be in vestigated iiwedietely as they - ^f.correct - indicate substantial error in the composition of the Arodor or contamination with ether materials. TAJ tea 1-27-48 i Copied by re 4/25/4 COMPM/y CONFIDENTIAL TRAN OIL 900 HARTOLDMON0024678 Beams be Chemical Company Aaaisfcea Wethod No. 14-35-48 TJBPDCT: Resistivity of Liquid Aroalars ME TO QD: Resistance 'Jeaeura-monta between Condu c t cr a Apparatus Uag^hn Bride1 Quaere 1 Radio Company Typ M4B, AC operated - 300 volts, serial No. 171, This is a direct-current '/heststone bridge for measuring high resistances, bride balance,being obtained thru us of a vacuum tube voltmeter. Rear#! 0.1 megohm to 10,000 megohms, Oovered by a dial and S-poeltion nailtlpllar switch. A resistance of 1,000,000 megohms can be detected. Teat Eleotrode*: Two ooncentrlo nickel eyliadere (or braes, nickel plated) with feet. Obtained from General Electric Company. The inner eleotrode bee outside diameter of 2.8" and height of 3.25", with area of 184 eq. e. The outer electrode hne inside diameter of 3" and like height of 3.25", with area of 196 eq. cm. The distance between electrodes Is therefore 0.1 Inch or 0.254 ca. By theory the electrode oonstant, area/ length, is 191/0.254 or 752 where 191 le the average area. In proetiee the oell constant supplied by General Electric Coapeny la used. For the electrodes now In use, the oell constant wee given ae 815. Glass Plate: Pyrax, about 3-1/2" diameter with ooncentrlo groove# to assist In speeing the eleotrodes. Obtained from General Electric Company. Oven: Ceneo-DeKhoteneky drying erven with two holes in beck well for por celain tubes for lead wires. Holes must avoid oven heating elements which occupy 2" paths vertically and horisontally intersecting at the center of the circular well. < Lead .'ires: Provide 500 ohm Amphenol twin conductor eeble to connect tlie electrode In oven to the poets of the bridge. The nortioes ex-nosed to oven temperature are bared end then covered with noroelein beads. Provide also a flexible lead to ground the bridge to a water pipe. Clean the leads, heeds, and porcelain tubes neriodioaily. Assembly of Teat Cell The grooved glass plate le placed in an 800 oe. beaker. The clean elec trodes are placed In the grooves of the glees olate with the connector poets directly opposite in order to give the widest possible spacing to reduo# surface conductivity. The cylinder# should be very clone to equidistant. The apparatus should be dried for 2 hours at 100G. before ues. . Heat the sample to be tested to about 110*C. on a hot plate and oour . into the eleotrode aseembiy until the Level of the liquid is 1/4 to 1/fe" above the electrodes. Care met be used to sake ear that the COMPamy TRAN 011901 HARTOLDMON0024679 SJBJEET: ResletlTlty of Liquid Aroclor a - Page 2, tf-IHOD: Resistance Mea but am not a between Conductors lip of the container, froni whloh tha liquid la poured, is clean. Tilt the beaker in suoh manner that all air bubbles In the Aroclor *111 rise to the surfaoe. Air cool to 103-104"C, ?)sen without removing thermometer, transfer to the cry an which is maintained at 100*C. and oonneot the electrodes to the two flexible vrirea whioh lead to the megohm bridge, Then the Aroclor ocnes to temperature (100*C.), remove themoDeter, check cen tering of eleotrodes, ond precede to measurements. Measurement with tlecoha Bridge ^' , Connect the two lead wires to the megohm bridge with the lead from the outer electrode'to the LCH uaknerm post of the bridge; the inner elec trode to the unknown post. Connect the 7ROUND port on the left side to a water pipe. Swing the spring oonneotor, pivoted on the "0" post, to the LO / Dost. Connect the attachment oord to the 110 7 po.;er ipply. /1th the Aroclor st 10CC., turn the oontrol knob (CnBCK-OF^R'.TE-CIt'JRGE) to the CHECK position. Thro-i ell 3 switohea et the rear of the Panel to ON. After 2 minutes bring the galvanometer pointer to zero by mcene of the ZERO ADJUST knob. Than turn the oontrol knob to CILIRGB for one minute. Turn the. 310b tc OPERATE and return the galvanometer pointer to zero by adjustment of the UJLTIPLT 0T switch and the megohm dial. Read after one minute, Repeot the CHARQE and OPJKATX positions for verification. The resistivity of the Aroclor la the product of the "multiply by" reading tines the dial reading times the electrode oonartant . Report In unite of 10 oh* om, rounded off to two significant figures. Example: "Hilt 1 ply by" reading: . Uegohm dial reading Eleotrode Constant 100 3.4 meg. ohms 813 cm Resistivity - 100' X 5.4 X 815 - 4.4 X 10s meg. ohm cm 440 X 10 ohm cm Value* for resistivity ere (jialifled by designation of temperature end voltage. These are 100"C. and 300 volte for the test above. Like con ditions are used at Plent 8. . COMPANY CONFIDENTIAL TRAN 011902 HARTOLDMON0024680 3JBJTCT: Resistivity of Liquid Axoolora Pane 5 ICTHOD! Heslatonoe ?eabutament a betvweo Conductors Caro of Apparatus The "Operoting. Instructions", General Radio Form 458-B, which acoompany the megoha bridge, recite detoile of lnatallation, mea surementa, tueg, and eonetruofclon, illustrated by fi^urea and circuit and 'Tirin'? dia'rramaNo attempt la made to reprodnoe euoh 1 nf oma11 on here. The operator should eoquaint hLraeelf with the oontents of the G.R. manual and refer to it for maintenance of tubea ond parts. .'hen not in use the megohm bridge ahould be closed and stored in oebinet. Cleaning Electrodej - After the measurements are made the eleotrodes are removed fron the . tested liquid, and allowed to drain until the liquid stops running from the electrodes. '..11116 still hot they are placed In a beaker filled jrith benzene under a well venilated hood and allO'd to cool. .lien cool, the eleotrodes are renoved fron the bonzene and scrubbed vith powdered tri sod lun phosphate end n benzene carbontetraohloride mixture (50-50 by volume), Thia scrubbing can be done with either a brush or the hands. The eleotrodea are then rinsed with acetone, followed by tap -wter and then distilled -Tatar. The eleotro.les should not be touched by the hands after the aoetone wash, after final rinalng the electrodes are placed in on or an ot 120#C. for one hour or until they are used again. The glass spacer plates are cleaned and hondlod in the sane manner as the electrodes except that they are wrapped In lense paper before being plaoed in the oren. Calibration For a rough check on the condition of the bridge, one or more cartridgetype resistances of known approximate ralue rtiould be kept on hand for periodic or enorcanay verification of the meter itself. rs 8/3/4A COMPANY CONFIDENTIAL TRAN 011903 HARTOLDMON0024681 Ltonaanto Chemical Campemf Am lato a Bethod No. 14-36-48 3JBXSCT: Dlaleotrlo Constant of Llouid Aroelor Mirra CD: Measured at 1Q0*C. and 1000 oyolas q5 ^ o^ o 3oops This method applies to Mineral oils and oil aobatituta used for insulotinr. purpose#. Apparatus Capeoitanoe Bridge Cathode Rey Null Detector Oecllletor Constant ranperature Oven Variable Air Condenser 1300 co. Pyrex Beater Genera 1 Radio Co., Type 716-AM General Radio Co., Type 707-A General Radio Co., Type 606~A Cenoo-DeKhotinsky #93000 General Radio Co., Type 334-T Procedure Electrode and beaker must be cleaned as directed under "Cleaning Appa ratus for Dleleetrie Constant", and be at 100*C. Heat A_rodor In the can to 105 C. Pour over electrode until ole tee and oeraaio insulation are covered. Connect leads. 3tlr with thermometer outside ovan until temperature reechss 101*; place in ovan which has bean oersfully adjusted to 100*C. At the tine sample is pinoad in oven its temperature should not have fallen below 90*C. Connect leads to capacitance bridge, observing that the lead frost insu lated aide of oondenser goes to Insulated terminal on bridge. Belanee bridge carefully according to direction under "Balancing Capacitance Bridge". Until Aroelor and oven taaperaturea have beooms identical the bridge balance will constantly shift. After oven temperature reaches 100*C,, maintain bridge balance until no pronounced shift is evident. Record reeding of capacitance scale multiplied by multiplier setting. Dleleetrie Constant. Capacitance in Aroelor at 100*0, Capacitance in air at 100*C. Balancing Capacitance Bridge Condensed procedure. Operator should read operating instruction for Bull Detector for complete details. 