Document 6J6YEOQmV45qYO7qQozq3GM4

& ~ROCLCR B..T~ BOOK Tob No. 171-451 Til# No. 141-27.1 April 27. 1348 R. S. Xnlffht RESEARCH DEPARTMENT ftotpiwti DWMm <.Uz ------ ^-------1 Monsanto Chemicals .1 COMPANY CONFIDENTIAL TRAN 011867 STLCOPCB4025083 RZFQRT WO. 2218 7IKAL RIKRT Q* THIS REPORT AND THE INFORMATION CONTAINED HEREIN is TmJ PROPERTY Of TH MON SAN 10 CHEMICAL COMPANY. AftOCLOR DATA BOCK Job NO. 171-401 nit Vo. 141-27.1 RXSSARCS DCTAiffUgff - PHOSTHAg D17151 OR Annirtoo, Alaban Raport 9obolttad - April 27, 1946 Cboalata: A.V. Illanburf H.R. Inl#2it Praparad by: R J. Inigbt Xlc&taaa oopiaa aaro aada of thla raport aad dlatrlbutad follow*: . So. 1. Eimrofa Til* Vo. 2. HI. 7Bklaa - O.B. Dartla - r.p.lo. S. B.R. Colo - R.3. vaabborly Vo. 4. V.T. IXirrott LaValla Vo. 9. H.T. Yaavar Vo. 6. 0-4. Hoolwwlt . o. 7. X.P. Buekor lo. 8. Mftf 1. Hardy Wo. 9. 7J. Rootoi Vo*lo. ]0. JJ. Root*a 11. A Jl. llloabwrg o. 11. 2Jl. lalrfit . lo. 19. Vo. 14. lO. 17. Vo. IV. Tila la oopy Vo. /3 COMPANY CONFIDENTIAL ' TR*N 011968 STLCOPCB4025084 hs'sarch DzPAimzm - HioipiL.n: oirriiar MCWTAJfPO CH22CCA1 CO'&'JFT Anniston, Alsbaaa 6. 5. 2. . k 2. * DATA BOOK Qensral Information on properties of Aroelor#, AtooIot process 4*U, uses of Aroolors, and physiological sffacts of Aroelor#. TORJ.IOFP Aa a means of presenting the available data on Aroalora to the in terested personnel within the Konsento orranitatlon, this looaalaaf aotabook la being oonplled, , Moat of tha dots ha a resulted froa work carried out within our on organization. Literature reference*, however, will be cited la all oaaaa throughout the eonpllstlon la order to allow acre detailed infor- aatloa to be obtained by the user. . The following detailed outline is for foellltetlnr the location of date in tha book and to assist in properly Inserting new date sheets. Ieoh Aroelor is to be given e series nuaber for location under the General heading,*. This aoheae at present is as follows: Aroelor 1221 - 100 series Aroelor 1232 200 earlea Aroelor 1242 - SOO eerlea Aroelor 1246 400 aarlaa Aroelor 1234 SOO earlaa Aroelor 1260 m 600 aarlaa Aroelor 1262 m 700 aarlaa tooAroelor 1266 - 800 aarlaa Aroelor 1270 - aarlaa . Aroelor 1271 - 1000 eerlea Other Diphenyl Aroelor a - 1100 aarlaa ' Aroolar 4469 m 1900 aarlaa s Otter .High Boiler .'.roelore m 2100 aarlaa ` Aroelor 9442 - 2400 serlsa Aroelor 9490 . 2900 sarlee Aroelor 9469 3600 aenas Aroelor 9466 - 2700 eerlea Aroelor 2969 _ 3000 aarlaa Related Compounds - 4000 eerie e TRAN 011869 COMPANY CONFIDENTIAL THIS REPORT AND THE INFORMATION CONTAINED HEREIN IS THE PROPERTY OF THE MONSANTO CHEMICAL COMPACT. STLCOPCB4025085 -2 - Tbs pegs pertaining to the solubility of Aroelor U63 in nrlrai solvents wuld be of thle typo "IAJ - 1300*. In eases where the lnformotion for all Aroclors can ba compiled on ona sheet, such as refraetIt a Indices, the para will be Inserted under the fcenersl Hesdinf and 111 bear ooly the ounber for the first ~roelor, for example, Lih - lOO. I, snreuL Ffcor'iirrisi or ,,roclor3 A. Ptajreioel Properties (a) General Fhyaloal Constanta 1. Jornula and aoleoular wei^it 2. SpecifioatIona for Manufacture (b) Density and Specific Gravity (c) Cubloal Coefficients of Expansion . (d) Vapor Praaaur# and Pat# of Praparatlon (a) Specific Haat and Seat Capacity (f) Thereal Conductivity (g) Vlaooslty y - (b) Rafractlva Index . . (1) Heats of Vaporisation - Other Thenaodrneiale Properties (J) Solubilities (h) rinsh and Plane Points (1) Uiscellnneous B. tlectrlcel Propertlas (a) Dleleotrlc Canatent a (b) Poeer Tactora (a) Dlelactrls strength (A) Volune Resistivity (e) Dipole Konents (f) Miscellaneous COMPANY CONFIDENTIAL r**N o",cl STLCOPCB4025086 -3 xx. Jcrnccs or iwotactorx* A. Uoaaacto Prxui 1. Raw ifctariala 2. Chlorlaatloa 3. Diatillatloa A. 3toraga aad jhlppla* . B. Caiman Prooaaa C. Othar Proeaaaaa III. U3M OF i\R0CL3 , A. Ilaotrioal 71aId .' 1. Traaafor*ara . 2. Capaaltera 3. Coat lag for Tlra 4. Otbar aaaa B. Vara1ahaa C. Plaatlaliara D. Hydraulic Fluid I. Fira Ratordaata F. Hoatlag aadluB l 3. Xlaaallaaaou S. . 3MB*rtiosa for aav Caaa if. nmioLoosAi PTrjw 1. 3kla Taata B. ( <?rataaatlo Taata I ' pram mwo aroclor9 COMPANY CONFIDENTIAL TRAN 0U3n STLCOPCB4025087 Thn boot la aubjoot to rewialon and ehan*aa nrloua daU art I oca tad. Orapha and dlagrana will b lnaertad whan poaalble and naw grtjpha drawn a a Information la oompllad. No lndloaa of aaetlona la plannad ,ut thla tlaa, but latar ralalona naj laeluda auch pacea If the woluna of Information warranta It. Contrlbutlona of naw and auiplanantary data ara aamaatlj ao- lieltad. Any dlaorapanelaa la tha axlatlnr data or adwiea aa to a battar maaaa of praaantlnc tha Information *111 ba graatfully ackaow- ladgad. Addraaa all oorraapondanoa to tha froup loadar In ahargw of tha raaenroh on nroolors at Fhoaphate Division - Resaareh Department, Ann1atanf Alabama. R. S. Knight rs 12/2/4T # % COMPANY CONFIDENTIAL TRAN 011372 STLCOPCB4025088 m k* STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE Dm3ION ANNISTON. ALABAMA Pi|i N. PRODUCT: ,, GRADE; Arftfllor U2I-------ntrafla--------------- CODE NO.: 'O4O-C2B-73-O0 S0^oi9S!ES?l^i_ PROD. DEPT. NOj _______________ ________________ <TTPFP<FDFA ri*--r>m^tlTa B,L*X. | ,\UUE.| T.E.n.l P.AJ, APPROVED BY (Initial*) ^-lo-ar, -------------------- -- Control Specification Cou Spacificaboa Crude Aroaler 11211 ~tp, Or. at 68*0, Aoldlty, ttr,. riaCn/flB. ( Aroolor 12311 ' Oolor Aoldlty, me. Naai/m. Tp. Or. at 60/13,5*0. Chlorine contest Visooalty at 10C*F 1.150-1.160 A 0.5 40 :J*U aax. 0,01 nax. 1.145-1U50 CO.3-21.3,; 30-41 9 NOTESe Copied ty r 4/8/ COMPANY CONFIDENTIAL tram oua73 STLCOPCB4025089 er - * STANDARD SPECIFICATION OF Mox&axto Chemical Compant PHOSPHATE DIVISION ANN ISTON, ALABAMA Pmfa Ne. PRODUCT. Aroolor 1238 CODE NO.: 1040-33<^>?s^ GRADE: Bculr PROD. DEPT. NOu ____ SUPERSEDE3i.."w^T*cVatWg ^W#| A*V*K#| 7.A.B. APPROVED BY (Initial*) 12-17-48 12-1B-46 12-19-46 19-ia-44 Control Specification Couunur Specific*tWn Qmd* Aron lor L132t Tp. Or. .1416117, BaOr/cju Aroolor L23i ir Color Aoldlty, ir*. RoOH/i. yp. Or. at 69/18,9*0. Chlcrin* oontnat riaooaity t 100*7, 1.840-1.840 <.0,8 90 -PH* aax. ,01 nx, 1.235-1.840 31.5-5J.8 46-49 173 NOTES: ooptN f ra 4/B/40 COMPANY CONFIDENTIAL TRAN 011874 STLCOPCB4025090 3TA5CMP 3PSC gTCATICW cr MDTTSAJfrO CHBgCAl COMPAJfT Produot: Chlorinated Diphenyl. dletlUedCod# Ho. l040-e40-73-09 Qteflei AroolOT 1242 ' Dote Authorize Juat 21. 194D Supersede# Speolfloatlon Dated Jaly 3. 1954 Tolerable Llalti Typioel Value 3p. Or. at &5A5.5*C. Color, WJJi. Aoldlty, Vffi NaOH/i. Tleoool ty at 34.4C. 1.338 to 1.548 0.5 lfexlmia .01 Uazlnam 47 to 50 Seeonda Saybolt Universal Approved by Approved by 1. Chief CbaKlet Mw. A. 0*1--1, Tt. lorfce Mu* gar Approved by Bobert 3. Soother!Kr3alee Woe per Authorlied by 7, I. Oerothere cbeKieial bireeior Copied by re 4/8/48 COMPANY CONFIDENTIAL TRAN 011875 STLCOPCB4025091 'TTAJCtAJP gysCinCATICB 0* . mcwsawto cksmical coupawt Produet: Chlortaated Diphenyl. distilled Code He. 1040-260-7*5-09 Oradet Aroslor 1248 Date Authorised June eiT 1940 Supersedes Spsslf ioetlon Dated Toly 3. 1934 Tolerable Limits Typloel Talus 3p. Or. at 60/XD.5*C, Color, W.P.A. Aeldlty, MgnNaCty'ga TLsooalty at 54.4*0. 1.404 to 1.414 0.5 Maxima .01 thxlma 69 to 76 Seooads Saybolt Universal Aroolor 1262 Op. Or. at 90/15.5*0. Color, W.P.A. Aoldlty, Mgn WaOR/^. Tlsoosity at 96.9*0. 1.572-1.585 1.0 Maxima .01 Maxima 86-100 505 Cods Wo. 1040~310-7S-09 Acrrotad by A. B. Oarbar -----------1------- CkTgTWsT Approved bp Hi. A. O'lsal. Jr. works lkaaffer Approved by Robert 5. Weatherly _______ Sales Qsaapr AatborlMd by 7, W, Caret hers___ ohciioal director Copied ^ ra 4/8/48 COMPANY CONFIDENTIAL THAN 011876 STLCOPCB4025092 3TAJCUPD S*1CITIC TI01T . or MDWSANTO CrmriCAL OOtCPAHT ' Product Ajoolcr 1354_____________________________ &<* Ho. 1040-280-75-09 Dlaleotrlo____________________ ___________ Authority _Jjfi/3/41 gaperaadae*. 6/el/iO Color, AFHA 3oale Coedltlem Specific Gravity at 88/18.5*0 Acidity, UfiP. !taaa/(?M Inorgml o Chleridea, pja. 3aybolt Tlaaoelty at 98.9*0, ae. Dlalaotrle Ooaetaat at 100*C Realatlvlty at 100*C, ofia-ca. at 800 valta Refractive Xadex at 28*C Dletllllng Ranee, Obeerved, 10* Obeerved, 50* Obeerved, 90* Pour Point . Satar, pjm. . fvaporatloo, 6 Era. at 100*C Corroalon Teat-Cbenee In welebt Acidity after teat Inoraanlo^ChToridee after taat Condition after teat Color ' al'ter taat ra s/u/4 100 Ifcx. Clear 1.495-1.805 .01 0.10 thx. 44.5-47.8 4.15-4.38 Above 800 X M1 1.8370-1.6390 S60-3B5*C 388-368*0 388-375*C 8 te 18 38 Max. 0.4* 0.0* 0.01 0.10 Uex. Clear ISO Hex. COMPANY CONFIDENTIAL TRAN 011877 STLCOPCB4025093 STANDARD tpec uicaticw or UCW3ANT0 CHEMICAL COMPACT Proust: Aroolor 1160_________________ Co** * 1040-g90-73-09 and*: Dlelactrlo______________ ____________ 0*t* Authorised UJWU Supersede*: 1/30/36 Color, ARIA 30*1* Condition 3 poo Ifla OreTltj at 90/13.5*0 Aeldlty, Il0i, ItaOE/ga. laorganlo Chloride*, pps. 3ajrbolt Vlaooaltj at 98.9*0, see. Dlalaotrlo Conateat at 100*0 RaaiatlYltjr at 100*C, oha-on. at 300 volt* Refractive Index at 88*0 Distilling Ranee, Observed, 10$ Observed, 80$ Observed, 90$ Poor Point Water, pj*. . preparation, 6 Bra. at 100*0 Corrosion Teet-Chang* In selght ao id it7 after test Inorganl o~fchlorld*s after test Goodltlon after test Oolor a?t*r test 100 Uax. Clear 1.330-1.560 .01 0.10 lfcx. 78-00 3.6-3.8 Above 300 X 10* 1.6433*1.6463 370-377*0 377-308*0 388-400*0 16-34 S3 lfcx. 0.1 $ 0.0$ 0.01 0.10 lfcx. Clear 180 Max. rs 5/11/48 COMPANY CONFIDENTIAL TRAN 011878 STLCOPCB4025094 as 3 a V PI S5 COMPANY conrdNT'al TRAN 011879 STLCOPCB4025095 C 4* ** STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON. ALABAMA P*f No. ____ PRODUCT: KTT*iar <1 l^amlnt)-------------------- CODE NO.-. lct&-4acHr3^a------- ________________________________________ AUTHORIZED; QctnMr A, 19,44 PROD. DEPT. NOj ____________ n,LJ. i APPROVED BY (Initial*) __________ ___ SUPERSEDES:_JaaAJL-JL24i n.r.;.i p.l.i iuu.i 1,,n ifJ TfH*m** HWadi Iflidrii--------------- Control Spedfication Conaumer Spocificaboa Appeuraaoex Color, N,P/'..* loftealn? Point (.i.c,r *u.) Aold I'Tusber (U&aon/fr.) Crystal Unity eLear, li.-fit 701100, brittle reals 2,0 W. 60 - 66*0, 0 - .036 \ No. epee. * Hal aloft eolor lllt to 2.0 nozlnan 1 rofrw4i4 beoeuoo Uianeetian rooordo ehov that all loto produced la 1944 hare bad a eolor of 1J&. NOTES; Copied >y T9 4/8/4 , COMPANY CONFIDENTIAL TRAN 011880 STLCOPCB4025096 STANDARD SPSCinCATICft cw MONSANTO CHEMICAL COMPANY Product ; Chlorinated High BoilerCod# Ro. lQiO-taO-TD-ot and#: Ajoalar 3460 Date Authorised IMy 10, 1940 Supersedes Specification Dated Deceaber 23. 1932 Tolerable Llalts Typical Value Appearance Color, H.P.A. CryetelllAlty Teat Softening Point, A3TM . Acid Number Mgi RaOH/gB. Chlorine Clear, light yellow, brittle reala 2 .0 mart win To pans teat 100 - 108.8*0. 0 - .05 59.0-80.6)1 Approved by A. B. Oerbar______ Chief Chaaiet Approred by IRw. A. O'laal. Jr. Corke Manager Anproeed by Robert 3. Weatherly. 5/6/40 --------------------- 9alea Manager Authorlxed by 7. R. Carothare. 5A0/*0 Chwtleel Director Copied by rs t/s/te comply ^fiDntial tran 011881 STLCOPCB4025097 Monsanto Cbealoal Coopanp Anniston, Alabama Aroolor Test llathoda and Designations 3peelflo Qrrrltjr of Aroelora Total Qilorlna la Aroelora Ooftanln* Polat at lolid Aroalora Determination of Iron in Aroalor Plaab and Plana Pointa Vlaooaity at Liquid Aroalora Distillation Rang# of Aroalora Kraporatlon Taat of Liqnld Aroalora Rsfraetira lad ex of Liquid Aroalora Realatlrlty of Liquid Aroelora Dialaotria Constant of Liquid Aroalora Aaid Nuabar of Liquid Aroalor Color of Aroalor - KFA seals Color of Aroalor - AlUA seala Aold lumber of solid Aroalora Pour Point of Liquid Aroelora Inorganic Chlorides in Aroelora Datar Contact of Liquid Aroelora 14-10-48 14-13-48 14-17-48 14-81-48 14-84-48 14-89--40 14-81-48 14-82-48 14-84-48 14-39-48 14-86-48 14-42-48 14-43-48 14-44-48 .14-46-48 14-47-48 14-48-48 14-68-48 COMPANY CONFIDENTIAL TRAN 011882 STLCOPCB4025098 Uonaento Chard oal Conpmny Aonietoa Method no. It-10-48 Specific Qravity of Aroolara The taaperature at whleh the gravities of liquid Axoelora are taken arlaa with the vlaooeity of the liquid. Note the temperature at wtiloh the gravity is to he taken for the Aroelor under teat and heat the eample to 10*C. above ,thot temperature. Pour the hot smnpls Into the a teas or hot water Jacketed hydra* tar jar provided for thla tart. Stir well with an aoourote themoaeter and adjuat the temoereture to the dealred point by ooatrolllnr the steam or hot meter feed to the Jaekst. Continue stirring until the temperature remains constant for half e minute. Allow the hydrometer to sink Into the liquid, than reed the hydroneter aoale at the point of the lower meniscus and raoord with the temperature. Report tbe speolfio gravity to the nearaat 0.001 unit. STLCOPCB4025099 t Monsanto Chaaieal Company Aanletoa Method No. 14-15-46 3JBJSCT; Total Chlorine la Aroclora ICTHOD: Volhard Titration follorclnc Peroxide Puelon Chlorine lb Aroolors nay be detemlned by fualoa of the sample -with odlua peroxide la a Ihireeee-Parr fualoa aup, extracting, the fualoa rrltb mter, acidifying tha eater extraat with nitric aold, aad nr*, olpltating tha ohlorlaa by addition of a axoaaa of cIItct nit rata. After filtration, tha axoaaa of allyar nltrata la determined by ti tration Mmlaat potaaalua thiocyanate, uala<* farrlo a-wwalua aulfata aa Indicator. Apparatua l%a fualoa cup uaad la tha Surge*e-Parr sulfur Bonb No. 3 for flame Ignition. A laod gaakat la uaad. For Ignition, tha boab la auapandad through a 1-&/16" rouad hola la a 1/8" traaalta olata. Tbla allows tha fualoa oup to axtand throurh tha olata for about 3/8 laeh. Ignition la affaoted by strongly heatlap tha bottom of tha fualoa oup with tha full fiaoa of a Halter burner for two minutes. Tha bomb, raskets, and tbo aodlun peroxide ara obtained from tha Parr Inetrunent Company, Molina, Illlaoli. Charge for Pualon Tha fualoa mixture la aada un of about IS rxaas (oaa natal aeoop) of aodiua paroxida aad 0-3 .grans of finely powdered oana. sugar. The reagents should be free from ohlorlaa, or a blank run and corrected accordingly. Ifce fusion mixture la mall mixed by plaelaw tha la/>?edlenta la a ana 11 glees atopparad bottle aad shaking vigorously. A measuring spoon for ttaa sugar la convenient. riOLID AHOCLCR3s Tha non-cryate Ulna type ara walrhad la tha fom of small pallets* These ara prepared by heatlar tha .uroelor until a eoaelatanay la raaahad as will permit dropping It froa a glass stirring, rod onto a tinned surface (a oaa top), eaoh drop formin': a pallet. Jhan aool these pallets oaa be reacted from the eurflce by inserting a spatula under than. .4 frame ara used. The pallets ara brushsd into tha botton of tm fualoa cun and tha fusion mixture nlnoed on top of than. After tiptoeing tha lid, tha chnriRe la ready for fuel. The oryatalllha type Aroolora ara welched la the pothered fom. >4 graaa being uaad. They ara charged In tha anna manor aa tha non crystalline type* COMPANY CONFIDENTIAL TRAN 011884 STLCOPCB4025100 Total Chiorla# 1a Arociara -8- LITin) AJtOCLQRS: 0 to .50 pram* are weighed by dro -- log frca a stirring rod onto a piece of tMn hemianherleslly shaped glees or ,1/2 ivlotla oapeul (QolatLa Capaulee No. 00 United Drug Company, Boaton - 3t. Lcule), which ha a been Juat nrarloualy tarad and which remaina on the balanoa. Tt la necessary to heat the wore'Tlacous Aroclora to "dropping" consistency. The piece of claee than easily alldea off the bc.lnnoe pen into the fuel on eup. Carer with the fuel on mixture.. ft* following quantities of e-splc, auger, and AgflOj are used for tl reepee tire ehlortne eonteatai Cl C intent 0* - 90* 50* - 40* 43* - 98* 501 - 66* 66* - 70* Procedure *tcht of Sample 0*9 grama 0.3 rrans 0.3 grana ' 0.3 PFWM 0.3 prams . Amount sur 0.5 g. 0.3 g. 0.3 g. o.s e* 0.3 g. 90 ml 50 ml 50 ml 75 ml 100 ml Place the fualoa eup, vhleh aontelna the prepared enable and fuel on mixture, in the translte lwltlon plate and apply the full flame of the Ueker burner to the botton of the fualoa cun for B minute a. (CACTIQE: Do not stand too near the fualon durlnr lmltloa. The use of e safety ehleld la reeenaended.) Then renove the flame end oool under the tap. '.'hen eool remora eerww oop. Thoroughly rlnee the oup oowcr with water, collecting the rlnata*e la a eleaa 400 ml. banker. Sian plaoe the fueloa eup on lte aide la the beaker end oower with e wetoh clone. 50-7 ml. will be In the beeker from rlnalne the oap, and thie le euffleleat to decompose the charge. Rewoce the eup end rinse well* '.'hen decomposition is complete, rinse off sower-glees and add purs a10,, with stirring, until sold la present la exeeaa to the extent of aboat 10 ml* (About 90 ml. of told ere required.) Add exactly 90, 70, or 100 ml. of atnndard ailwer nitrate aoiution from pipet (depending upon chlorine preaent) and atlr to affact eoemlatloa of allvmr nitrate precipitate, filter with auction through am aabeatoa pad oa a 1-1/E" perforated poroelalA plate end we ah beaker and filter 4 tinea with anil port tone of oold water. Allow the filter to drain eanplately between washings. Transfer the filtrate beek into the 400 ml. beeker end rinaa the flank twlee, addin.- the rinelar.e to the beeker. Add 5 ml. of ferr la iron Indicator to the solution and titrate with standard KCH3 eolutloa until a distinct pink tint le Juat obtained. %%Z ial TRAN 011885 STLCOPCB4025101 Total Chlorlai la Aroelare -3 Caloulotlon of Chlorine Content t Subtract the volume of KCItJ required from the volume of KCTI3 required to tltrata the amount of etondard ac^03 solution used. TMa will o^vq the volume of KCIfs aqulTalaat to the chlorine In the aeriDle. Multiply the to lone so obtained by the chlorine value of eeeh ml. of KCWl end divide by the weight of sea->le taken. for example: If 50 ml. of silver nitrate solution la equivalent to 61.4 ml. of RCR3 solution and the value of 1 ml. of KCNS solution is .003770 wan Cl; them if it is found that O.S '-ram of sample mi owe a SEN? titration of 10.4 ml. the percent of ehlarlae la: (61.4 - 10.4) I .003770 X 100 _ 64.09* Cl .3 In oaae the fualon mixture or other reagents oontaln oh lor Ins, the amount mist ta determined and deducted fra the chlorine found. 3olatlone Required Standard k&Os Solution: Diaeolva 22 (Tens of silver nitrate in eeeh liter of vmter. Proteot tbs solution from light. standard SCN3 Solution: Dissolve 10 "rama of ICR1 in 1 liter of mater. Perrie Iron Indloator: Use a asturoted solution of ferrlo amonlua alum, about 50 g. par 100 ml. of water. Pure Nltrlo Aold: Stoek aeld suffices provided it is oolorjasa. It can be boiled in .a beaker until oolarleaa if naeaasar~ using 600 ml. HM03 and 300 ml. of ^0. StandardlnatIon of Solutions .sigh 0.3 at4 0.19 rru portions of purs dry RmCl into saps rats 600 ml. beskars. Add 290 ml. of dlstlllad satsr to sseh and 10 ml. of purs 50* altrls ssld. Vibem solution is complete, tdd 50 ml. of standard ARs solmtlom TTm plpst. Stir sail sad filtsr ttrough am asbestos mat om s pmrformtsd porosltin plats, using sustlom. Tlash filter sad transfer ^ flltrsts bask to tbs beaker la the asms manner as when working with s earn Is. Titrate tbs filtrates with standard ICRS solu tion, using farris iron, indloator. Tbs value of 90 ml. of AdR* so lot ion la terms of ICRS solution Is found by sobtrastlng tbs ml. of ICRS solution in titrating tbs O.S gram of RaOl from twloe tbs number of ml. of ICRS solution used in titrating the 0.19 gram of laCl. company STLCOPCB4025102 Total Cllaria* la Aroolars -4- This valus la ahacked by titrating 30 al. of AgfO, .olutlco added to 400 al. of water and 10 al. of pure 30> *0S with KCUs solution. Thl titration should agree very cloaely (i 0.1 al.) with the value found froa the tltratloa of ftaCl. The titration suet be nade elowly to avoid drwlaaee error. 31aoe jura RaCl eontalaa $0.68^ Cl by theory, the value of the XCK3 U terns of ehlorlne my be found by dividing the weight of ohlorlne In the 8aCl taken by the ml. of HERD equivalent to the eilver nitrate required. Szajaplet Two 0.3 gran port Iona of HaCl ahow BDK'3 tltratloae of 13.11 and 13.13 al. ' . Two 0.19 gran port Iona of ItaCl show 8CN3 titration* of 37.38 and 37.3d al. The KS7f3 equivalent to 80 al. of AgN0| la than (37.28 37.24) - 13.12 or 61.4 al. By tltratloa of 90 al. of AgNOf against KOn solution, it la found that 61.36 al. era required. Thla erreaa withIn .04 al. of the value obtained fron the RaCl titratlona. The ohlorlne value of the XEN3 la than, .6066 X .3 divided by 61.4 13.12 or .003770 grame Cl per al. of SO83. The ehlorlne value my alao be ealeuleted froa the titratlon of 0.1S gran of ReCl. 0.6066 X .19 divided by 61.4 - 37.26 rives .003770 grans 01, per al. of KCH3. Preeautloaa 1. The fusion natarlals have explosive properties If handled Improperly; ooneequently ears nast be taken to use safe proportions, to aaoura a good alxture free of largs lumps, and to croparly seat the oovar of the fudoa sap* The fusion alxture anot be kept away froa -itr or aolst sir, either of w) ieh my lgalte the oharga. The fusion airfare sbould not be ground to reduo* lisp*. 2, Tb* aetfeod as daeerlbad la not appiloabl* to volatile organla eanpounde anleae precautions are taken to avoid lose of Maple during weighing. Iffeet of Terloblee 1. On aeoount of the high ehlorlne eentmt of may of the Aroelors and the Mall mount of am*>le taken, greet noeureey le retired in weighing, tronefer, and aiming of the Maple. The pi pet and buret for meeurinr tha standard solution# vast be very clean to avoid drainage arrors. _^ COMPANY TRAN 011887 CONFIDENTIAL STLCOPCB4025103 Total Chlorine In Aroolora 9 2. raalosj which show black carbon dsToeltee on the cover and aid# of tho fusion oup may or nay not "It# the full ohlorln# content. If a carbon deposit la fcxind, a second fusion should be made ueinp a staller sands or reducing the enount of sugar in the oharme or both. 3. The temperature at whloh the standard solutions are standardized should be noted. In case root temperature# vary from this tem perature, approprints volume correction# should be made. 4. The fusion mixture materials should be essentially free of chlorine. T e chlorine oontent may be determined by natclar e bleak fusion, that Is, without addition of sample, and titrating la the usual wy, yive al. of AgNOg may ba added instead of SO ml. cart ions of A^O, solution in like volumes of solution end nitric sold. Heferenoss Beam!A: Determination of Organic Ilalorene, lad. Eng. Cham., Anal. Ed., 6 392 (1934). Copied by ra 4/20/48 COMPANY TRAN 0U388 STLCOPCB4025104 Hona*nto Chmiaai Cospany Anniston L'athod Jfo. 14-17-48 -PBJnCT:_ "oftsalnc Point of Telld Areolora UrfflODi 3aU aBd ri^ This -Mthod la a modification of tha A.I.T.'i. standard 'wthod of tart tar softening point of bltuninoua materials, serla' designation: 3 28-597, Tha method dlffara from tha standard raathod la that tha rln&a are largar than apaolflad. A two ring support la alao used la order that two taata nay ha mada alraultanaoualy. Apparatus Tha apparutua eonalata of tha following: (a) Two taparod brass rlrva, 3/8" Inal da dla. at bottom, 11/16" laalda diameter at top usd 1/4" deep: thickness of nail 3/32". (b) Too ataal balls, 3/8" dlamatar -.wlghtr*: 3.45 to 3.35 :x*ns aaoh. (a) A 800 al. Orlffln lor forn >e*ker. (d) A rl% support for tha two rlncs ha Inc a braaa olata axaetly ->ne inch balow tha Plata supporting tha ring, (a) A 300*C. A.3.T.