1. Connect to power supply leads to oscillator and null detector. Ground the oscillator. 2, Turn on oscillator by pushing 3000 ohm, 10 mltiplier, 100 cycle frequency buttons. Adjust harmonic ontrol until oscillation begins as shown by dosing of seotar in cathode ray tub. TRAN 011904 HARTOLDMON0024682 fw #3 Dielectric Constant of Liquid Aroclor - Test 1 *-36=<s0 aoaoitanee Dial) must be in balance position. If the ellipse rrad- ually opens when the line is horizontal it my be brou-ht baek to the line eg in by makitr slight chants in this control. If confusion remits, balance both controls ags in ns in (13) end reseat the suc ceeding adjustments. This la the position of bridge balance: An alteration of the power-factor control will tilt the line which does not open sppreelsble thru an an*le of 30 to the horizontal both ways; on alteration of the capacitance dial opens the ellipse but does not change the inclination of the major axle. The apparatus say be left In this balanced condition, turned off by switching off first the brillianoe knob of the detector, then the power switch, then turning off the osc ills tor. For suooeeslye measurements the oontrole are not changed, the apparatus left in adjustment. Then the following steps define the procedure: . 1. Connect all lends as previously dirscted Including that from null detsctar to bridge. 2. Turn on oscillator by wishing 100 oycle frequency button. 3. Turn on null detector, wait 15 eeoonds then turn on osthoJe ray tube. Turn sweep amplitude to oxtreme left end adjust brilliance to obtain a fine vertical line on soreen. 4. Brlnr this line to b dot by adjustin'* the two bridge controls. Initial adjustment is facilitated by having "Gain" control to laft. Whae final adjustment is obtained this knob must be at extrema right. 5. This dot rtiBining unchanged shows condition of brld-e balance. Cleaning Apparatus far Dielectric Constant The eondsnser is removed from the tested dlsleotrlo and allowed to drain while still in the oven et 100*0. The condenser is then placed, while still hot, in a beaker of benzene under a well ventilated hood and allowed to cool. It Is tben thoroughly washed with powdered trieodlua phosphate ond a 50-50 mixture of benzene and earbcsa tetrachloride followed by an aoetona rinse. The operator should be very careful not to touch the metal plntee of the oondenser .after this point. Tbe oondencer is tben rinsed thoroughly with tap water followed by distilled water end dried on a clean paper in an oven et 120*0 for at least one hour or until it is again used. twb 3/1/48 TRAN 011906 HARTOLDMON0024684 Jteng&oto Chemical Company Anniston IJethod No. 14-42-48 'UBJr.CT: Acid Number of Liquid Aroolors 3kT_'TM!0D: Titration with Alkali using Phenol Red .2522J. Th Aoid Number la the weight In milligrams of -sodium hydroxide re quired to neutralist one grera of Arcelor to pH 7.6, It thus inoludeg any hydrochloric acid, ferric chloride, and other inorganic or organic oonat ltuante having eid characteristic*. It oorreaoonds to the Neu tral! sat ion Number of A'TEJ Dea iraantlon D108 except that the latter is expreseed in terns of KOH instead of HeOH and has a somewhat higher (phenolphthalein) end point. Procedure To 100 ml. of adjusted (pH 7.6) solvent containing lad Icetor slonly add 0.1 N NaOT dropwlee until the col* oerrssoondg aonroxlmately to pO 7.6 when compared against a suitable reference solution. Readjust if neoessary to maintain pH 7.6. Add SO gram* (tig.) of Liquid . Aroclor and stis well. Titrate from micro buret with 0.01 N NeOB until the original red oolor of the solvent is restored. A portion of solvent in a similar container is e useful reference in determinin'* the end point. The match ia governed by eatlnetion of the intensity of red because the hue is not exactly reproduced on aooount of the yellow oolor introduced by the Aroclor, 1 ml. of 0.01 H Re GO 0,4 I!gn, HaOB. Calculate in terms of Mm. NaCE per gsa. of sample,"* Report ta 4 decimal nlee. al_of 0,01.NJIaCff I 0,% m g, of nple naon/gm.. XxaapI: If titration is 0,00 ml* for 50 g, of Aroclor, the Acid Number is 0.08 I 0,4/80 0.00064 L?ot* NaDR/gs. Resort as 0,0006, 3olutlsns' Regulrsd Solvent? flix 600 nl. of benzol, 200 ml. of 5A alcohol and 200 ml. of ae#ios#s Add 5 1#' of 0,&% phenol red solution, Ffeesiol Bed Solution, QJ%i To 0.1 ot* of toy indicator in a snail beaker add exactly 2.0 ml, of 0.1409 N HaOH. Itir to dissolve and dilute with 5-A alcohol to 50 si. Reference Buffer pH 7*St Dissolve 0.41 g* t$s3$P^ and 0.89 gn. HsgltPO,* (both Mhydrcms) ia 100 ml* of water. Add 0.5 ml. of 0.2,.' phenol red. 'Solution in used for reference ia adjusting ths solvent if Lefiotte pH 7.6 @olor standard is sot available. COMPANY confidential TRAN 01140? HARTOLDMON0024685 Aeid WuWr of Liquid Aroslara - B - Standard 0.01 I H&CE! 6 ml, of .5 K N&CM to 250 ml. rol. of 3-A al cohol . Protect at all t Lm*s from atmoapherio C0a, . Hot a ' By uslELg 250 al. asefeoas Lb solrsnt Laat^ad of 200 ml. a 100 gm, gaspl of 1254 my b taken for analysis. FABi at 1-30-45 Copied by r 4/23/48, COMPANY CHFIDENTial TRAN 011908 HARTOLDMON0024686 Monsanto Chemical Company Ann Is tea Method Ho. 14-43-48 SJBTXTi Color of Aroolor on N.P.A. Deal LT^TTIQD : Kalllrg Poo'rat Comooratar 3 oops The method is applicable to Aroclors 4445, 5460, or others hoTing N.P.A. oolore in the range 1 to 5. Procedure `.'am the Aroclor is necessary to obtain pouring consistency, rill the test oup of the Hellige Poofcst Comperutor, liodel 605, with Aroclor, insert cup In the comparator, and aoapare against the color disc (No. 620o-0, Lubricating Oils and Petrolatum) whleh has N.PJk. colors from 1 to 5 in one-half steps. Report color to nearest 1/4. Clean the test oup with a mixture of CCl* and benzol, with final rinse of benzol. 4311' oolor numbers coincide with Notional Petroleum Assocletion color number (1915). The relation of the N.PJt. color numbers to other oolor scales Is tabulated below: NPA Color Nos. (1915) NPA Names Onion Petro leum Co. A3TU Color Roe. Lowibond Analysis Red Yellow Blue 200 510 1100 1/4 1/2 3/4 1 1-1/2 2 2-1/2 5 S -1/1 4 4-1/2 5 6 ? 8 -- - - Lily white 0 Cream white H Extra pale 1 Extra lemon pale J Lemon pel* K Extra aran-se L Orange pale U Pala N Light Had 0 Dart Had P Claret Red I --1 0.12 1.5 0.60 2 2.5 2.5 4.6 3 6.9 3.5 9.4 4 14.0 4.5 1.0 3 35.0 6 60.0 7 60.0 8 166.0 0.6 1.1 1.7 2.4 8.0 26.0 27.0 32.0 45.0 50.0 56.0 93.0 60.0 106.0 64.0 - aw aw - .55 .55 .55 1.90 TaStem 1-26-45 Copied by ra 4/27/46 COMPANY CONFIDENTIAL HARTOLDMON0024687 Monsanto Chemical Company l Ann 1 grtoa Mathod No. 14-44-48 CPBJgCTi Color of "'Tatar 7h 11 " Aroclor s 13TTIDD; Cofrrparlson against A.P.H.A. Toala 3oope , The method la appliocble to Aroclors 1254, 1260, or othsra hay Lag oolor laaa than N.P-A. #1 ( ".a tar '..Tim"), A.P.H.A. Ttanderde Thee oolor standards are sold solutions of potassium ehloropletinata and oobaltous ohloride. Tha unit of color is that produced by 1 me. of platinum per liter. The ratio of cobalt to platinum nay be rerled if neoassary to matoh the hue. Because the hue of Aroolor 1254 ami 12 60 seems best matohed without cobalt, this has been omitted In the or e para tIon described. D1 s so It s 1.245 g, of potassium ch loro pint inn te (K*PtCl) contain^ 0.5 g, of platinum In water with 100 ml. of oonoaatrated hydrochloric add, and dilute to 1 liter with distilled water. This solution has a color of 500, Prepare standards from 10 to 100 in steps of 10 by diluting 1, 2, 3 ml. etc. of tha abore solution with distilled vrater to 50 ml, in standard high farm Messier tubes. Protect the tubes from eTsporetion. Refer to pegs 13 of "Standard Methods for the Examination of .'eter end Sewage" eighth edition (1936) for details of standards containing cobalt. Published by American Public Health Aesociation, 1790 Broadly, Hew York. Procedure Fill a matchlng Messier tube with Aroolor to