-. low dlatlllatlon tharreoaetar gr-duatad 1*C. Preparation of tha qaapla Tha sample shall ha malted oad atlrrad thoroughly, oroldisr orarhaatlnT or Incorporating six hubhlaa In tha mass and than rourad into tha rlnr o u to leave n elicit areaaa on eooliac* Olnoa tha Aroolor a shrink oona id archly on cooling, tha rlnr should ha rail fIliad, nearly to over flowing. A llttla of tha azoass should ha drawn over tha top of tha ring at aararal point* so as to prevent tha ooolad Aroelar rron dropping out of tb* ring. In tha saa* way, tha saeond ring, la fIliad with a atandard Aroalcr of known softanInc point. Tha standard Aroolor should hart a softening, within at laast 10 to 15*of tha Aroelar being tastad. Tha rlnra whlla balar fIliad ahould rest on a laan oan lid or on a braaa plat* whloh has bssn amlpaaatad to prevent tha Aroelar from adharlnc to It. Iba Aroolor la tha rlnss ahould b* fully ooolad and hardanad bafor* jrooeding with tha taat. Prooadura m ' Add wool aolutloa (swploy water for softening point between 0-80"C, glyeerla for bebweac 80-500"C., mineral oil for above 200*C.) to tha baakar until tte surface of tha aolutloa la 8" abort the Plata holding t)M rings wfaoa tha rine support is suspend ad in tha baakar. Place tha rinfti oostaining tha Aroolor to be tastad and tha standard Aroolor on tm ring support. Plata a ball an tha osdbsr of tha upper surface of tha Aroelar in each ring, 'Suspend tha thermometer so that tha bottom of ths bulb is level with tha bottom of tha rise* aod just aldway bo- twean tha two rings* COMPANY CONFIDENTIAL rR1N ous9 STLCOPCB4025105 Softening rout of Tolid Aroelor* - 2 - Place beaker and apparatus os a 6 Inch round hat nluta and heat at suah a rata that the temperature la ralaad 5*C. each ralnuta. Th* temperature reoordad by ttaa thermometer ot the laatant the Aroelor taiohee tha bottom plate la reported aa the softening point. The heat ing la continued until both Aroolors hare dropped to the bottom 'lata. No oorrootlone are made for enerraat stem. * Notes 1. The standard Aroelor la run alonr with the aanpla under test in order to oompeneate for variations In rata of tor,tin?, dilution of glyoarln, and thamono ter variations. 2. Tha softening point of tha standard sanpla la determined by rtnicli^ eatera 1 datamlnntlona ualng fraah glyoarln and earafully chaeking tha rlea la temperature of tha glycerin ao that it la aa naar aa poaalbla to 3C. per minute. 3. The slycar In nay ha used repeatedly for tha testa after rm-.oval of tha Aroalor. 4. Bensol la used for olaanlng the rings and belle. 3. ' star oan be ueed Instead of glyoarln for softening points up to 90*C. 6. Tor softening point a abort 100*C, -all boiled glyoarln should be used. Tha usual glycerin la not satiafaotory abort 123 to 130*C, ' it boll* with lota of water while tha temperature remain* praetioaily constant. It la wall to hare n aupoly of hlrb-bolllar, glyoarln on hand to be used only for softening point* abort 100"C. ?. Air bubbles o* the rings and ball* during tha teat ahould be avoided aa far aa poaalbla. B. Tha rata of rlaa of temperature of tha rlyeerln ahall be uniform for each minute after tha first 3 minute a of beotlnr and not ararmged orar tha period of tha teat. TAJ: am 1-81-46 Oopiad by ra 4/20/46 TRAN 011890 STLCOPCB4025106 L'o&sBfiio Cbanlcai Company Anniston Uathod So. 14-21-48 3PBJTSCTt Dateralnatlon of Iron la Aroalcy Iron La Aroalora nay bs iitamlnai by rtraatloc a banzai aolutlon of tha Aroalor with dlluta hydroahlorle aold antLI forthr aztraotiona show so appreciable iron oontant. The Iron in tha eaablnad axtraota ia than-daterainad by dlohrcaata titration. Proaadura Tran afar 3-10 grana of aanola to a olaan aapnratory funnal of about 130 al. oopaolty. Add about 30 nl. of bansol and ahaka until tha anspla la la aolutlon. Than aolutlon la oonpleta, add 10 nl. of 1:1 Iron-free BCl and ahalea for about 2 ninutee. Let auad until separation of tha two layara la oonpleta, then draw off and preserve tha aeld axtraot. Add anothar 10 nl. of 111 OC1 and shake again. Draw off tha aold layar aad oonbine with tha first axtraot. Contlnua until HC1 layar la elaar. Detarnlna tha Iron by naual dlohroBata titration aathod. 7AB:ea 1-31-48 Coplad by ra 4/21/48 TRAN 011891 STLCOPCB4025107 Mon#*ato Chanloal Company Anniston Method 'Jo. ODBTSCT: LiTIDD t n* ah and fla.'aa Po<"ts Clara Land Open Cup The flush aad flan* point* of Aroolor *h*ll b# determined la the Cleveland Open Cup Teater, following the prooedure described In Asm `"v D 92-33. Apparatus The oup shall be supported by a as tel plate 1/4" (.639 oa) In thick ness and 6 inches (15.24 om) la width. The plate ahall be of brass, east Iron, wrought iron, or steel. In the center or the ilat* ttmre shall be a plan* depression 1/98" (.079 oa) in depth, aad of Just sufficient diameter to fit oup. There shall b* a circular opening 8 3/16" (5.90 cm) in diameter, cut thru the plate, oenterlir with tha ocnter of the above mentioned degression. The plate shall b* covered with a sheet of hard asbestos board 1/4* In thickness, and of tha same shape as the metal plate. There ahall be eut in the center of the esbeetoe board a circular ho la Just fitting tha oup. Heat may ba supplied from any convenient source. Tha uaa at a ras burner, eleetrle bee ter, or eloohol lamp la parmlttad, but undsr no elrauaataneaa are products of com bustion or frsa flams a 11owed to oone up around the eup. The souree cf heat ahall be oentsred under the opening la the plate and shell be of a type that will not produce loeal superheating. If a flam* heater 1* ueed, It any be protected from drafts or excessive radiation by any suitable type of shield, that dues not project above the level of tha upper surface of the aabestoe board. The therraomater shell conform to the requlrs.-asnta of themaneter Ho. 8. (Tee A3TO table of thermometers). Procsdure The thermometer shall be suspended or held In a vertloal position by any suitable devloe, the bottom at the bulb shell be 1/A in. (.639 oa) from the bottom of the amp, and above a point half uay between the center and beck of the eup. The oup shell be filled with oil to be tested In mich a manner that the top of the aenlscua Is exactly at the filling 11ns at room tmaporatur*. Tha surface of the oil shall b* fro* from bubbles. Tlr* shell be eo oil above the flUlar. line or outside of apparatus. The teat flame ahall be approx limitely 3/38* (.897 cm) in diameter. The test flam* ahall be applied es the temperature read an the thermo meter rceehee each suooesslv* 5*T mark. The flame shall pass In a straight line, (or om tbs circumference of a circle hawing a radius of at least 6 inches.) aarees the eanter of the cup aad at right angles to the diameter pasting thxm the thaxnoaeter. The teat flam* *11, *11# passing aeroce the surfso* of tbs oil, be la the plane of the upper edge of tb* ip. tbs time for the pa aear* of the test fleas serose the cue shell be acvcxl- aotely 1 second. COMPANY CONFIDENTIAL TRAN 011392 STLCOPCB4025108 71s ah and Flane Polite 2 The oil shall be has tad at a rata not exoecdlnr 30*? oar nlnuta tm- noratura rlaa till a point la reeohed a v-roxlaetely 100*? below the probable flash point of the oil. Thereafter tha rata of haatlnr shall ba da or # sad and for at lsaot the last 50*F bafora the flash point la raaohad tha r-ta shall ba not lass than 9*7. or more than 11*F per minute. . Tha flaah point shall ba taken as tha temperature reed on tha thamonetar whan a flash ap'eurs at any point on tha surface of the oil. Tha true flash must not be confused with e bluish halo which son*times surrounds tbs tsst fleas. After determining the flesh point, the haatlnr shall ba oontlnasd at tha spsolflad rets of 9*7 to 11*7 par minute, sod application of tha test fleas aha] 1 ba mads at the apacified intervals until tha oil lrsltes arid con tinues to burn for a period of at least five saconds. Tbs method of application of the flane shall ba the asms as for flaah point. Tha tem perature read at tha time of tha fleas application, which causes burning for s period of five seconds or nore, shall be reoorded as tha flans point. Tha flash point and flane DOlnt testa shall ba made in a room or com partment free fron air drafts. Tha operator shall avoid breathing over the surfaee of the oil. It la deelnble that tha roon or compart- sent nap ba darkened sufficiently so that the flash nay ba readily dim- oarnibla. Note Aroolora 1248, 1254, 1260, and hl-her chlorinated Aroelors do not have a distinct flaah or flane point below their boiling temperatures. FAB:am 1-26-49 Copied by re 4/21/48 COMPANY TRAN 011893 STLCOPCB4025109 Monsanto Chsnlcnl Coapnny Annlaton Method JTo. li-29-43 'PBJTCTt Llgl'aaP: Tlacoalty of Liquid Aroslcrg 'Saybolt Unlraraal, A.3TM D 88-44 Viaeoaity Is a naaaira of raaietanea to flow. It la aaaaurad by tho time naoaaaery for a ohoaan Toluaa to b foroad thru a tub# of ehooen length and internal dlaaeter. By thaory tha Tlaooslty of a fluid la related to the aTerage dlaUnea boVraan lta noleoulea and to thair rag# epeed and their alze. Apparotua Tlaooalaatar aeoaitbly with oil tuba, hath, rsoalTer, tbaraoMtara, strainer, tlaar, and plpet to neat all raqulrananta of ASTIM 0 88-38. Tho Tlaooalaatar sow In aaa la aada by Kraba Xiao, and Ufg. Co., Ifaw fork, purobaaad froa FJtll Oalnar Co., thalr 2-tuba eapaolty fees. On# tuba - on loft hand - ha a bean cart Iflad by tha Bureau of Ttenderds. Prooaduro Tha Tlaooalaatar la aat up In aoaordanea with mnufacturers direction# ueing Ifo. 20 motor oil for tha bath. Tha prooadure and mathod of reporting raaulta ara thoaa daoerlbad undar A3TU D 98-44. Cara of Apparatua Bath: At eonelnaloa of taat, opaa tha contact point# until 1 or l Lnohaa apart ao aa not to rut undua atrain oa t hemostatic control whan both ooola. Put a faw dropa of oil la notor eupa oeaaalonally. Keep outalda of both wipad fraa of oil or Areolar. Corar with hood whan not in uaa. Maintain propar laral of oil by oeoasloaal additions thru hola in frost. Thu oil blaoks&a, dl riantla, elsaa baatara, tubas, and orifloan, than refill with fraah oil. Oil Tuba: Alla atill hot. ranora all possible Aroolor frot gall ary withpipet. Than aoolad to 70-60*, fill tuba and gallery with benzene, drop thru orlfloa into beaker, drain -allery with plpat, ropaat with aoatona, and wlps dry with absorbent papar in such a "ay that fihara eanaot fall Into tabs. Ropaat until aloan. Oeaaalosilly aorar tha laathar pluarer with alzad thin papar (*eopya . COMPANY CONFIDENTIAL TRAN 011894 STLCOPCB4025110 Tieoosity of Liquid Aroelcre - 2 - sheets) and *ib walla of tuba before ualQf' cleaning fluid. Tbie keeps sails pollebed. Carer oil tubes with lldi when not in ues. Orlflosi orlTToa'. foroepa. dean. Do not paas wires, strlarrs, pipe cleaners, etc. thru the IT a hair falls across orifice, raicrre with long handle IT tha orlflae beoones cloeeed, dismantle apparatus to Calibration Cheek the tlaar occasionally for 60 second oerloda. Cheek bath tharKsmetar from time to time. Cheek performance of Tlseoalaeter osriodieadly by running a reference sample of Arcelor oa which careful deter minations hare been aade. Available for eallbretlon Is also an oil standard, called "Alnha 48", of the Aaerloen Petrols* Institute. The oil is obtained fron the Atlantic Refining Company, Philadelphia, Pennsylvania. Because suoh oil standards ere subjeot to obanre they are cheoked annually. T/vB:* 1-31-43 Copied by rs 4/21/48 Company TRAN 011895 STLCOPCB4025111 Chemloel Company Vaalstac Uethod No. 14-31-43 TTBJTCTt Distillation San<*a of Liquid ^roelort *TTI0D t A.T.T.M, D--20 with Mod If loatlona The apparatus, oonslstinc of flask, eondmssr tubs, shield, and thsrnoaster, is exactly ths cane ss described under A.g.TJt. tert D-0 "Distillation of Bitumlnoue Ksterlsls suitable for Hoed Treatment". Attach a 6 inch auxiliary thermometer (0 - 150C.) to distillation thermometer, Pines bulb half *ssy between top of oork and orobeble averuGC of distillation ra&ne. Cover both thermoneters with a 3/4" diameter glass tube to Insure a unlfora temperature oorraction for ths exposed stem, baroaetrlo pressure end thermometer error. The procedure Is cbnnced only to the extent that thermceter readings are taken whan specified peroeatcres (usually 10, SO, and 90^) of Aroclor have been distilled instead of following the A.^.Ta:, proce dure of velgil&g the distillate between speoifled themaoeter res dines. In testlnc liquid Aroclors, 100 rps. of snple ere welched Into the diatllllnr flask end distillate received In a tared flask or beaker resting on pan of a Torsion balance with 100 p?n scale. Procedure ,'elgh out 100 grama of sample into the distilling flask. Aeeeobla apparatus as described under A.S.T.M. 0-20. Ineert thermometer (A.'.T.U. high distilling 0 - 400*C.) thro eork in the neok of the fleek ee that the top of the bulb is level with the lowest point of Juncture of the tabuleture end neck of the fleek. Apply heat to the fleek supported on two sheets of 20 nesh wire ^use ao thet the first drop oonee over La fron 9 to 19 minutes. . Cpnluet distillation at rate of 90 to 70 drops per finite. Collect distillate in n 290 nl. beaker tared on e balance. Tate temperature readlnc* t 11, 3?, H, 101, 80%, 901, 4051, 901, WJJ, TO', 801, 90f., 991, 991, Ml, 971,. sad dry. Correetioae for enereent atam and pressure are applied to the thermo aster readines If required. Take correction readings st first drop. Id, SOI, 901, and dry. Be port the temperatures to the nearest 1*C. Dample: (Trposed stem In decrees) X (tenpernture difference in degrees) X 0.000198 decrees stem eorreetion ne srpoeed stem is read from the top of the mrk. The temperature differenee is the reading of the thsmnaatnT mime the tenpereture of the auxiliary theroaneter. COiVc-Ajsyy CONFIDENTIAL TRAN 011396 STLCOPCB4025112 Olftlllatloa Raaft of Llqpld Arcelor* - 8 - O.OOOU T\ & b boroeotrie correction norml bollinj point La deer*** abaolata; A jf ahanra La traasura froa 760 i. Eg. Tba eorreatlon la added If barortatar la balo* aarml and aubtraated If the barcaatar la aboea oonal. (UaeOouwll - "Thamodynaraloa and Cbajalafery* pp. US). Corraotad Teaperatura Obaarred taaparatura Tl t Ti. ' TAB tm 1-29-48 Coplad by ra 4/88/48 CGMrA.viV CONFIDENTIAL TRAN 011697 STLCOPCB4025113 ttoneanto Chemical Caapeny Annlctom Bethod No. 14-32-46 UBJICT: gveporatlon Teat of Liquid jgroolara CTHOD: 6 Houra Heating ot 100*C . AST.' D6-39T - T'odlfled Prooedure ,/eigh ob a roupfc bolanoe abwit 30 rroma (* .3 ge.) of tfaa wall mixed Aroolor lato am aoeurotely tar ad t La box, 33 cn, 61a. X 33 on. deep (3 os. Olll-etyle ointment box, deep pattern), Tleher #1<480. Let rtand until box and aaapla era .t roan tamperetura, than weigh accu rately. Fine# tba box la a ventilated oonveotlon oven maintained at 100*C. 1 1* for 6 hour*. Remove, cool in deeloeator to roan temperature tad aoeurataly rewelgh. From the loan In weight calculate the evaporation In per oemt* Report to aeoond deelmel olaoa only. Note# 1. Be aura box la at room temperature whenever exact weight la taken. 2. The oven 4>oulfl not contain other semnlea which might Interfere with evaporatioa n. 3. Beeauae the evaporation loea la aenaltlve to tei^erature, the air bath met be oloeely maintained at 100*C. ' FAB:am 1-29-48 Copied by re 4/23/48 COMPANY CONFIDENTIAL TRAN 011898 STLCOPCB4025114 ltaiMAto Cheoloal Conpeny Ana If too Method *o. 14-34--49 . ' krilHOD: Rcfrnctlre Index of Liquid AjooJi^^t^ Abbe Refrnotoraetsr Refreetire Index The refraetlr* index of any medlua la defined *e the ratio of the r*looity of light la air to the reloolty of ll-ht la that mdlua. It la neaeured by the ratio of the alae of the laeldaet ancle to th* alna of the angle of refraction. The deoeer the aedlua, th* -neater la tt rafractloa toward the normal (higher rafraotlT* Index). Because the rafractlTe Index la cbereeterlatle of each substance, it la ueeful la identifying 11 quid a end Tariffing their purity, la detemlaing the co la ou la r structure of organic compounds, aad la aoae quaatltatlT* aaalyaea of alxturee. Aa applied to Aroclor testing refraetlr* Index pro rides a Tcrlfleetloa of oonposltloa aad purity. Apparatus Abbe Refrsotaaster with soeessorles, Bauseb aad Lomb, Cat. #550, Serial Bo. 377. Calibrated to rood directly la terns of rafraotlT* index of th* D 11a* (eodlua) at a temperature of 20*C. Proodur* Operators should b* familiar with the Bau*eh aad Loob Direct lone f* Use" aad traetle* the Manipulation as ther* 4*sot 1 bed before atteatptlag determinations oa Aroelor. Th* abridged direction* b*lo* prorld* a working outline but et the expense of omiaalon of oeeentlal explaaetory detalle whleh are contained la the B. ead L. dlreetloae. 3orew thermometer Into lte socket In onter Jacket of upper prim. Open prime* and ehek their oondltloa. Clean if they are tolled, streaked, or spotted. Bitb loner fixed print horlsontal, place on It or 3 drops of the Aroolor tram a atlrrlng rod - sufficient to fill the soaoas be tween primm when *la*p*d together. Cloaa prisn* aad look with lock aut. Adjust tbs instrument aad alrror to raflest Alta light into the rafraotoaiter. Bo spots on nlr pockets should bo risible. Connect water Jaeket to aoureo of ooastamt tSRporatura -*ater, usually tbs tap, aad pass water until tba tbenaneter has been constant to 0J*C. for at least 9 niautac at 25*C. Tbs Aroolors flow nor* easily at S*C., heaoa tbs choice of this tenperatur*. - With primes illuminated, rotate tba prisms by nasns of the Index eras until tlm border of the light aad dark fields paeaaa exaetly thru tbs Intersection of the eroes hairs. If the bordw line Is fringed with color, rotate the compensator until the color disappears. If the boua- COMPANY CONFIDENTIAL TRAN OH*" STLCOPCB4025115 Refraotlve Index of Liquid Area lor* - 2 1I7 le not sharp, adjuet mirror until dietiaot half ahado-r is ob tained. IT the line or the oroaa hairs are blurred, adjust aye-iaca until a good roeus is obtained. Secure final fin# adjustment by naans of the aloe motion scree. Head the refract ire index, estlmtlnc to the fourth deoimal ^leoe. If the temperature at the water Jaoket la other then 23*C., oorrect to 13* by use at the.correction factor, 0.00044 per C. This fjetor is applieable only to Aroelora 1040, L234, 1260, and 1262. It nee found by aareful neaauremant on each Aroelar thru the ran,?e 10* to S0*c, The oorrection is subtracted when the workiar, teaperature is below kS*c. and added *h above 23*C. ' Example: If t>e refractive index is found to be 1.6422 at 13*C., the index corrected to 2S*C. is 1.6422 - (10 X .00014) - 1.6378. Care and Oelibratlon of Instrument Immediately after use, eleen tbs prists with swabs of pure cotton dipped in benzol, finally wiping dry with a soft sloth. Ths Time, sspeelslly the upper one, tarnish and aeretch easily. Oonsequsntly great eara mist be taken in eleanlrg. Before use the crlsne should always bs Lnspsotsd and reelsaned if necessary. Then not in use, refraetonetar should be kept In its closed oese. Tor pjwotiee or for cheeking arfamarca, distilled water la useful. ;atr ha a a refract Ira index of 1.3330 at 20*C., with temperature co efficient of 0.0001. A test else# of apeotal rlasa of known refractive index ia supplied with the lnstruasnt for calibration end adjustment If neoessery of the position of the Index arm. Refract Its Index of Aroclors - Typioal ' Careful measurements at 23*0. have given the following typical values for Aroelora. Aroelor Aroolar Aroelor Aroelor 1248 1234 1260 1262 1.6298 1.6376 1.6460 1.6462 Substantial departures (over 0.0010) froa these values riiould be li^ vsetigated iaewdlately as they - jr. correct - Indicate nibstential error in the composition of the Aroelor or eoataainatlon with other aaterlele. TAB tea 1-27-48 Copied by re 4/23/40 COMF>a yy CONFIDENTIAL TRAN 011900 STLCOPCB4025116 Hoasanto CtumiMl Coop* ay Annlstoa Matted No. 14-35-48 uaJ!^uf; Haelstlvlty of Liquid Aroalcrc 1CTOQD: I^eelataoce '-Ieasuranea.te between Conductje Apparatue I.'aeohn Bride*: Oeaerel Radio Company Type 3445, AC operated - 300 volte, aerial No. 171. TM# la a direct-current Vheetstone brides for meesurli^ high raalatanoas, bride* balance.belnc obtaiaad thru us* of a vacuum tuba TOltMtar. Rang*: 0.1 megohm to 10,000 aagohma, covered by a dial and S-poeltlon multlpilar switch. A resistance of 1,000,000 megohms eaa ba dataotad. T*at Slactrodea: Two ooneentrlo nlck*l oylladara (or bra**, alekal plat*d) with f**t. Obtained from General Slaetrlo Coepmay. The iaaar electrode ha outside diameter of .8" aad height of 3.5", with are* of 1B4 *q. cm. Th* outer electrode ha* iaeide diameter of 3" aad like height of 3.29", with area of 198 *q, cm. Tb* dlstaac* between electrode* 1* therefor* 0.1 inch or 0.254 co. By theory the electrode constant, are*/ length, 1* 191/0.254 or 752 where 191 1* the average area. Ia practice the cell conetant supplied by "reaeral t leetrio Company 1* used, for the electrode* aov la use, the cell constant was given a* 815. Olaaa Plate: Pyres, about 3-1/2* diameter with eoaeantrio groove* to assist in spacing tb* electrodes. Obtained from Oeaerel Electric Company. Ovaa: Caaeo-DeKhotensky drying oven with tw hole* in beck wall for por celain tubee for lead wire*. Hole* mu at avoid oven besting elements which occupy 2" paths vertically aad borlsontally Intersect log at the canter of the drooler well. - Lead Vires: Provide 500 ohn Amphenol twin conducts cable to oomeet tii electrode* is oven to the posts of tbe bridge. The nortlona exposed to oven taaperatur* era bared and then eovered with noroeleln baads. Provid* also a flsxibl* load to ground th* bridge to a wtir nip*. Clean the leads, baads, aad poroslain tubas oerlodlomlly. Assembly of Tea* Call Tha grooved glass plat* la plecsd la an 800 oe. baakar. Phe clean electrodea ar* plnead la tha grooves oi tha glass olat* with tha eoansetor posts directly opposite la order to give tbe widest possible sneelng to reduo* surface conductivity. The cylinders *ould be vary cion* to equidistant. The epparetue ahould b* dried for 2 hoar* at 100*0. bafor* tb* sample to ba tasted to about 110"C, on n hot plate end aour into th* electrode aeeembiy until the level of th* liquid le 1/4 to l/E- above th* eleotrodee. Cere mat ba used to make ra that th* COMPANY TRAN Oli^Ol STLCOPCB4025117 gjBJTCT: Resistivity of Liquid .