a height equal to that in the standard tubes. Compare with standards by looking vertically downward through the tubes upon a white or mirrored surface placed at suoh an angle that light la reflected upward through the solium of liquid. A solar tube support (Fisher #7-065, 30 ml.) Is oonrenient. Inaranueh ae the proportions of the standard so lor solution in the coraperleon tubes are suoh ae to represent an aliquot part of a liter, the readings are direct aa parts per siillloa. Colors up to 100 are recorded to the nearest 5. Direct comparisons are satisfactory up to 100. Abore this the sample should be diluted with Carbon tetrachloride (saximrn A.F.H.A. color, 5), and tbs color obtained to nearest 10 by multiplying by the dilution ratio. FAB: era 1-80-45 Copied by re 4/2 7/48 COMPANY confidential tran 011910 HARTOLDMON0024688 tonsanto Chemical Company Annie ten Method No, 14-46-48 `TPBJSCT; Acid Number of Tolld Aroclora and Heavy Llculd Aroolors 1ETK0D: Titration ulth Alkali using, Phenolphthala in Procedure Dissolve 50 grams of the Hjoolar in 50 ml, benzene in a 400 ml. beaker, warning to hasten solution. Add 50 ml. 3A alcohol, 200 ml. distilled water, heat to boiling, add 1/2 ml. 1% pfaenolphthalein solution, and titrate, in the esse of the diet Iliad Aroolore with 0.01 N sodium hy droxide solution, to a faint pink color which is permanent for at least two minutae after rigorous etlrrlne. A reecoot blank should bs run con currently. The acidity of the sample is oeloulcted as milligrams of sodium hydroxide required per gram sample. Calculations Using 0.01 R KCR, Aold No. ml. titration X 0.4/samnle weight Tor 50 ga. ~ Aoid No. (ml. tit, ml. blank) I 0.006 Using 0,1 R NhCE, Aoid No. - ml, titration X 4.0/eamnie weight For 50 27C. Aold No. - (ml. tit. - ml. blank) X 0.06 Apparatus 10 ml. burette In .05 divisions. Conversions 1. To obtelm Neutralization Number in terras of XQII, multiply the Aold NuJriber in terns of KaQH by 1.40C. Inverse feotor is 0.713, 2. Uhltiply the Acid Number by 1000 to obtain the parte of NeOH re quired to neutralize one million parte of Aroolor. Thus Aoid Nunfeer of 0.0006 is equivalent to 0.6 parte of KeCS per million nerta of Aroalor. S. The large amount of water used oeusee sharper separation of the aqueous layer from the non-equeous layer, thereby making the endpoint sore really distinguishable. If the titration is carried out against a very light background or In e fluore scent light, the end point la easily seen. 4. Aside fraa free sold as a oaua for NaQH consumption, ferric chloride Bkieh is usually present in nail amounts, also consumes RaCU In neu tralization to phanolphthalein. It therefore follows that an Aroolor of very low acid number rust be ale extremely low in ferric chloride. TAB test 1-26-45 COMPamv TRAN 011911 HARTOLDMON0024689 Monsanto Chemical Company Anniston Method No. 14-47-48 ^IBJSCTi Pour Point of Liquid Aroolorg I.STnOD; A.3.T.M. D-97-39 The pour point of an Aroolor la the lowest temperature at which the material sill flow when It Is ehilled under certain prescribed condi tions listed In AJTU D 97-39. Apparatus Apparotus ooaslsts of teat Jar, thermometer, oork. Jacket, disk, gasket, and bath as described under A. j.T.13. method D97-39, The thermometer is the A.O.T.M. Cloud and Pour Test, ranee -30 to 50 *C. Present eoDeratua Is the Emil Orelner Co. IfcBl 2234 einr.la unit with Or2242 test Jar. Procedure for Aroolcr Follow D97-39 in all respects except that the centiprede scale is sub stituted. Only on outline follows: Add 40 ml. of Aroclor to test Jar. Adjust thermometer to center of Jar with beginning of capillary 1/0 Inch below surface of the Aroolor. '..'arm the Aroclor without stlrrinr to 46*C . 3Lri a bath at 46-48*C. Cool to 32*C. In air or water bath at 25*C. Trans fer the Jar to the Jacket of the cooling bath which is maintained at 0 to 3*C. Becinninc ut a temperature 8 to 10 degrees above the pour point, at each interval of 2*C., remove the test Jar frcm the Jacket and tilt Just enough to determine if there is movement of the Aroclor. This inspection should not retire more than 3 seoonde. './ben movement la not promptly apparent, the test Jar should be held in a horizontal position for exaotly 5 seconds as noted by a stop watch. If movement occurs, imedlately return the test Jar to the Jacket, Repeat test for flow at the next temperature 2*C. lower. Continue the test In steps of even degrees centigrade (14,12,10, etc.) until the Aroclor shows no raovamsnt when the tet Jar is held horizontally for exactly 3 seoonde. This Is the solid point. The pour point la the previous temperature, 2C. above th solid point. The pour point is thus the lowest toraperature et wETcY the liquid will flow or pour under the test conditions. Technicians mast familiarize themselves with D97-39 which rives complete details of apparatus end procedure, reproducibility of results, effects of thermal history, etc. The directions above are inadequate except as a working outline. The both teepereture is controlled by adding dry ice to acetone for pour points below 0C. ?AB:ea 1-3D-4S Copied by rs - 4/27/48 COMPANY CONFIDENTIAL TRAN 011912 HARTOLDMON0024690 Tb Testing of Aroelors for Inorganic Chloride . z ,, volumetric flask, On ml. then ooatg In 2 microgrBra of Cl. Transfer 1, 8, *nd 3 al, port lone to 10 ml. tub. Lake to the 10 ml. mark with Cl free HgO. Place standards end sample in light free box from which only the top of tubes are erpoeed add 0.5 al. of the silver nitrate to aoh tube compare La a specially prepared tast tube rack. The coaperieon is to be made quickly tad from a eons test soiree of light, preferably day light froa a window away from the sunlight. Compari eon is easier when other aouroee of ll^bt are shielded from the comparison reek. Look directly Into the top of the tubes and compere. Bote the known solution ?&lch nost nearly autchea the -rater extract estimating to the nearest whole ml ohogram. The extraot blank and the distilled -Tatar should show no turbidity. Calculation Divide the ohloride content In micro,'-rens of the known solution which raatohas the extract by the weight of the Aroolor rapresented by the ertraot to obtain the ohloride oontent of the Aroolor In p.pja, , In the procedure described, the 10 ml. extract represents 40 -rams of Aroolor (1/5 of 200 g. taken). The three known contain 2, 4, end 6 aicrosrsAs of Cl, thus rearesantlng O.CC, 0.10, and 0.15 p.p.a. ratpeotlvely. Values should be reported to the nearest 0.025 ppm. Precaut Iona Because of the seneitlvlty of this test, serious errors may result through very allft contamination or inattention to details. All equip ment must bra scrupulously cleansed, the distilled water absolutely e hi or Id @ free end testing done away froa fumaa of B31 or chlorine fuaaa. rs 4/27/48 COMPANY CONFIDENTIAL tran HARTOLDMON0024692 UeoBtLoto Chemical Coapa&y Anniston Hethod He. 14-65-48 3UBJ10T; '.star Content of Liquid Aroolors U&THCO: Tltrat lop with Karl Fischer Rearent Outline The Aroolor is dissolved In a mixture of bong^n and aethanol whloh baa been titretad with Fischer reagent to the characteristic end point. Fischer reagent is a solution of iodine, sulfur dioxide, end pyridine. Iodine is consumed as long ae any water is cere sent. The eolution to araln titrated to obtain the water content introduced by the Arcus lor, Solutions and Apparatus Karl Flschar Reagent: Weigh into a flask 264 grans of pyridine, Barrett E~A or Eastman 214-G, and add 61 (mm of liquid or gaseous sulfur dioxide. Add the liquid sulfur dioxide directly from the inverted cylinder by attaching to the outlet Yalta a glass tube extending; into the pyridine. Sulfur dioxide gas oan be bubbled into the pyridine until proper amount is added. Store in a glass stoppered bottle. Transfer 65.6 grans of the pyr idine-SO mixture and 134 al of absolute methanol to a 1 litar Florence flask. Cool thoroughly in an ioa water bath. Add 16.9 grams of iodina, stopper, cool again before shaking. Alternately cool and swirl until the iodine is in solution. Hakes 800 nl of reagent. Store in glass stoppered bottle. Let stand 84 hours before using. 