\roclars - Peg* 2. METHOD: Resistance teaeurarante between Conductors lip of the container, froni which the liquid la poured, la clean. Tilt the beaker In aioh manner that all air bubblee In the Axoolor vill ri8e to the aurfaoe. Air oool to 103-104"C. tlien without removing thermometer, transfer to the oven which la maintained at 100*C. and oonneet the eleetrodes to the two flexible irlree whioh lead to the megohm bridge, '/hen the Aroclor oomee to temperature (100"C.), remove thermometer, check cen tering of electrodes, and precede to measurement a. Measurement with Megohm Bridge _' , Connect the two lead wires to the megohm bridge with the lead from the outer electrode-to the L(T7 unknown post of the bridge; tt inner elec trode to the unknots post. Connect the ThAIND post on the left side to s water pipe. Swine the spring oormeotor, pivoted on the "0" poat, to the L07 no at. Connect the attachment oord to the 110 7 po.jer supply. /lth the Aroolor st 10CC., turn the control knob (CnECIC-OFTl \TE-c:r.RGS) to the CHUCK position. Thro-i all 3 atrltobas at tha rear of tha Pwnsl to ON. After 2 minutes brine the enlvanometer pointer to aero by mean* of the ZERO ADJTJ3T knob. Than turn tha control knob to C7L'POE for one minute. Turn the. sob tc OPERATE end return the ralT&nooetdr pointer to zero by adjustment of the UJLXIFI.T 37 switch and tha rasgohn dial. Read after one minute. Repeot tha CHARGE and OPBvATE positions for verification. Tha raaiatlvlty of tha Aroclor is the product of the "multiply by" reading times the dial reading tlmaa tha elaotroda constant. Report in unite of 10? ohm cm. rounded off to two siilfleant figures. Example: "Multiply by" reading: . Megohm dial reeding Electrode Constant 100 5.4 nag. ohms 815 em Resistivity 100 X 5.4 X 815 - 4.4 X 10S meg. ohm cm - 440 X 109 ohm em VwXues for resistivity srs giallfltd by dsslmstlon of temperature and voltage. Tbeee nre 100"C. and 500 volta for the test above. Like con dltlons are need at Plant 8. . COMPANY CONFIDENTIAL TRAN 011902 STLCOPCB4025118 3J3JTCT: Realstivlty of Liquid Aroolora - Pare 3 1CTHCDs Resistance Measurementa bet-jeep Conduotore Cara of Apparatus The "Oparotlnp, Instructions", Oenersl Radio Form 45S-B, rkiieh teoompany the megohm bridge, recite detalle at Installation, measurements, uses, and construction, llluetreted by figures end clroult and -?lrln diagrams No attempt la made to reproduce such information here. The operator should acquaint himself with the contacts of the T.R. manual and refer to It for nBlntenance of tubes and perts. 'hen not Is use the nw'ph-i iTldr.e should be olosed and stored In oeblnet. Cleaning Elactrodej After the maasuramants are made the eleotrodes are removed from the . tested liquid, and allo-ed to drain until the liquid stops runninr from the electrodes, Till# still hot they are olaced In a beaker filled -slth benzene under a nail van listed hood and allo*cd to eool. .Tien cool, the eleetrodes art removed fron the benzene and scrubbed with pondered trl- sodlum phoaphate end o benzene carbontatraohlorIda mixture (30-50 by volume). This scrubbing can ba dona nith either a bruah or tha hands. The alactrodaa are than rlnaad with acetone, foil on ad by tap -ter and than distilled "*tar. The eleatro.lee ahould not ba touched by the hands after the soatone trash, ftcr final rinsing tha electrodes are placed In on oven ot 120"C. for one hour or until tbay are uaed again. Tba glaaa spacer plates are eleaned and handled in tha same manner a a the elaetrodaa exoept that they are virapped in leone paper before being placed In ths oven. Calibration For a roupfi cheek on tba condition of tba bridge, one or more eortridgetypa reslateness of known approximate value rtiould ba kept on hand ror periodic or aaorccaay verification of tha mater Itself. ra S/3/40 COMPANY CONFIDENTIAL STLCOPCB4025119 Monsanto Chemical Ccapaay Anniston Bethod No. 14-36-48 OBJECT! Dlslectrlc Constant of Liquid Aroelor MTISCD; Measured it 1QQ*C. and 1000 ayelag 2222* This aathod appllea to mineral oils and oil substitute used for lasulotlry. purposes. Apparatus Capaeltaaee Brldpe Cathode Ray Nall Detector OseIlls tor Cofistaat remperatura Oran Variable Air Coodeoaar 1300 ce. Pyraz Beaks r General Radio Co., Type 716-AX General Radio Co., Type 707-A General Radio Co., Type 606^A Cenoo-OeKhotlnaky #93000 General Radio Co., Type S3W Prooedure Electrode and beaker must be eleeaed as directed under "Cleaning Aope ra tus for Dleleotrlo Constant", and be at 100*C. Heat Aroelor in the can to 10S"C. Pour over electrode until olates and ceraaio insulation are covered. Connect leads. 3tlr with thermometer outside ovsn until temperature reaches 101"; pises In oven nhich has bsan oarsfully adjusted to 100*C. At the tlae saaple is placed in oven it a temperature hhould not have fallen beloa 90*C. Connect leads to capaeltaaee bridge, obearring that tha lead fra* insu lated old# of oondenser goes to insulated terminal on bridge. Selaaoe bridge carefully according to direction under "Balancing Capacitance Bridge". Until Aroelor end orea t ampere ti* as have beooae ldeatleal the bridge balance will eonstently shift. After oven temperature reechee 100*C., anintela bridge balance until no pronounced shift la erldeat. Record reading of oapaeitaace eoale multiplied by mltlplier setting. Oleleetrie Constant. Capacitance in Aroelor at 100*C. Capaeltaaee in air at 100*C. Balanelng Capaeltaaee Bridge -J v Condensed procedure. Operator should read eparetlag instruction for ^ Null Detector for eomplate details. 1,3 ot s 1. Connect to poasr supply leads to osslllstor and nail dstcetor. Qround tha oscillator. 2. Turn on oscillator by pushing 3000 oha, 10 mltlpller, 100 cynic frequency buttons. Adjust harmonic control until oscillation bcglna as aho by closing of sector in oathode ray tuba. TRAN OUW STLCOPCB4025120 Pago *2 Dielectric Constant of Llcuid drooler - Teat 14-38-40 3. On null detector turn brilliance knob to extreme left, the foou* knob to strata ri^ht, gain oontrol to artrar.a loft, erees amplitude at mid-eeale .otition, the aweep frequency awitch on iLna alda. 4. Turn on power awltoh, lighting allot light, 3. "alt fifteen seconds, turn brilliance knob to extreme right. 6. Adjust fooua and brilliance knobs until shorn fine line. 7. Conneot external terminals on deteotor to output terminals cm oaolllator. Switch sweep frequency to external aide. 8. Connect detector terminals of bridge to input tcrainala of detector, taking care that the black wire (around wire) of the lead goes to grounded terminal on both enda of lead. 9. Sat ewin control at mld-eoole and eeleotivity to extreme left. Turn aweep aaplltude to oxtreoe left, obtaining vertical line. "i'lth 10. v;ith turning oontrol knob obtain the maxlasa lenrth of thla lina, keeping it always under 1/4 inch with ain knob. a 11. Set sweep amplitude to extreme left. 12. Set r*in oontrol to rive vert leal straight line of about 3/6 inch. 13. Balance bridge .by adjuat In" power faetor and capacitance dials until only a dot remains on the screen rdiao the rain control la at extrema right. 14. Set sweep amplitude beyond mid-point, and slightly 'displace the pouer-faetor dial to obtain a tilted elipse. 15. Adjuat phase control until thia ellipse cloaee Into a straight line Inclined to the horizontal. IS. Bring power-faetor dial beck to balasee position, which should restive the horizontal ctraljtfit line. Displace this control the seme amount in the opposite direction. This should again tilt the straight line but in tta opposite direction. Adjuat phase oontrol until there la no tendency for this line to open up when it la swung 50 degrees from horizontal in both directions. 17. Throughout these adjustments the other bridge oontrol (the TRAN 011905 STLCOPCB4025121 PS** }Z Dielectric Constant of Liquid Aroclor - Test eabacltanca Dial) aust be In Palace* position. If the alllpaa rradually opens whan the line la horizontal It nmy be brought baek to the 11a# aln bj tiakltc alLght ohannaa In this aontrol. If confuelon results, bale no# both controls vs In as In (13) end reoaat tha sue. oaedloft adjustments. This is ths position of brldgs balanos: An alteration of the power-feetor aontrol will tilt ths lins whieh doss not opsn appreola bia thru aa av,l* of 30* to ths horlaontal both *wya; an alteration of ths oapsoltanos dial opens ths ellipse but doss not ohange ths loollnation of ths major axis. Tha apparatus say ba left in this balanosd condition, turned off by switching off first ths brlllloios kncb of tha dstsotcr, than the power swltoh, thao turning off tbs oscillator. for sue ossa ire asaaurwaonta ths oontrols ara not changed, ths apparatus lsft In adjuetnant. Thsn ths follminr steps define tha proosdure: 1. Connect *11 lands as previously directed iaoludtnr that from null detector to brides. 2. Tun on oscillator by oushins 100 oyel* frsausncy button. 3. Turn on null detector, wait 15 seoonds than turn on oatho-1* ray tubs. Turn sweep amplitude to eatress left end adjust brilliance to obtain a flaa vertical line on sorssn. 4. Briar this lias to a dot by ad Jus tl nr ths two brldrw control . Initial adjustasat Is facilitated by bavin? "Gsln" control to loft. When final adjustment is obtainsd this knob Bust bs at extra* rlsht. 5. This dot rsloins unchanged shows oondltioa of brld~s balance. Clssalas Apparatus for Plelsatrlc Constant Ths sondsnssr is removed from ths tested dielectric and allowed to drain aftil* still la ths oven at 100*0. Ths ooadecssr is thsn placed, nhlls still hot, la a beaker at benzene under a well vent Hated hood aad allowed to seel. Zt Is then thoroughly washed with powdsrsd trleodlua phosphate oad s 50-50 slxturs of benxane sad carbon tetrachloride followed by aa aeetone rinse. The operator should bu ary careful not to touoh the natal pin tea of tbs condenser .after this point. Tbs oondenoer Is thsn rinsed thoroughly with tap water followed by distilled water end dried oa a elaaa paper la aa otsb at 1S0*C for at least on* hour or until it la asala used. tab 3/1/4 COMPANY confidential TRAN 011906 STLCOPCB4025122 Jtonsaato Chemical Company Anniston Uethod No. 14-42-48 TJairiTr; Acid Humber of Ll.-uld Aroolore iT.'il'.0D: Titration vrlth AlZili using fteaol Red The Add Number la the weight In milligrams of sodium hydroxide re quired to neutralize one grera of Aroolor to pH 7.6. it thus lnoludee any hydroohlorle eeld, ferric chloride, and other Inorganic or organic oonstltuente having eeld charaoterletlce. It oorree^ole to the Neu tralization Number of ATT.: Designation DIOS exoeot that the latter Is expressed la tens of KOH Instead of HeOH and has a somewhat higher (phenolphthaleln) end point. Procedure To 100 ml. of adjusted (pH 7.6) solvent containing Indlcetor elonly add 0.1 N NaOH dropwlae until tha oolcr corresponds sonroxlastely to pfl 7.6 when compared against a suitable reference solution. Readjust If necessary to maintain pH 7.6. Add 50 grams (tig.) of Liquid Aroolar and mix wall. Titrate from alero buret with 0.01 IT NaOfi until the original rad color of tha solvent Is restored. A portion of solvent In o similar container Is a useful rafsrsnea is detenlninr tha and point. Tha natch la governed by estimation of tha intensity of red beeeuee the hue le not exactly reproduced on aooount of tha yellow color Introduced by tha Aroclor. 1 ml. of 0.01 If RaCD 0.4 lies. NaCH. Calculate in terms of UfTI. NaCE per sB. of sample.