'Then fresh, one ml of reagent is equivalent to about 0.0053 gme. of water. Aroolor Solvent: Mix 8 parts dry benzol with 1 part anhydrous methanol. The dry benzol is prepared by ahaklng the commercial grade with anhydrous oalelua chloride, decanting into a flask and distilling, rejecting the rirst 10>v to cone over. Keep in glass stoppered bottles with minima exposure to air. Micro Burett 10 al. x 0.06 ml. Koch automatic with glass stopoared reservoir. Ick and Krebs #18460. Squlp reservoir with a moisture guard tube containing Drierite or a similar dehydrating agent. Procedure Heat a clean BOO al. narrow south Erlenraeyer flack in an oven ear on hot piste ant 11 thoroughly dry. 9weep out for 10 minutes or until cool with air which has been thoroughly dried by passing thru tubes containing 8 mesh Drierite. Disengage the flask from the esplretiag train and 1me diately close with a paper cap hald by a rubber bead. COMPANY CONFIDENTIAL TRAN 0U915 HARTOLDMON0024693 I 'Jur Content of Liquid Aroeiors ~ 2 Hthout delay, transfer 100 ml, of the benzene-methanol solvent to th flaait thro a Mil hole punctured Lnto th peeper cap, Cover a rein with paper. Titrate at once with Karl Fischer rearat to distinct red-brown end point irilieh does not fade after swirling eeTarml time*. Tbe Flaoher reagent Is dispensed fro the mleroburet the tip of which projects into the flaek thru the punoture In the paper cep. At the end point any water content of the eolrent he been reaoted, Ouperlnrpoe fresh paper e*o imnsdlately, Obtain weight of th eolrent and well-covered flaek cm a T'relon balarwe or equivalent. ^ilokly Introduce with e dry pipette about 100 'ra'se of the lightly warmed Aroclor to be tested. Cower at onoe and neigh ealn to obtain the weight erf Aroolor to nearest gram. Shake until the Aroclor le dissolved. II the mixture la cloudy, warm ellgrtly. If cloudiness persists another mixture should be preoared. Puncture a small hole In the paper cap for th Insertion of the burst tip end titrate with Flaoher reagent to the first dsflalte brown color, agitating with s castle swirling faction. The sod point ehould nerslst through several swirls* The end point may slowly fade through alow aoaeas of ataoapherie moisture in which case it is restored by drop or two of reagent. If not so restored, the ead point may have been a false one or the closure is faulty. A definite end point Is Impossible if humid air la not wall exeluded. From the amount of reagent required and the weight of AtooIot used, cal culate the water oontent in p.p.au Oallbrotlon of Flaoher Reagent and ?tandard 7eter Solution Standard water solution In methanol: Transfer exactly 0.40 ml. of water fraa a micro buret or s 1 ml. measuring plpet to a IOO ml. volume trio flask. Fill to the mark at onoe with anhydrous methanol and mix. One al. of solution thee contain 4000 micro-rams of rater In addition to asy water which may be present in the methanol. Transfer exactly 5 al. of the above standard water solution (equivalent to 0.0S crmj&f of water) to e 200 ml. Urlenneyer flaek which has been dried m& swept with dry air. Close with paper oep and titrate with Flaoher reagent in the some manner as the ample. Ti# end point Is sharp. A methanol blank, found by titrating 5 ml. of the methanol used In asking up the rtezdard water solution to a like end point, aust alvays be aibtracrted from this titration. Divide th* amount of water taken by the net Fisdher reagent required to obtain the titer of the Fischer reagent la terns erf water. Example: A 8 ml. aliquot of standard solution, equivalent to 20,000 microorams of water, required 6.61 ml. of Fleebar reagent while 8 ml. COMPANY * CONFIDENTIAL tran ou< HARTOLDMON0024694 Content sf Liquid Axoelors - 3 f the th&nol retired 9,55 of Fitefessr reagent. 20,000/(6.61 - 0.55) - 80,000/6,06 3500 microrsrana ter/ml. Reealibrations: Rsasoss the Fluchas* rea-ent deteriorate rapidly, it* titer must fee determined for each days use. If the uju standard water solution i used la reoalibration as in the initial calibration, the tltar of the Fischer rea^sat aut be calculated froa its total water contact (including that introduced by the methanol) . Th total water i the product of the initial rross titration and it* titer. Thi ia th exampls abort tha total water content of a 5 ml. aliquot is 6.61 X 3300 ** 21813 ralerograms. If on reoallbration 7.3? ml. of Fischer reecent is 21815/7.37 2960 alerogrsms of mter per ml. Two or more calibrations bould be made with agreement witfeLn 0.025 ml. Calculation of S..0 eengla Standardisation sf Standard BgO eol. Titrate 5 ml. mixture H0 aol. Titrate 5 ml, of methanol Tit of 5 ml* mixtor a A Tit of 5 ml. suihanol - 9 ' A - B ml, reagassfe for SgO added 5/100 of A Divide 5/100 X .4 by A B * faotor grama of HaO/al. Jiiltiply feotor X B giving ss. of H*0 in 5 ml. of methanol. Add this wt, of H*0 to .08 already added giving Bs0 in 5 ml. (Total) Factor m_ HgO St'd Titration * ^ - T|_ X ammpla T1 faction f, Tg X 1,000,mo pjm H*0 wt. imp! ' FAB: am 1-87-45 Copied by rs 4/27/48 COMPANY CONFIDENTIAL TRAN 01LID HARTOLDMON0024695 Pros* Utter to !T,,C.!!./s!.T.Bolsr (HaIowa* Prod act D 1t.,,Union Cert) Id and CrWn Corp,,, 30 S. Forty-Second 3t., W.T. 17, M.VT.^IAL mraBTO no. looo Ho. 1001 o. 1013 Ho. 1014 Color* flow Point ('tod. AST!! Softening Point) dff. F. White to Pal Strew 'Tbite to Pale Yellow Pale Yellow Liquid 194-201 247-252 -P--el-- Y. el, l."r BTf-Zm S .eolfic Gravity at 77 deg. F. 1.19 - 1.25 1.53-1.59 1.65-1.71 1.73-1.81 P-notretlon (!'od. A3TTI) 200-e. load at 77 d. F. 10-15 3-8 8-8 V jcoelty (Saybolt Universal Second*) Di dtillation Ranp (ASTf) dr- F. 33-37 at 77 d/'. F. 400-590 33-37 t 266 ter.. T. 600-660 31--35 at 266 deg.F. 415-656 33-37 at 302 d^.F. *=aeh Point (ASTi! Cleveland Open Cup) dec. F. 203 .284 356 3n Fir Point (AST!! Cleveland Orwn Cup) der. F. Fn-ver Factor at 1,000 ayalaa at 10 eyelee 338 Hone to boillnp: Hone to boiling Hon to boil Lav -- Leas then 0.2!" Lean than 0.2^ Ham than 0. 0 43 0.70? 0,705 l electric Constant at 1,000 cycles at 10 cycle* 0 C. Roaistivity {wo?., cat.) at 30 d*. C. -- 3-6 4-5 4-3 5-6 4-5 4-6 -- Over 107 - 108 Over 107 - 108 Over IO7-10a Copied by Serb V2/ia THAN 011918 CQm p CMFlDC,vnAL k 1 HARTOLDMON0024696 I-A-B-4000 From - Halcmi Products Division Union Carbide and Carbon Caroarstlon 50 last 42nd Street New Tork 17, New Tork Letter - V/.C Jl./J.ll. Cola, Tech. Rap, 8/16/48 Zyrox 3009 (11-313) OENERAI INFORliATIOH Color 3p. Oravlty Softening Pt. 3torner Viscosity 3aybolt Furol Viscosity Penetration et 50*C. Penetration at 25*C. Plash Pt. Fire Pt. Coabustlbility Fraoture Acid Resistance Alkali Resistant* Volatility P.T. at 25*C. (1000 cyoles) Dial. Constant st 25*C. (1000 cycles) DC Resistivity at 2S*C. - Brown - 1.40-1.45 at 23*C. - 79-83*C * - 39-89 at 130*C. - 79-100 at 130*C. - Approx. 15 (200 gn. load) - Less than 3 ( 200 ga. lend) - Approx. 590*F. - Rone to 600* P. - Util not support combustion - Concho14*1 - Excellent - Excellent - Average for 24 hours at 130*0. Less than 0.10 mg./s^.ea./hr. - Approx. .001 - Approx. 1,96 - Over 10 meg. me. Copied by ra 4/2/48 COMPANY CONFIDENTIAL TRAN 011919 HARTOLDMON0024697 From - Haloyw Product! Dl-rlalon Union Carbide and Carbon Corporation 30 East 42nd Street New York 17, New York Letter - VJ.C.U./J.K. Cole, Tech. Rep, 2A6/48 Zjrrox 3007 (11-308) TG3UL DTFCRttvTlCK Color 3p, Oravity Softening Pt, Stonier Viscosity Saybolt Furol Vlaooalty Penetration at SO dec* C. Penetration at 25 das. C Flash P%. Fire Pt. Combustibility Fracture Aold Resistance Alkali Resistance , Volatility P.F. at 23 dag. 0. (1000 cycles) Dial. Constant at 25 dag. C. (1000 cycles) DC Resistivity ot 25 deg. C. - Brovex -1.29 - 1.32 at 25 deg. C. -65-70 dag. C. - 20-27 et 130 deg. C. - 20-30 at 130 deg. C. - Approx. 75 (50 g. load) - Leas than 3 (200 n, load) - Approx. 330 deg. F. - Rone to 500 deg. F, - .'ill not aupport combustion - Conoholdal - Excellent - Excellent - Average for 24 hrs. at 130 dag. C. 0.20 rag./oq^.era./hr. - Approx. .004 - Approx. 