-Report to 4 decimal nieces. ml._of_ 0.01 N ITaCB X 0.4 m \l&i. MOE/&. . C* of nple Example: If titration is 0.06 ml. for 50 g. of Aroclor, the Acid Number la 0.06 X 0.4/50 0.00064 U#i. HaOH/fft. Raoort as 0.0006. Solutlena Regulrad Solvent: Illz 600 ml. of benzol, 200 ml. of 5-A alcohol and 200 ml. of aeetona* Add 5 ml* of O.&i phenol rad solution. Phenol Red Solution, 0To 0.1 mi* of dry indicator in s small baa tear add ezeetly 2.0 ml. of 0.1409 IT NaCH. stir to dissolve end dilute with 5-A alcohol to 50 ml. Reference Buffer pQ 7.6: Dieaolva 0.41 g. ItallaPQe and 0.59 (ca. Ifa#rff04 (both anhydrous) in 100 ml. of water. Add 0.5 ml. of 0.2/ phenol red. Solution is used for reference in adjusting tha solvent if Lal'ott* pH 7.6 oolor standard la not available* COMPAMy confidential T RAN 01H07 STLCOPCB4025123 Ael& Ituabtr of Liquid Aroalora - 2 standard 0.01 If ItaCB: 5 ml. of .5 R HaOH to 250 ad. rol. of 5-A al- eobol. Protaot at all time* froa atmoanharlo C0a, . Wot a ' 9y usla 330 ml. soetoos la aolTaat Instead of 200 ml. a 100 pa. sampla of 1234 may be taken for analysis. TAB: m 1-30-48 Copied by rs 4/23/48. V r TRAN 01l3 STLCOPCB4025124 Uooeento Chenical Ccapany Ana 1too Method no. 14-43-43 A?ttTXTt Color of Ajoclor oa R.P.A, Tcale trjTTKX; Halllgs Pocket Comnratar ___ 3oo p# The method Is applicable to Aroclors 4465, 5460, or others hawing n.P.a. oolors In the ranee 1 to 9. Procedure '.'arm the Aroelor Is necessary to obtain pourlap 00 ns latency, nil the test oup of the Helllgs Pookat CompBrutor, llodel G05, with Aroelor, Insert oup in the comparator, and compare against the oolor disc (No. 620e^0, Lu hr looting 011a and Petrolatum) which has R.PJl. colors from 1 to 9 la one-haIf steps. Report color to nearest 1/4. Clean the teat cup with a mixture of CCI4 &nd benzol, with final rinse of benzol. A.7B! oolor numbers eolaelde with Notional Petroleum Association oolor number (1915). The relation of the R.P.A. color numbers to other color soelee la tabulated below: NPA Color Noe. (1915) NPA Namea Union Petrlavas Co. attu Color Roe. Low!bond Analyala Red Tallow Blue 200 510 1180 1/4 1/2 3/4 1 1-1/8 2 8-1/E 5 5 -VI 4 4-1/E 5 6r 8 - - *. Lily white Cream white Extra pale extra lemon pile Lemon pel* Extra orange Qrsaee pale Pale Light Rad Dark Had Claret Red ` - - 0 H Z 7 K L U N 0 P W 8 m -m -1 0.12 1.5 0.60 8 2.5 8.5 4.6 3 6.9 3.5 9.4 4 14.0 4.5 21.0 5 36.0 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 - - ,55 .55 - .55 1.80 TABism 1-26-46 Copied by re 4/27/46 COMPANY CONFIDENTIAL STLCOPCB4025125 -bn a* ato CSami cal Company ' Anniston Method No. ] 4--11 IS XBJSCT: Color of -'Tatar Vhlta" Aroclors :2T`DD!__ Corrparlaon acmlnst A.P.H.A. -Soala 3oopa The method la applioobls to Aroclors L>54, L26C, or ottars having oolor lean then H.P.A. fl ("..atsr .11160"). A.P.H.A. "tandarde Theae oolor atendarda are aold eolutlona of potaaslum ehloropletlnate and oobaltoua Ohioride. The unit of oolor la that produced by 1 ng, of platinum per liter. The ratio of oobeit to platiaua nay be varied if neoeeaery to ntoh the In*. Beoouae the hue of Aroelor 1254 and 1260 seems beat matched without oobalt, thla tea been onltted in the prepara tion described. Dissolve 1.245 g. of potassium ohloroplatinate (K*PtClt) eontalnl^ 0.5 g. of platinum in water with 100 ml. of ooneentrated hydroohlorlo sold, and dilute to 1 liter with distilled water. Thla solution has a color of 500, Prepare standards from 10 to 100 in steps of 10 by dilutinr 1, 2, 3 ml. ate. of the above solution with distilled vater to 50 ml. in standard high form Hasalar tubes. Protect the tubes from evaporation. Refer to pepe 13 of "Standard Methods for the txanlnatlon of .star end Sawape" sighth edition (1936) for details of standards containing eobalt. Published by Amariean Public Health Association, 1790 Broadway, Hew lark. Procedure Till a match Inc He alar tube with Aroolacr to e height equal to that in the standard tubas. Cooper* with standards by loolclnr vertically downward through the tubes upon a white or mirrored surfeoe pieced at aueh an anrla that light is refleeted upward through the column of liquid. A oolor tube support (Tlatmr #7^)65, X ml.) is convenient. Xnawsh as the proportions of the standard eolor aolutlon in the compari son tubas srw sueb as to represent an aliquot part of a liter, the readings are direst as psrts par million. Colors up to 100 are recorded to the nearest 5. Direst comparisons era satiafaotcry up to 100. Above this the eaaple should be diluted with Carbon tetraohlorlda (maxima A.PJ.A. color, 5), and the oolor obtained to nearest 10 by mltlplylng by the dilution ratio. PABism 1-90-40 Copied by re 4/27/48 comply CNFIDE!\it/al tran 011910 STLCOPCB4025126 ilonaaato Cbsmlosl company ' Anniston Method No. 14-46-45 TJBTSCT: ... Acid Number of -solid Arocltxs m Hoary Llculd Axoclar. ICTROD: TKrttion with Alkali using Phcnolphthaleln Prooedure Dlasolvs 50 gratae of the Mj-oolar In 50 ml. benzene In 400 ml. betker warming to beaten eolation. Add 50 ml. 3.1 alcohol, 200 ml. dlatllled * water, beat to boiling, add 1/2 ml. \% pbemolphtbalein eolutloa, and titrate, la the oeee of the dlatllled Aroolcws with 0.01 N sodium hydrozlde eolutloc, to a faint pink aolor whloh la permanenT for at leaet two minute a after vigorous stirring. A reagent blank should be tun con currently. The acidity of the sample Is oeleulnted aa milligrams of sodium hydro*Ids required per gram neanle. Calculations Using 0.01 N NaCR, AoId No. ml. titration X O.i/aamnls weight for 50 m ~ Aoid No. {ml. tit. ml. blank) X 0.006 Using 0.1 N NhGB, Acid No. - ml. titration X 4.0/samnle weight for 50 0ft/~ Acid No. (ml. tit. - ml. blank) X 0.06 Apparatus 10 ml. burette In .05 divisions. Conversions 1. To obtain Neutralization Number In tame of JODI!, multiply the Aold Nujfeer In terms of ItsOH by 1.40B. Inverse faotor le 0.713. 2. 11aIt Inly the Aold Number by 1000 to obtain the perta of NaOH re quired to neatrellse one million jmrts of Arooler. Thus Aold N\u*er of 0.0006 Is equivalent to 0.6 parts of IVsOB par ml 11 toa nerta of Aroalor. S. Ths lares amount of eetsr used eauaea harper maceration of the aqasons layer from the non-equeooe layer, thereby making ths endpoint more really distinguishable. Zf the titration la carried out against very light beekjTOuad or in e fluorescent light, the end point is easily seen. 4. Aside ffan fires aold es a osuse for NnCH consumption, fsrrie o hi or Ida Aleh is usually present in nail amounts, also son sums RaOU in neu tralisation to phanolphthalsln. It tbsrsfors follows that an Areolar of very low aold number rust ba also srtransly low In fsrrlo ohlorld*. TABtarn 1-26--45 Coplsd by rs - 4/27/46 company ONFiDENTfAL tran 011911 STLCOPCB4025127 Monsanto Chemical Company Anniston listhod No. XBJTCTi Poor Point of Liquid Aroclore I--11 lul>: A.3.T.1*. D-97-39 The pour point of an Aroolor la th# lowest temperoturs at which tha material will flow when it la ohilled under certain prescribed condi tions listed In AJTU D 97-99, Apparatua Apparatus consists of test jar, thermometer, cork. Jacket, disk, gasket, and bath as described under A.3.T.11. method D97-39. The thermometer is the A.5.T.U. Cloud and Pour Test, range -36 to 50*C. Present apparatus is the Bmil Greiner Co. j/OR 2234 ainrle unit with Qr2242 test Jar. Procedure for Aroclcr follow D97-39 in all respeots except that the centigrade seals la sub stituted. Only an outline follows: Add 40 ml. of Aroelcr to teet Jar. Adjust themoreeter to oentcr of Jar with beginning of capillary 1/8 inch below surface of the Aroclcr, '.'am the Aroolor without stirrlnr to 46*C. ill a hath at 46-46*C. Cool to 32*C. in air or water bath at 2S*C. Trans fer the Jar to the Jacket of the cooling bath which is maintained at 0 to 3*C. Becinninc ut temperature 8 to 10 degrees abore tha pour point, at each interval of 2*C.t remove the test Jar from the Jacket and tilt juat enough to detexnine if there is movement of the Aroolor. This inspection should not require more than 3 seoonds. /hen movement is not promptly apparent, the teat Jar should be held In a horizontal position for exactly 3 seconds as noted by a stop watoh. If movement oecura, lmedlately return the test Jar to the Jacket, Repeat test for flow at tbe next temperature 2*C. loner. Continue the test in steps of even debase centipede (14,12,10, ate.) until tbe Aroclar shows no eoveaent when the test Jor is held horizontally for exactly 3 seoonde* This is tbe solid point. The poor paint la tbe previous temperature, 2*C. above the solid point. The pour point ia this tbe lowest temperature at wEteK' the liquid will flow or pour under the teet oo adit lone. Technic lane mast familiarize themselves with 097-39 which nivee oomplete details of apparatus end procedure, reproduolbllity of results, effects of thonaal history, ate. The directions above are inadequate except as e wo tiring outline. Tbe both twapereture is controlled by adding dry ice to acetone for pour points belwi 0C. TAB:cm - 1-30-45 Copied by re - 4/27/40 COMPANY CONFIDENTIAL STLCOPCB4025128 ltonsaato Chaaionl Company Anniaton Mathod Vo, 14-46-43 'JT&J1XT: Tha Tcating of Aroolora for Inarrjanle CMorldsa i&TITOD: ~olutlona Required %andard Clilorlda Solution: Dlaaolra 0.660 extuna of cure sodium ohlorlde la sufflelent water to measure exactly 500 *1.; 1 ml.'then contains 800 ralcrocrcne Cl. Pipette 25 ml. of this solution to a 500 ml. flask and make to the mark to fire a 0.00113 U NaCl solution, 1 ml. of whloh con tains 40 mlcrofysms of Cl. Preserve In a Pyrax bottle. Caution: The outer usad la praparutlon -ruat be ohlorlde fras by tbs Tyndall Beam teot; tbs 0.00113 13 solution should not bs kspt over 1 month. * Slltsr ITltraU Solution 10: Diaaolre 5 rrams of ellrer nitrate eryatala In 40 ml. of mater and add 10 ml. of oonosntrated nitric sold. Ohlorlde fra a distilled `-star. Apparatus Raqulrad LnHotte 10 ml. oolor tubas (13 at. 1 100 mm). Test tuba rook with a black surface at tha bass for uniform comparison (Rota: me are using blsok gasket rubber over the entire board that sup port* tha bass of tsst tubas during oomperlson.) Bos. About 7* long and 4" elds. This box oontalnn holes In top and notches In the bottom to hold Lamotte oolor tnbas. It la Just hi< enough to allow 1/4" of tsst tubs to extend through the holes In the top. The box should be painted a flat blaok on the lnaide and on top and should oontain enough holes to aoeoaodote at least ssrsm tubas. Method Clean nil flanks, tubes, sad pipettes to bs used. Than rlnaa with dilute nltrla asid than ritfc ohlorlde free dljtlllsd astar. Add 90 ml. ohlorlde free water to s 290 nl. Srlenaeyer flask, heat to boiling, add 200 gram of the Aroolor to be teated, *dieh has been heated to 100*C, shake rigorously for 1 minute, cool in ooollag pan. Carefully daoaat om of the water extra at to a separatory fummsl. 7aah with pure ethyl ether (ohlorlde free). Tranafar 10 ml. of tha ether washed extraot to a 10 ml. Lalbtta oolor tube after rlnsinc tube with portion of extraot. Prepare standard* by diluting exactly 5 ml. of the 0.00133 M WaCl solution to 100 ml. in a COMPANY CONFIDENTIAL TRAN 011,1 STLCOPCB4025129 Ths Tasting oX Aroolors for Inorganic Chlorides - 2 - roluaatrle flat*. Ob# 1. thsn oontsla* 2 mionvrrsms of Cl. Transfer 1, 2, and 3 al. portion* to 10 ml. tubs*. Uke to tha 10 ml. nark with Cl frea 3,0. Place standards and sample in light fra# box from whloh only tha top of tubas art txpoasd add 0.3 al. of the allTar nitrate to eaoh tuba oompara In a specially prepared taat tuba raok. The ooaparlson Is to be made quickly and from a constant aourca of light, preferably day llit froa a window away from the sunll/fct. Comparison ' la easier whan other aouroee of lidbt are shielded from the eomcarlson raek. Look directly into the top of tha tube end aompara. Rota the known aolutlon idiich roat nearly n_tohes tha star extract estimating to tha nearest whole alotofyaa. Tha ertruot blank and tha distilled -rater should show no turbidity. Calculation DlTifle the ohlorld* oontant in alaror-rena of ths lmom solution whloh mutohas tha extraot by ths wsicht of th* Aroelor rapresented by ths sxtrmot to obuia th* ehlorid* oontant of ths Aroclor in p.pj*. In tha procedure described, tha 10 al. extract represents 40 ~rana of Aroclor (1/3 of 200 g. tclean). Ths three known* oontala 2, 4, and 6 alerosrta* of Cl, thns representing 0.C6, 0.10, and 0.13 p.p.a. rsspaetiraly. Values should be reported to tha nearest 0.029 ppa. Precaut Ions Baeauas of tha senaltlwlty of thla taat, aarleua error* nay raault through Tory all^t contamination, or Inattention to datalls. All equip ment isaat b* aorupuloualy eleansad, th* diatlHad water absolutely ehlorid* fra* and taatlng dona away froa fuiaaa of BC1 or chlorine funs*. r 4/2 7/ COMPANY CONFIDENTIAL TRAN 011914 STLCOPCB4025130 1 Uoosaato Chemleal Cowpaay Anniston Method Ho. U-53-48 sJSJXvT: '-ator Content of Liquid Aroolors fXCTPCO: Tltratlai with Karl Tlsoher Reavegt Outline Ths Aroclor Is dissolved la t alxture of bon tons sod aothanol whloh boa boon titrated with Fischer reagent to tho ahorootrlstlo and point. Fischer reagent is * solution of Iodine, sulfur dioxide, tad pyridine. Zodins Is oonsuaed os long as any watsr Is mint. The solution is o~in titrated to obtain tbs water oontsnt introdueod by tbs Aroclor. Solutions and Apporatas Earl fisc bar Reagent: Velgb into a flask 264 grass of pyridine, Barr att E-A or Eastman 214*41, and add 61 press of liquid or gaseous sulfur dloxlda. Add tbs liquid sulfur dioxide directly from tbs Inserted cylinder by attaching to tbs outlet tolta a glass tube sxtsndlng Into tbs pyridine. Sulfur dioxide gas oan be bubbled Into tbs pyridine until proper saount is added. Store in a glass stoppered bottle. Transfer 65.6 groan at the pyridins-SO* mixture and 134 al of abeolute netband to a 1 liter Florence flaak. Oool thoroughly la an ioe we ter bath. Add 16.9 glass of iodine, stopper, sool again before shaking. Alternately oool and swirl until tbs iodine la In solution. Kabos 800 al of reagent. Store la gl*** stoppered bottle. Let stand 84 hours before using. Then fresh, one si of reagent is equivalent to about 0.0033 91s. of eater. Aroclor Solvent: Mix l parts dry benzol with 1 part anhydrous asthsnel. The dry benxol la prepared by shaking the eoanerelal grade with anhydrous oalolua ohlorlde, decanting Into a flaak and distilling, rejecting tbs first 10S to ooaa over. Soap in glass stoppered bottles with alniaua sxposurs to air. Micro Buret: 10 al. x 0.06 al. Eoch autonatlo with glass stoppered reservoir. Xsk and KTabs 8460. Equip reservoir with a moisture guard tube containing Drlerlte or a similar dahydrating agent. Procedure * East a slean 600 al. narrow south Erlenmeyer flaak in aa oven or on hot Plato until thoroughly dry. 9weep out for 10 aiautss or until oool with air which has been thoroughly dried by passing thru tubes sontainlng 8 ae* Drlerlte. 01 seagage the flask fxoa the aaplretia* traia sad lam- dlatoly oloso with a papar cap held by a rubber bead. I COMPANY CONFIDENTIAL TRAM 011^15 STLCOPCB4025131 I './star Content of Liquid Arooion - z . without daisy, transfer 100 al. of tbs banzens-mthaaol solvent to tl fin tit thru t Mil hols punetured Into tha papar oap. Cower araln with papar. Tit rata at oaea with Karl Tlaohar reagent to dlatloct rad-brown and point rtileh doaa not fade aftar awLrllnc aereral times. Tba Tlaohar reagent la dispensed fro* tha mlereburwt the tip of whleh projaote Into tha flaek thru the pincture In tha paper oap. At tha and nolnt any water oontant of tha aolwant haa baan raaotad. Cuperimpoee a freah papar oan Immediately. Obtain weight of tha aolrant and well-oowered flaalc on a T>rwlon belanoe or equiralent. ^ilokly lntroduoa with a dry pipette about 100 oraws of tha slightly warned Axoolor to bw teated. Cowar at onoa and weigh a^ln to obtain tba weight of Aroolcr to naarart gran. Shake until tta Aroolor la dlaaolwed. IT tha mixture la aloudy, *ra sllgitly. If eloudlneaa paralata another mixture ahould ba prepared. Puncture a small holt In tha papar oap for tha lnacrtlon of tha burnt tip and tltrato with Tlaohar reagent to tha first dnfinlta brown eolor, agitating with a oantla swirling not loo. Tha and point ahould werelot through sawaral swirls. Tba and point nay slowly feds throutfi slow aoeeas of ataospharls mol stum la whioh easa It la rwsb<red by a drop or two of raegant. If not so restored, tha and point say hare baan a falaa ona or tha oloeura la faulty. A definlta and point la Impossible If huald air la not wall axaludad. Troa tha aaount of reagent required and tha aalgbt of Aroolor uaad, aaloulata tha watar oontant In p.p.a. Calibration of Tlaohar Reagent and standard Tatar Solution Standard watar solution in aathaaol: Transfer axaetly 0.40 ml. of watar froa a mloro burat or a 1 *1. net aurlng pi pat to a 100 ml. wolunatrlo flash. 7111 to tba nark st onoa with anhydrous methanol and six. Ona 1. of solution than oontalna 4000 nloroTono of Tatar in addition to any water whleh mj ba praaact In tba methanol. Tmnofar exactly S al. of tho abort ataadard atar solution (equlTilant to 0.01 {7*ao of watar) to a 290 ml. Tlrlanneyar flask whleh has baan drlad sad owapt with dry sir. Closa with papar cap sad titrate with Tlaohar rearest la tba sans wanner a a tba saapla * Tha and wolnt la aharp. A aathaaol blank, found by titrating 9 al. of tha aathaaol uood in mkl^ up tha ataadard water solution to a Ilka and point, oust a 1-ay a ba aubtrseted froa thlo titration. OlTlda tha mount of watar taken by tha net TieAar rea<*eat required to obtain tha tltar of tba Tlaehox reagent la tame <X watar. Example: A 9 ml. aliquot of standard solution, tpulmlent to 30,000 nierorrnme of watar, required 6.61 al. of Tioobar rwa-ant while 9 al. COMPANY ' CONFIDENTIAL TRAN Oil STLCOPCB4025132 '7atar Content of Liquid Aroalora 3 of the aathanol retired 0.33 of Tieetar rea<t. 20,000/(6.61 - 0.33) *0,000/6.06 3300 alcronrana water/nl. Reeallbratlona: Baoaoee the Tiaehar rea-ent deteriorates rapidly, ita titer wat be determined for each day, uaa. If the ease etandard water eolation la uaed la reoallbration aa la tha Initial aalibratioa, tha titer of tha Tiaahar reagent aigt ha aalculatad from ita total *(? oontant (ineluding that introduced hy tha nathaaol). Tha total water la tha produot of tha initial rroaa titration and Ita titar. Thla la tha example ataoTa tha total watar eoataat of a S id. aliquot la 6.61 X 3300 21813 nierojgraaa. If on raoalihratloa 7.37 al. of Tleober raacant la 21813/7.37 2960 aicrograma of water par al. Two or more oallhratlona ahould ha made with asra^nent within 0.023 al. Calaulatlon of ^0 aaapla Standardisation of Standard 3,0 aol. Titrata 3 al. alztura 3,0 aol. Titrata 3 al. of aathaaol Tit of 3 al. aixtwa A Tit of 5 al. aathaaol B A - B al. reageSt for 3,0 addad 5/100 of .4 DIt Ida 5A00 X .4 by A - B faoter graaa of HaO/al. IdaIt1 ply feotor X B giTlfif 0ts. of 3,0 In 5 ail. of aathanol. Add thla wt. of 3,0 to .08 alraady addad giTing 3,0 In 5 al. (Total) Z!2i22------------------ . t, 3,0 St* 4 Titration A Tj_ X aaapla Titration T, T, X 1,000,000 PI* 3,0 wt. aaapla 7AB:oa 1-27-48 Copied hy rs 4/27/48 COMPANY CONFIDENTIAL TRAN STLCOPCB4025133 UuTiAlAL MOBBO 4 ' Trom . PB0P*.HTIE3i OF BASIC HAL0r.Ar rBOgPCTS Uttar to H.C.V./M.T.Bolnsr ftalownx Prodaota DIt. .Ifoloo Cart Ida and Carbon Corp., 30 K. Forty-Saoood St.. N.T. 17. M.T.). Uttar datad Fab. 27. 1940. * Mo. 1000 No. 1001 Mo. 1013 So. 1014 Colors T-ym Point Clod. ASTU Softsnisr, Point) dsr- P. Chita to Pala Straw Tblto to Pale Tallow Pals Tallow Liquid 194-201 ` 247-252 Pble Tallo ......... ..... 1 T 2T7-2S3 S.aoiflc Gravity at 77 da#r. P. 1.19 - 1.25 P-notration (fOd. A3TT!) 200-<j. load at 77 dag. F. -- .1.53-1.59 10-15 1.65-1.71 5-0 1.75-1.^ 6-8 P* jeoaity (Saybolt Onlvarsal Saoonda) Distillation Reaps (aSTT() dar.. P. 33--37 at 77 da*. F. 480-590 33-37 at 266 dar. F. 600-660 31-35 at 266 dag.F. SI 5-^656 35^7 302 VO-Wfl -1 *aah Point (ASTi! C lava land Opan Cup) dar. P. 209 .284 356 39* Plra Point (1ST! Cl avaland Onan Cup) dar. P. F.-ter Factor at 1,000 ayalaa at 10r ayalaa l vlactrio Constant at 1,000 oyolaa at Mr oyolaa 0 C, Raaiativlty (naff, ea.) at 30 dar. C. 338 -- wa IL m --. Nona to boilinr Lass than 0.2/ 0 43 5-6 5-6 Ovar 107 - 10* Mona to bo11 lor Laa a than 0.2/ 0.70/ 4-5 4-5 Ovar 107 - 108 Mona to boll inr tsi O.TCK 4-6 4-6 7 Ovar lO -lO STLCOPCB4025134 Coplod by nab 4/2/48 Co^dutW F KAN 011918 i 4 *L I I-A-B-4C00 From - Hilonx Product! Dirlalan Uaioo Carbide and Carbon Caroaration SO Saat 42nd Street flaw Fork 1?, Raw Tork Lattar - V/.C Jl./J.tt. Cola, Tech. np. 8/18/48 Zyrox 3009 (11-313) qgNERAl XOTORU'.TIOB Color 3p. Orarlty Softening Pt. 3toraer Vlaeoalty 3aybolt Furol Tlaooalty Panatratlon at 30*C. Panatratloe at 25*C. Flaah Pt. Tlra Pt. Coabuwtlbillty Fracture Acid Resistance Alkali Resistance Volatility P.T. at 25 *C. (1000 cyclaa) Dial. Constant at 25*C. (1000 ayelaa) DC Reslstlxlty at 2S*C. - Brow - 1.40-1.45 at 25*C. - 79-83*C. - 59-89 at 130*C. - 79-180 at 130*C. - Approx. IS (200 go. load) - Lace than 3 (200 on. load) - Approx. 590*7. - Kona to 600*7. - Till not support oonbuatlon - Conoholdal - Excellent - Tieell ant - Average for 24 houra at 130*C. Last than 0.10 ag./aq.ca./hr. - Approx. .001 - Approx, f.96 - Over 10 nag. erne. Copied by ra 4/8/48 COMPANY confidential THAN 011919 STLCOPCB4025135 Fron - Halwwx PTduota Dlwiaion Onion Carbide and Carbon Corporation 30 Zat i2nd nreet New Tork 17, New Tork Letter - ;.C.Il./T.M. Cole, Tech. Rep. 2A8/4S Zyrox 3007 (11-300) CgTgRAL PffTCRMiTIOK Color 3p, Orerlty Softening Pt. 3tor*er Tlacoelty saybolt Furol TlecoaltF Penetration at 30 dec. c* Penetration et 23 dec- C. Pin eh P*. Tire Pt. CombustIblllty Fracture Aold Reelatanoe Alkali Resietanoe . Volatility P.F. et 23 deg. 0. {1000 eytlea) Dial. Caaetant at 25 deg. C. (1000 eyalee) DC Realetlwlty at 25 deg. C. - Brom -1.29 - 1.32 at 25 dee. C. -63-70 deg. C. - 20-27 at 130 def. C. - 20-30 at ISO deg. C. - Approx. 75 (50 g. load) - Leaa than 3 (200 n, load) - Approx. 330 dag. 7. - Nona to 600 dag. T. - 'ill net eupport ooobuatlon - Conoholdal - Exoallant - Excellent - Awarece for 24 hre. at ISO deg. C. 0.20 rag./aQ.on./hr. - Approx. .004 - Aprrox. 3.0 - Over 10 Beg. aae. Copied by re 4/2/48 COMPANY CONFIDENTIAL TRAN 011920 STLCOPCB4025136 STLCOPCB4025137 MO. STLCOPCB4025138 STLCOPCB4025139 COMPANY CONFIDENTIAL APPENDIX Fr on: II. PHT3ICAL AND CHEI3CAL PROPCHTr:'! OF CLOTTON QIL9 (ae quoted Id I. C. Furben's aales sheets) B. 1.0 ,rI. Final Rept. No . WO Item Nos. 1, 7, 22, A 31 Pap;ea 100 - 109 Jo! B.<C <O O STLCOPCB4025140 Clophon A30 Clophen A40 Clophen A30 Clophen A70 Clophen A80 Fora ..................................................... Colour .. .......................................... .. Ipsclflo Gruvlty at 20*C .. .. SolidifyLog Point............................ Float Point* ., ............................ Sbrlnko/ro: 100* - 20c .. .. 