3.0 - Over 10 eg. mm. Copied by re 4/2/48 COMPANY CONFIDENTIAL TRAN 011920 HARTOLDMON0024698 I-A-b-40 HARTOLDMON0024699  1C O N HARTOLDMON0024700 COM f* a k \\y r Hi 'J ! I-A-<2-600 Q I HARTOLDMON0024701 COMPANY /vrtunnrMTlAI UUNrlULI'J S IHL From: B.I.0.9. Final Rept. No. 093 APPENDII II. PHTSICAL ;AND C1D-MCAL PHOPCRTUn OF CL0PHFN OILS Item Nos. 1. 7. 22. & 31 Pares 108 - 109 (aa quoted in I. C. Furben'a sales sheets) Property Olophen A30 Clophen A40 Clophen A50 Clophen A60 Clophen A70 Clophsn A80 Form ...................................................... Colour............................ .. .. .. Specific GTuTlty at 2Q*C .. .. SclldIfyLnG Point ............................ Flash Point* ., .. .. .. .. 5hrlnka/ro: ICO* - 20*C 50* - 20*C .. .. .. .. Viscosity ut 100*C.................... .. Bellinc Point Limit at 12nn. of Lercury .. ............................ Lose during FTaoomtion \after 6 Laura at 100*C) .. Liquid Liquid Nearly colourlass Nearly colourless 1.35 1.49 -10*C --5*C 166* 193* (Pensky - Cartons) # 3/v 11*L 67 3; 1.2*E 165 - 195* 100 - 215* 0.037 0.037 Volatility at 20*C ............................ (imm. of Uarcury for 100 hours) He it ConductItity at 40*C (in Calorlos per metre per hour per *C). Saponification Ho................................. at 0.00# 0.095 0.0 Aeh ............................................................ PrrmittiTity at 20*C .................... I3i - ikdcwn Ctrcreth .. .. .. .. I</.alotion Resistance In 0hm.cn. V. small 6.0 -CO.001 200kV/cm. 1 X 10L3 <jo .oos,: 0.091 0.0 V. waall 3.4 <0.001 200kV/cn. 1 X 1013 Liquid Liquid Nearly Nearly colourless colourless 1.55 1.60 12*'/ *30*C 222* 236* In en open crucible 6-; 37* 1.5*E 67 3; 1.9*E Firm Nearly colourless Tlnn, cry stall ins ~hlt 1.7 1.72 - 1.77 50 *C >160*C 240* 290* or -errar . (Penalty - Martens) 5 - 67- - #- 4*K ** 190 - 230' 195 - 25C* 200 - 255* 210 - 260* 0.027 -CO.Olf. 'CO. 009^ <0.009* 0.017 <0.00# 0.0 (2 hr3. at 125 <0.00# 0.007 0.066 0.0 0.0 0.0 V. snail 5.0 <0.001 >C00W/om. 1 X 10 14 V. small V. small 4 - 4.5 3.0 <0.001 <0.001 > 200kV/cm. - > 1 X 1014 >1 X 1014 0.0 V. small 3.0 > 1 X 1014 Clophora arc not combo -r. ible nnd do not- suDnort combustion of materials Into v/hlrh they are impregnated. 0 T - -V -I TRAN 0 1 1 9 2 4 HARTOLDMON0024702 I-A (J) - 500 Stability of Credo P Uycar and Teflon in Aroclor 1254 at 130*C and 45*C Dhort Form ileport No. 2179 File No. 141-27.1 . December 29, 1947 Notebook references: Traith 45137 Credo P Hyoar end Teflon Immersed in Aroclor 1254 Material Terap. Hour a Oa In In ".'t. % Cain in Thicloie se Grade P Hycnr erode P Hycer Teflon Teflon J.30*C 45C 130'C 45*C 285 285 285 280. 68.6 26.3 No fill 8 lb Is Negligible 26 6 Negligible Negligible rs 1/14/48 company CONFIDENTIAL TRAN 011926 HARTOLDMON0024704 I-A-l - 500 From - Meno P.G.B./R .L..T. 3/22/48 Aeravox Corporation New Bedford, Maasachu9etts DetemlnLnc Fluoroscence in *roclor "The ultraviolet llfht '; uoe for determining fluorescence in Aroclor ig manufactured by Geor'-o 7. Ckitc.s and Company, Franklin Square, Lone Inland, New York. It is a CH 4, 100 /att, G. E. Mazda Lamp with filter. "Our procedure 1s to pour a small amount of Aroclor into a 5" watoh class or a 5" Pyrex evaporating diah and obaerre for the decree of fluorescence under the CH 4 lamp, preferably in a dark room. If the sample has been contaminated with Mineral Oil it will allow up as o streaky or milky fluoresoence as compared to pure Aroolor. The fluorcsoonce around the meniscus of cure Aroclor ie not to bo oonfusod with the fluoreeoence resulting froa contamination. "This tost is quclitmtlvo and, os such, is based on the experi ence of the person performing it. 'It keep standard sample for comparison. If there arc any further Questions please fool free to contact us". Copied by rs 4/2/48 COMPANY TRAN 011927 HARTOLDMON0024705 n - 100 December 2t 194? ELECTRICAL DiTA ON ,,ROCLORo Introduction Time hae cot permitted ua to carry out electrical measurements on all of the Aroclor samples sent by your laboratory and as listed In your letter to Dr. C. K. Bump of June 27, 1947, It -roe hollered that dielectric constant, ions factor, and direct current resistivity measurements over a temperature range for e Ion chlorinated and highly chlorinated biphenyl; also one sample each of the terphanyl and the mixed biphenyl and terphenyl aeries would represent the electrical be havior of Aroolora. The tj*end of the eleotrlcsl properties of the samples not measured oan be estimated; l.e. as the viscosity of the \roclors of a particu lar series increases, the loss factor will decrease and the loss faotor maximum (II' within the temporature range measured) will be shifted to higher temperatures. An increase in viscosity will increase the resis tivity of the Aroclor, The dielectric constant of material is a meosure of its polBrizability. Therefore, any ohange in the structure of the mleoule which will Increase its polarizability will oauae an incroase in dielectric constant. Accuracy )f Data The accuracy of the alternating current data is dependent on the dissipation foctor of the dleloctrlc at a particular frequency and a particular temperature. The dielectric constant values are acourete within .2% provided tho dissipation factor la less than 10JS. The error is greater with increasing dissipation factor. The accuracy of loss factor (dielectric constant 1 dissipation factor) is also dependent on dissipation factor, Aroclor 5442 was the only sample which had a dlasi rat ion faotor greeter than 10 and that occurred at the following conditions; 41 *C, 500 cycles . 41 *C, 750 eyolea 35*C, 500 oyolee It will be noted that the dielectric constant* extrapolated to 100*C. ohock satisfactorily with the value* listed in your letter to Dr, Dump. The direct current resistivity values have a 30ft error for the greatest rralstance readings on our Instrument. For lower resistance values the error decreases. Aroclora 1221, 1254 showed an increase in resistance with time whioh is indicative of polarisation effects. For these materials then, resistance was read after the voltage "ms epplled and then at the end of one minute - an empirical method used for taking a reudable value. Aroolora 4465 and 5442 did not show noticeable pola- COMPANY CONFIDENTIAL TRAN 011923 HARTOLDMON0024706 "2 - 13 100 ' December 2, 1947 rlz.etlon effects, even at the high tcnperaturea. Data The dielectric constant of Aroclor 1221 and 1254 is Independent of frequency, The dielectric conntant of Aroclor 4465 end 5442 Is also Independent of frequency at the high temperatures. The liquld-llke properties of 4465 and 5442 disappear at the lower temperatures where dispersion region becomes evident. It will be notloed that the dielectric constant curves (at the lover tempera tures) hate the earns order as those of the corresponding loss factor curves end the inflection regions ooour at the loss factor maxima tem peratures* The loss factor curves of 5442 at the higher temperatures show a eharp up-awing, indicative of o large conductance component in the lose faotor. Similarly, the loss factor curves of 1221 and 1254 seem to be In the conductance region. Aroclor 1221 showed on unu.iual sensitivity in changing lose factor values and os great an insensitivity to change in dielectric constant. It was found that a sample measured Initially at room temperature and meusured at successively increasing temperatures gave different loss footor values when compared to meesurenents made with the initial tem perature high and then successively lowered. Results showed that raining the temperature of the liquid or allowing the material to stand in the open for long periods always lowered the Iosb factor, probably volatilizing the more conducting or the high loss substances in the Aroclor, Below 5000 oycles this effect was very noticeable, the diffe rences inrreaslnr with decreasing frequency. It may be mentioned here that loss factor measurements at low frequencies might possibly be used os an analytical tool or ss a oontrol method of indicating volatile subetanoes contained in ths Aroclor 1200 series. The log resistivity versus 1/T graph is useful as an indication of the chang,e that occurs in resistivity with temperature - or what is related, the change in viscosity with temperature. The actual slopes of 4463 and 5442 cannot be assured since there should have been more measurements made at high temperatures, However these two Aroclor a have a much larger viscosity-temperature coefficient than the other two plots. It is hoped that the enclosed -ranhs will summarize the dielectrlo properties of the Aroclors measured. More complete information or any questions concerning the data will be sent on request. acm/ Copied by re 1/15/48 COMPANY CONFIDENTIAL R. Lerreeult Monsanto Chemical Company Plastics Division Bpringf ield, Ida ssa chusett TRAN 011929 HARTOLDMON0024707 V '' I-S-10 HARTOLDMON0024708 HARTOLDMON0024709 TV_ L./... iA.. 1 ) . COMPANY CONFIDENTIAL 7# --.*/t*T HARTOLDMON0024710 II-B From - B,1.0.3. Final Report No. 893 Item Nos. 1, 7, 32, and 31 Fbhos 12, 13, 14, 15, 16, 4 17 m . COMP D IFHTJfYL 1. General. Chi or ice ted diphenyl is manufactured by I.G. Farben under tne trade narw of Clophen, Gone types are liquid and others solid at norraal tempersturea. They are used as impregnanta aa alternatives to hydrocarbon oils end 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 os T64 is made by 1.0. Ferben, suitable for trans former cooling. The total output of Clophen A50 and A60 for the years 1930 and 1943 wae:- 1939 Type A50 21 tons * A60 132 1943 w A50 170 W IV A60 506 W The coat of the material in Germany i:-- Type A5Q IK. 50pfy. to 1I.T. 60pfg. per Kilogram " T64 1U. 20pfg. per Kilogram. The following is a list of the principal prewar consumers of Clophen :- Gienens-Gchuckert, Berlin. A.E.O. (Hydrawerk), Berlin. Kioafil (Brown Boveri), Zurich, Alsthom, Paris. Duceti, Milan, Italy. Switzerland. It wee stated that no German capacitor manufacturer uses Clophen for the manufacture of small capacitors for radio and telephone purposos end where these have been used by the Ger man fighting services they were supplied by the Italian firm, Ducati. - 2. Manufacture. (1) The synthesis of diphenyl from benzene. Diphenyl is synthesised from benzene as shown in the figure, following:- COMPANY CONFIDENTIAL TRAN 011933 HARTOLDMON0024711 --v'W'v---Condenser Distilling Column S\ 500-650*C - 200 *C Two-stace Host Drchenger Reaotlon Coil 800*0 Synthesis of Diphenyl from Benzene The synthesis occurs in the vapour phase, at 000*0. and atmospheric pressure, in an electrically heated reaction coil of copper-nanconeoe alloy. No catalyst is required. Th appoyatus, apart from the reaction coll, is of iron, and operates at the temperatures shown above, /.bout 10,' of the benzene vopour Is converted Lnto diphenyl in one passage through the reaction coll. The purity of the benzene is of importance for the elec trical quality of the ultimate chlorinated produota and a specification Is attached overleaf. The benzene used was believed to contain 0,2 to 0.3JC of paraffins but little definite information could be obtained regarding any undesirable Impurities or the mechanism by whioh they cause poor electrical performance. Thiophene wes stated to be definitely harmful, and vague reference vb made to "nitro-compounds", to "aliphatic hydrocarbons" and to "substances which could not be chlorinated". The pre iae nature of these materials was not known, but their absence woe ensured by obtaining benzene always from suppliers whose product wos known to be satisfactory,, Analytical Speciflcatlon for Pure Benzene Appearance: Clear and colourless. Density at 20*u .: 0.876 Distilling range: first 5f. within 0.25*0. S* - 95/. " 0.25*0. 95,", - end " 0,25*c. Solidification point; Dot leso than 5*0 . Bromine consumption: Dulphurlc acid test: Not more than 0.5 gm. bromine per 100 c.c. Not more than 0.15 9a, K2Cr2o7 Carbon disulphide*. Shall be free from CSg. COMPANY CONFIDENTIAL TRAN 0L193, HARTOLDMON0024712 Difficulty in the synthesis wan still bein^ experienced, due to rapid corrosion of the copper-manganese reaction coil, operating at 800*U. A smell scale experimental pporotuo using a fused silica coll had been made, but had not beon developed for production use. In addition to diphenyl, ebout 5% each of 1-3 and 1-4 terphenyle are produced by the process. These are se parated, chlorincted and used in seeling Tarnishes; present production is about 4 tone per month. No use is mode of chlorterphenyls as paper lmpre^nants, since the materials are resinous and tend to crack; moreover the permittivities are lower then thoas of the chlordlphenyls. The crude diphenyl is next purified by distillation. During this process the ternhenyls remain in the residue. They ere extracted In the following meaner;- fhe 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 tex-phenyl with malting point of 208*C . The 1-3 isomer, remaining in solution in benzene, is more difficult to Isolate. The solution is clarified with activated char coal, filtered, und the benzene evaporated. The residue is distilled to yield 1-3 terphenyl with siting point 80-64*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 passes. In. The addition of chlorine is continued for 100 hours at a rate of 130-135 kg/hur during which tine the tem perature is raised gradually from 110*C. to 130*C, The end point of the chlorination is determined by measuring the density of the product. To remove hydrogen chloride formed in the process, dry air is blown through the liquid for 2 hours and this hy drogen chloride is recovered. The product Is transferred to another vessel and treated with 1/25! of solid sodium hydroxide, heated and agitated. The sodium hydroxide is allowed to settle oat and the Clophen drawn off from the top, transferred to another vessel to which Fuller's earth and soda are added and the liquid redistilled. The stills for this process are gas heated. COMPANY CONFIDENTIAL TRAN 011935 HARTOLDMONOQ24713 3 Prcpcft Le b ,, ' , (1) Capacitor impregnating grades. A surjnury of the physical and chemical >rocertiaa of the capacitor lrapregna ting trades of Clophen la given in Appendix II, Thera m six gradeo of capacitor iBpregncrnt, A33, A40, etc. up to AflO, the 7, 4, 5, etc, indi cating the number of chlorine radicals combined ",1th the diphenyl. Tech grade contains a proportion of the adja cent homologuea not erceedlag 2Of.. Grade A30 has the highest value of permittivity. Theoretically the highest Talue obtainable -vith s chlorinated diphenyl Is 9.0, and a grade haring a permlttlrlty of 7.0 has been prepared, but is cheniotlly unstable, and very sensitive to moisture and impurities. The most eonnonly uoed grades are A50 and A60; A50 is the most stable grade and has the lcriest dielec tric loso. &-ade A60 is conaldered by 1,0, to possess the optimum combination of non-inflammability, stability and riecoaity. Aa urlth Gibran, It is considered that no addi tives are required since the substances are stable in use,, provided that the capacitors are efficiently sealed against tho air. t:icufll of Zurich are the only users of <130 and A40. Tho following table shows tho variation in capacitance and povjcr foctor with temperature for a Clopben impregna ted paper capacitor. Tho lmprecnant is A50, tho dielectric is Ochoeller and Hoeoch "A" finish reg tissue (density 1.2 - 1,25) with a thickness of 10 d; froouoncy of measurement is 000 o/s. Power factor shows a maximum value of 0.052 at about M*CV while capacitnnne falls off by some 2Cf at temperatures below thia critical'value , Variation In cc.pecitance and pcroor-factcr with temperuture for a Clophen-impregnated capacitor. Temperoture (*c.) Relative Capacitance Power VactoT -60 0.07 0.035 -40 0.91 0,024 -20 0.94 0.013 0 1.02 0.048 4 1.06 0.052 (rasx.) CO 1.10 0.006 40 1.10 0.005 60 1.10 0.004 80 1.11 0.005 No evidence was obtained from I.G. on the use of any of additive with a view to depressing the temperature which the change of state occurs. COMPANY CONFIDENTIAL TRAN 011936 HARTOLDMON0024714 The method adopted for evaluatin'' the '.Tatar content In oils such ss Clophen ia described In Appendix III. It Is also applicable to 3uch solids as Nlbren, rn/ielhardt stated that no source of failure had been ex perienced durinr the whole period of production of Clopben, which is about 17 years. Consequently no improve ments or nodificetions had been mde or found necessary during this period. (2) Transformer-coolin'? ryadc (Clophen T64) . No detailed infaristion was sought on this material, since it is unsuitable as a capocitor lmprejment and is only used as a ooolont for tranuformers and phase shifters. A summary of ite physical and chemical properties la civen in Appendix IV. It haa a low viscosity, la moderately stable under electrical stresses and has the distinct ad vantage over mineral oils of beln^ non-inflammable. The principal users of this product are A.E.O. and "Jlemene, but It is understood that, as with other chlorinated ecropounds, consorvotism end prejudice amonc customers have prevented its wider use. No stabilisers are added to the material a a their function of absorbing hydrochloric acid would be defeated by the formation of "chloride salts", which In turn become elec trolysed. It was ssid to be very important to avoid con tamination of Clophon T64 which may occur In transit and for this reason the use of leather for raskets must be avoided. 4. Methods of use, precautions, etc. No details were obtained on the method of impregnation used by I.G. for the construction of test-specimens of Clophen-impregnated capacitor. This was pertly coused by the non appearance, after the first day, of Engelhardt, but it is not considered likely that any novel processes are Involved, For information on the precautions necessary in the use of Clophen, teti lection II, 5, above. r 12/19/47 COMPANY CONFIDENTIAL TRAN 011937 HARTOLDMON0024715 IIT-A-t - 500 ">on - R.1,0,0, Final heport Mo, P93 Item tJos. 1, 7, 02 and 31 P0 x It Clophen Is mode In several rT-dos, which oorrecpond closely with their U.3. counterparts, A,50 beinc the crude moat commonly used for capacitors, t L'xcept for very rare use by "Uemons and rialnke for special orders, Clophen hc-a not been used In Germany for amall capacitors of the tele communication typo, but it hes been ueod extensively by Olenons-ichuckert for pov/er oapacitors. It la interestin." to note that the German forces used Clophen imprecated and filled tubular capacitors mode by Dueatl, of IJilan, who obtained the imprecnont from 1,0. The prejudice apsinst Clophen vraa, however, boinc produnlly overcome and several manufacturers were oontemplatinc an extended use of this material, Gome of them con sidered it to be equal to or possibly hotter than mineral oil for opera tion at power frequencies. ro 11/2^/47 COMPANY CONFIDENTIAL TRAN 011938 HARTOLDMON0024716 III-A-b-50 FTora - B.I,0,G. Final Report Mo. 893 Item Noo. 1, 7, 22, end 31 Pap,os. 98, 99 (2) Clophen The only chlorinated impregnant used by GiemensGchuckert is Clophen, supolied by lo0. In power factor correction and hlph roltage applications It Is consider ed practically ideal* The only type of Clophen used in bulk is A.50, pentachlordlphenyl, (corresponding to Aroelor 1254). A.30 end A.40 have been tried and found unstable, A.60, A.70 end A.80 ure too viscous to allow for pood irapregnatl on and have lower permittivities. Although the viscosity of A.50 at room temperature Is much rreater than that of oil, the viscosity at Impregnation temperature la sufficiently low to give do trouble in attaining thorough inrpregpna t ion. A routine check on conductivity Is mode on each drum of Clophen, and formerly if the conductivity were too high, the Clophen was treated with po?/dered chalk to neutralise the free acid. As the result of continual pressure on I.G. over a period of years, the acid content had gra dually diminished, and It la now possible without chalk ' treatment to work to the same rejection limit of resis tivity as for oil, vlx. 1013 ohn..em. at 20 *C. Drums of Clophen foiling to pass the conductivity test are returned to I.G., unless urgently needed. A certain elasticity is permissible in view of the hi^i standard set- Apert from conductivity, further acceptance checks are specific gravity (1.54-1,55) and permittivity (5.0 5,2). Permittivity is measured at 800 oycltjs and 20*C. on a Gchering bridge at low voltage. The acceptance standards for Clophen A.50 are shown graphically in Appendix XXXIV. Clophen costs about 1 li. 60 pfg./kg., and la therefore much dearer than oil (30 pfg./kr.). This extra expense ia offset, however, by the use of a special design whieh reduces the amount of Clophen required. An ad vantage claimed for this iapregnant Is that Is has a similar permittivity to paper (via. 5). Other lmpreppanta studied. As Clophen la considered nearly ideal, no serious attempts have been made to find superior moterials or addi tives to improve Its performance, This ettitude Is sup per ted by service experience, in whieh no failures have been reported. It is realised, however, that on froezing discharges nay oeeur in the eoatraetlon voids, whieh may result in decomposition of the Clophen and failure of the COMPANY CONFIDENTIAL TRAN 01 L9 39 HARTOLDMON0024717 dielectric. Tests were performed (see 'Section 17, 2, (3)) to check whether this depredation does in fact occur, end no failure we3 noted. Nevertheless, 1.0. supplied snail samples resembling Clophen A.50 but having a lower melting point so thut this possible source of failure r. >uld be Investigated. De pression of the temperature at which the dipoles bacerr* lrmoblle should raise the maximum usable frequency and hence broaden the range of applications by introducing those ror eudlo-frequenoy furnaces. Two of these I.G, sonnies, with references A.1621! ond A.162N, are, like Clophen, rode fron benzene, but hare a lower chlorine content because of the presence of un additional alkyl croup (CnH2n`,T) Qn(5 hence a lower density. Their advantage over Clophen A.50 is that the setting point (l.e. tamporcture of maximum dispersion and of capacitance diminution) la lo-.vored from -0*C. to -17*C, The permit tivity, viscosity and non-inflamroblllty resemble those of Clophen A.50. The viscosity/temperoture curves of these two samples, K.7 mineral oil and Clophen A,50., are oompared in Appendix XX0CV. re 11/19/47 COMPANY CONFIDENTIAL tran oh9ao HART OLDMON0024718 III-B--2500 December 22, 1947 TO: PHO-!PlI..n.' DIVI3I0N 'AL'T^'J JJBJ: Arcelor 5460 oe Used In Tthylcellulooe Lacouer RE: Federation of Paint and V u ra l a h Production Clubs Official Digest (October, 1947), Aroclors used as plasticizers aDd reslno Import excellent Qualities to ethylcellulose. Ethylcellulose Is used In lacquers of vurlouo types, the ethylcellu lose acting as a lonr chain oolyner to Impart toughness and flexi bility and to Increase the speed of drying. Come of the prlncipol uses for ethylcellulose lacquers ore for the ooatlne of high tension Ignition cable; heat sealing locouers for foil and paper where the slight discoloration which may develop in nitrocellulose luoquere on heat sealing is not permissible; linoleum lacquers whore alkell resistance lo essential; textile printing; printing inis, particularly in multicolor dosirns wlro hydrocarbon solvent does not soften or blood into previously printed designs; ulroroft lacquer for rcaistunce to both heat and cold and to nuiolc temperature obanmes; record lacquers, especially for home recorders; and in wood sealers where good saDding and flexibility ere essential A good pigmented ethyloellulose lucquer bus been made, based on the following fornula: Ingredients Ethylcellulose N-22 Aroolor 5460 T103 Menthylphenol Toluene Ethanol farts (by weight) 6,4 6.4 4.2 0.06 67.0 16.0 100.06 rh Copied by rs 2/2/48 Benignus COMPANY CONFIDENTIAL TRAN 011941 HARTOLDMON0024719 IT1-0-300 From - fie*10 G.Y. Frankle/P.O. Benlrnus March 11, 1948 Soil-Poison Conoentrcte As desoribed belou, the -.e materials are formulated Into a v/ater emulaifloble soil-poison ooocentrate carrying almost 30 per cent by weight of uotlve lnpxedicnts. Aroclor 1242 Triohlorobenzene (Mxed isomers) Pentochlorophenol Isopropyl alcohol Toluene or Xylene Sterox 3E* Santomerse 3 Paste 33.5'/. 33.5 10.0 3.3 16.7 1.5 1.5 100.09: * Other non-ionic type emulsifyin* events auch as Triton NU or Span and Tween oon be used to replace the Storor 3E. Coplod b;i rs 4/2/48 COMPANY CONFIDENTIAL TRAN 011^2 HARTOLDMON0024720 Chemical Abstracts POl'IQLF. U'JE OF APOCLCfm Vol. 41 Page 6067 ni-H-io U.S.P. 2,425,973 to Anderson and Coalahan, (Hercules Powder Company) . Foundry cores sprayed with 15/ solution of chlorine ted naphthalene in hydrocarbon solvent show /Treater scratch resis tance thoD untreated cores. Cl2 content remains from 40 - eo.) Cla . Particularly rood for use "fith '.1 castings. ro 12/2/47 COMPANY CONFIDENTIAL TRAN 0119A3 HARTOLDMON0024721 IY-10 FTsm - B.I.0,3. Final Keport Mo. Syj Iten Nos. 1, 7, 22 and 31 Pares - lo and 11 Much loss trouble hes boon experienced with chlord 1 ohenyl thnr, with ohloraaphthalene , probably because the fomer, being liquid, in volves lee* physical Contact in disposal. (2) Prevention. Very thorough washing of ell areas of the akin likely to be contaminated with solid, liquid, or fumes has always beon the basic principle in prevention of skin troublee, and in still looked upon ao fundamentalo '/hen fatty soaps ceased to be ovailoble, because of the di version of fats to food, it became essential to Insist upon the use of barrier creaius, of which the best was one named "SUIJ.IBO", raede at Tromraersdorf. This has now been replaced, for lack of supplies, by an alternative mode by I.G., named "MITIGAL", which is considered inferior to 'uimbo but satisfactory. The Flsaan firrii put up a special powder named "'-'.CTTFELTOLVFRn to act as a barrier, but this was found to be inefficient except to allay Irritation on skin areas exponed to fume3 only. For this purpose it still finds use at Leverkusen and at the Hydrawerke faotory at 3erlin. . A special point io .`node of fume extraction, and the minimum uir speed away from the operator is 1 metro per aeoond ,, To chock the efficiency of the precautions, a thorough exami nation is made every 4 weeks of every worker coming into contact with chlorinated hydrooarbons, and since the enforcement of the precautions, no deaths or symptoms of internal Injury have occurred. Tinea superfatted soaps have ceased to be available, a cleansing composition containing dlchlor-fnethane has been devised. This is so powerful a detergent for chlorinated materials that barrier creams are considered unnecessary, but it is uncomfortably Irritant to many ski ns. (3) Cure. hen severe attacks or ahloracne and internal sickness were encountered, in the eerly year*, when the properties of chlorinated materials were not well understood, extensive rest periods had to be prescribed, together with a generous diet, entire absenoe of further contamination, end long periods In tie open. Tines precautions Have been token to minimise the effects, only a few mild cases of chloreene have been met. Thea have been treated with a solution of acetic and salicylic adds In methylated spirits. COMPANY CONFIDENTIAL TRAN 011944 HARTOLDMON0024722 2- (4) Cooclualona and Recommendstions. 1.5. oooaldor that neither toxicity nor skin affection need now be any deterrent to the use of chlorinated naphthalene, and that chlordlphenyl is if anything 133 troublesome, Certain people, notably those "1th fuir skins, show distinct ollorcy, and are boat diverted to other work not lnvolvinr contact. Ccrupuloue cleanliness of the skin ( lnclufiing the face, neck, and arms) and of the clothier (esnecially iindirrcrments) I3 ossential and needs strict enforcement. fashing v/ith hot water and good soap is sufficient, so long as the soap is superfatted,, since tho skin beco/nos sensitive to irritation by alkali, Barrier cream should be used on those parts of the skin which oome into contact with solid or liquid material,, and the area of contact should be minimised by tho use of protective clothing and gloves wbero possible. Areas of the akin wnioh ore contacted by furaoo only, and particularly those ohafed by olothing (e.g, the nook adjuoemt to tho edc of the clothing) need protection by a suitable soothing powder. .'here fumes are generated, thoy should be drown sway from tho operator at an air speed of at loost 1 metre per secind, It may be found essential to hove two ducts, one at floor level, end one overhead, with exhaust in two directions simultaneously. In case the procautions are being, e7udpd, or lest there should bo seme idlosynoraay, monthly medical inspection is desirable. ro li/24/47 COMPANY CONFIDENTIAL TRAN 011945 HARTOLDMON0024723 IY-3-100 From - The Journal of Industrial Hygiene and foxlcology Volume 20, Humber 2 February, 1930 I'ORPHOLOCICn'l CR^OCO IN T1F LIVT1(3 OF R.n REX'LTINO FROM EXPOXHl' TO CERTAIN CHLORINaTI'D im>ROC.d?BONO * Chlorinated hydrocorbone, particularly chlorinated nuohthclenes tmd ehlorinuted diphenyl, h:.ve been used extensively in certain In dustries. Tbelr uoe in the rrmnufacture and nreoarntion of many typea of electrical equipment Is constantly lncreaeinr. Although It Is known thot some of tber.e compounds cause acne, only recently hes the possibility of more serlouo oyntemic effects been recognized. The present paper describes tlw> pathological chanros obserred in rots that had been exposed to vuriou j chlorine ted no'hthslcno c ors** pounds and to chlorinated diphenyl., Compound (V (chlorinated diphenyl) was administered to two 'rouon of animola in low concentrut 1od3 . ,un uvorume concentration of 0.57 mgms. por cu. m. wug employed 16 hours dally for 134 days In the first experiment. In the second expsrIr.ont (employing on overure sir con centration of 0.93 mgns. por cu. n.) the snimal3 -'ere exposed P hours dally for 143 days. The present experiments demonstrate that chlorinated noohtholene compounds and chlorinated dlphonyl ore c&pablo of producing mnrkod liver damage in the wh lt.e rat without demonstrable ml croocoilc chjnncs appearing in the other' org-.ns. Furthermore, the characteristics of the liver looions resulting from comparable amounts of any '-iven com pound are the aamo, regordlc os of the method of administration (inha lation, feeding, or subcutaneous lnjeotlon). Of the various chlorinated hydrocurbona tested, ohlortn ted di phenyl guTe evidence of bolDg the ;oo9t toxic. '/hen administered by Inhalation In very low concentretiona (overage 0.57 to 0.93 m'-me. per ou, m.) liver cell changes were very pronounced after the first exposure period. The /post striking chango t the hyalinlzation of t the oell cytoplasm ( aeo fig. 6, piste III). Such cellulor alterations were essentially unchanged after a 2 month recovery period. In these animals small eublethal doses of Ourbon tetrachloride and alcohol uni formly produced extensive liver necroslo and was highly fatal to there (firs. 1 and 2, pluto VII). Chlorinated diphenyl fed in small doses nrodueed similar but more marked liver injury (see fig. 5, plate III). In large doses this compound was highly fatal. The liver ebonies In animals dying, after short exoosures viere inconaolcuous end consisted mainly of swelling, of cells and active regeneration (see fig. 4, plate III). However, animala removed from exposure before beinp' fatally HARTOLDMON0024724 -2 - poisoned, subssquently developed hyaline degeneration of liver cells alallar to that produced by prolonged ud-nln lstrotlon of small doses of this compound. Thus the results of the -recent study, as rail os certain field studios that hove boon mud (1) surest tf-.ot the solution of t ho in dustrial hazard Involved Is dependent largely on a reduction of the air concentration of those compounds to a level that -fill not oroduce liver daraore. The present experiments indicate that lovrer air con centrations must be obtained in the case of the more highly chlori nated naphthalene oomoounds and chlorinated diphenyl than for tricolor- naphthalenes if a safe environment for 'TOrkmen is to be assured, he- cuuse of tlie pronounced toxlo effect of snail doses of carbon tetra chloride on the 1 Ivors of an Louis already injured by exposure to chlorinated naphthalenes and chlorinated diphenylits use as e sol vent for thnee compounds vnuld apneor to be very hazardous. ro 2/3/49 COMPANY CONFIDENTIAL TRAN 011^7 HARTOLDMON0024725