30* - 20C .. .. Viscosity ut 100*C ................... Liquid Liquid Nearly colourlass Nearly colourless 1.35 1.48 --10*0 -3*C 166* 193* (Pensky - Cartons) 3,: 1.1`E 6* 3^ 1.2*E Llqu Id Liquid Nearly Necrly colourless colourless 1.55 1.60 12f 30-C 222* 236* In an open crucible 6,1 3* 1.5*E 6,". 3/ 1.9-E Firm Nearly colourless Fir*. crystalline "bite 1.7 1.72 - 1.77 30 *C >160*C 240* 290* or -orar . (Pensky - ftirtana) 5 - 6r. - 3* - 4*R -- 9ciline Point Llolt at 12tm. of I'aroury................... .. 165 - 195* 100 - 215* 190 - 230* 193 - 25C* 200 - 235* 210 - 260* Less during r.Tapomtlon (after 6 hours at 100"C) .. o.oo>; Volatility at 20*C ............................ <0.009* (Inn. of Uaroury for 100 hours) 0.03," <0.009,1 0.02* <0.009* < 0.01`,1 <0.009* 0.01" <0.00951 0.0 (2 hrs. at 12b* ) <0.009* lie it Conductivity at 40*C lin Calorloa par aatre par hour par *C). Saponification No. ............................ 0.093 0.0 0.091 0.0 0.007 0.0 0.066 0.0 0.0 V. ana11 V. mail V. nail V. am 11 V. mall JO > Permittivity at 20*C ................... 6.0 3.4 3.0 4-4.3 3.0 Pc.vor Footar ................. .. .. <0.001 <0.001 <0.001 < 0.001 <0.001 o (h ? ikdcwn Otrcn.sth................. . .. 200kf/om. 200kV/cn. > COOkY/ora. > 200kV/cm. - Ii ,.i Lot Ion llcslitanoo In Ohm.on. 1 X 1013 1 X 1013 1 X 10 14 ^11 1014 >1 X 1014 r\j 0.0 Y. small 3.0 - > 1 X 1014 4 4 1 V i> Clophers sro not rom^u<t lble nnd do not auDnort combustion of mnterlnls Into v/hlrh ttay are Impregnated. TABLE I Fron - United Itates Patent 2,070,268 Patented February 9, 1937 P3'-0 2 o o o m5 1-------2-------- 3-------4-------- 5 --6-------- Hydrocarbon compositions . Diphenyl Dlstilled blrh boiling COM-- pounds Percent 0 0 00 60 50 50 Percent 100 10C 20 20 50 50 Properties of dielectric Ohiorlne content Percent 23.9 40.3 41.2 52.2 42.0 36.4 Viscosity 9ec. >oy- bolt at 210* F. Aieclf le oreTlty at 65*/65 C. *3 290 35.7 47.5 48.0 40.8 1.251 1.405 1.352 1.490 1.383 . 1.324 Dielectric constant K at 100* C. (1,000 eyeles) 4.35 4.98 4.07 4.56 4.84 4.89 Properties of cblorlnoted diphenyl 7-------8-------- 100 100 70 > Z Copied by re o 2/2/40 f<\J0 \j> 0 54,0 0 42 .0 46.0 j1.523 34.0 1.380 j ______ L 4.30 4 .80 I l <JT Ul I (u O(>-* 3CC, STLCOPCB4025141 I-m (J! - 50C Stability of Grado P Hycar and Teflon in Aroclor 1254 at 130C and 45*C Short Form ileport No. 21?9 Tile No. 141-27.1 . December 29, 1947 Notebook references: Smith 45137 Grade P Hyoar end Teflon Immersed in Aroclor 1234 Material Temp Hours Oa in In '.'t. % Gain in Thietene Grode F Hycnr Crude P Rycar Teflon Teflon 130*C 45C 130'C 45 C 283 2es 285 283. 68.6 26.3 Negligible Negligible 26 6 Negligible Negligible rs 1/14/40 company CONFIDENTIAL TRAN 011926 I STLCOPCB4025142 I-A-l - 500 From - :'a.io P.G.B./R.L.T. 3/22/43 AeroTox Corporation Non Bedford, V.aasachusetts Determining Fluoroecence In /vToclor "The ultraviolet lipht ne uoe for determinin'* fluorescence in Aroclor is monufoetured by Geor-o Ootcs and Company, Franklin Square, Lonr Inland, Hew York. It la a CH 4, 100 latt, G. Itazda Lamp with filter. "Our procedure la to pour a small amount of Aroclor into a 5" wateh (jlaae or a 5" Pyrex evaporating dish end observe for the decree of fluoreseer.oe under tbs CH 4 lamp, preferably in a dark room. If the sample haa been contaminated with Mineral Oil it will show up as a streaky or milky fluoreaoenco ae oompured to pure Aroolor. The fluorcooence around the menlacua of cure Aroclor le not to bo oonfusod with the fluoreaoenee resulting fro* contamination. "This tost la qualitative and, os auch, le based on the experi ence of tha peraon perfcmluR it. 'It keep a standard s-npla for comperleon. If there arc any further oueatlons please feel free to contact us". Cooled by re 4/2/48 COMPANY STLCOPCB4025143 : - ico December 2t 1947 ELTCTRICAL g,T,\ OK ,,ROCLOR3 Introduction Tima ha# not permitted ua to corry out electrical measurement# on ell of the Aroclor samples eect by your laboratory and as listed In your letter to Dr. C. K. Bump of June 27, 1947, It wee ballered that dielectric constant, Ions fuctor, and direct current resistivity measurements orer a temperature range for a low chlorinated and highly chlorinated biphenyl; alao one sample each of the terphenyl and the mixed biphenyl and terphenyl series would represent the electrical beharlor of Aroolora. The ti-end of the eleotrlcal properties of the Bennies not measured oan be estimated; l.e. as the Tlacosity of the \roclors of a particu lar eerie* increases, the los9 factor will decrease and the loss faotor maximum (If within the temporature ran^e measured) will be shifted to higher temperatuxes. An increase in rlacosity nlll increase the reslstirity of the Aroclor. The dielectric constant of a material Is a meoaure of ita polarizability. Therefore, any change in the struoture of the mleoule which will Increase Its polarizability will cause an lncrooee In dielectrle constant. Accuracy it Datm The accuracy of the alternating current data Is dependent on the dleslpatlon foctor of the dleloctrlc at a particular frequency and a particular temperature. The dielectric constant values are accurate within provided the dissipation factor la lesa than 10%. The error la greeter with increasing dissipation factor. The accuracy of loss faetor (dielectric constant X dissipation factor) Is also dependent on dissipation faetor. Aroclor 5442 was the only sample which had a dis sipation faotor greater than 10 and that occurred at the followlnr conditions: 41*C, 500 cycles 41*C, 750 cycles 35*C, 500 cycles Zt will be noted that the dieleetrle constants extrapolated to 100*C. check satisfactorily with the values listed in your letter to Dr. Dump. The direct current resistivity values have a 30* error for the greatest rrslatanee readings on our Instrument. Tor lower reelstanoe values the error decreases. Aroclors 1221, 1254 showed an inoreasa In resistance with time whioh Is indicative of polarisation effects. Tor these materials than, resistance was read after the voltage '$ applied and then at the and of one minute - an empirical method used for talcing a readable value. Aroclora 4465 and 5442 did not abov noticeable pole- COMPANY CONFIDENTIAL TRAN 011923 STLCOPCB4025144 ~2 - 13 - ICO ' December 2, 1947 rirction effects, even at the high tcnqeraturea. Date The dielectric Cbnstant of Aroclor 1221 end 1254 Is Independent of frequency. The dielectric constant of Aroclor 4465 and 5442 Is also independent of frequency at the high temperatures, The liquid-lllce properties of 4465 and 5442 disappear at the lower temperatures where e dispersion region becomes evident. It will be noticed that the dielectric constant curves (at the lover tempera tures) have the same order aa those of the corresponding lost factor curr* end the infleotion regions ocour at the loss factor .maxima tem peratures-. The loss factor curves of 5442 at the higher temperatures show a sharp up-swing, indicative of o large conductance component in the loea faotor. Similarly, the loss factor curves of 1221 and 1254 seem to be in the conductance region. Aroclor 1221 showed on unu.iual aeneltlvlty In changing loss faotor values and os ^eat an lasersitlvity to change In dielectric constant. It was found that a sample measured Initially at room temperature and mausured at successively Increasing temperatures gave different lose foctor values when compared to measurements made with the initial tem perature high and than successively lowered. Results showed that raining the temperature of the liquid or allowing the materiel to stand in tbs open for long periods always lowered the loss factor, probably volatilizing the more conducting or the hifdi loss substanees In the Aroclor. Below 5000 eyclee this effect was very noticeable, the diffe rences inrreasinr with decreasing frequency. It may be mentioned here that loss factor measurements at low frequencies might possibly be uaei os as analytical tool or aa a oontrol method of indicating volatile subatanoes contained in the Aroelor 1200 series. The log resistivity versus l/T graph is useful ee en indication of the change that occurs in resistivity with temperature - or what is related, tbs change in viscosity with temperature. The actual slopes of 44S3 and 3442 cannot be assured sines there should have been more measurements made at high temperatures. Ho.?ever these two Aroclor3 have a much larger viscosity-temperature coefficient than the other two plots. It ia hoped that the enclosed -ranhs 'till summorize the dielectrio properties of tha Aroclors measured. More complrte information or any questions concerning, the data will be sent on request. aom/ Copied by re 1/15/48 COMPANY CONFIDENTIAL R. Lerreeult Monsanto Chan leal Company Plastics Division Springfield, Uasaaehusatts TRAN 011929 STLCOPCB4025145 1-5-10 STLCOPCB4025146 /.too COMPANY CONFIDENTIAL Ip f tc>0'_______ n c o y /9 oo- y f oo ________ f ^ o o '________ frc oo j ui&rrz.t -,U----------------------- - .: COMPANjy CCNF;-':.'2 .'4714 TRAN 011931 STLCOPCB4025147 CO Mpj\hjy confidential TV # / -* STLCOPCB4025148 II--B From - 3,1.0.3. Final GeDort "c. 93 Item Nos. 1, 7, 02, and 21 Taros 12, 13, 14, 15, 16, 4 17 III. CrXCRghiTTP DIFITTjm.. 1. General. Chlorinated diphenyl la manufactured by I.G. Fsrben under tne trade nans of Clophen. 3one types are liquid and ottars solid at norrael temperatures, They are used as lmpregnanta as alternatlTes to hydrocarbon oils end mazes. 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 erode known os T64 la made by I.G. Terben, suitable for trans former cooling. Tfte total output of Clophen A50 and A60 for the years 1938 and 1943 tvas:- 1939 Type A50 1 tons . * A60 132 " 1943 " - A50 170 " A80 508 " The cost of the material in Germany 1s:-- . Type A50 IK. 50pfg. to IK. SOpfg. per Kilogram " T64 111. SOpfg. per Kilogram. The following Is s list of the principal prewar consumers of Clophen :- Gienens-Tchuckert, Berlin. A.E.O. (Hydrawerk), Berlin. Kiaafil (Brown Boverl), Zurich, Switzerland. Alsthom, Poris. Ducatl, Milan, Italy. It was stated that no German capacitor mnnufaeturer uses Clopben for the manufacture of small capacitors for radio and telephone purposos and where these have been used by the Ger man fighting services they were supplied by the Italian firm, Ducatl. - 2. Manufacture. (i) n synthesis of diphenyl from benzene. Diphenyl Is synthesised Tran benzene as shown In the flcure, following:- 1 COMPANY CONFIDENTIAL TRAN 011933 STLCOPCB4025149 f fH1 --s.'WV---Condenser r] Distilling " Column 500-650*wC< 200 *C Two-staae Host fbrchancer Heaotlon coil soon; Synthet.ls of Diphenyl from Ueazene The syntbosls occure in the vapour phnee, at 000*0. and atmospheric pressure, in an electrically heated reaetion coll of eopper-aangoneoe alloy. No catalyst is required. The apparatus, apart from the reaotion soil, is of Iron, mid oporotes at the tanperuturea shorti above, ..bout 10,' of the ben2ene vcpour is oonvertod Into diphenyl in one passage through the reaction coil. The purity of the benzene la of importance for the elec trical quality of the ultimate chlorinated produots 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 undeslroble Impurities or the mechr.nlov by which they cause poor electrical performance. Thiophene ms stated to be definitely harmful, and vague reference vs made to "nltro-compounds", to "aliphatic hydrocarbons" and to "substances which could not be chlorinated". The prs lss nature of these materials was not knows, but their absence wea ensured by obtaining benzene always from suppliers whose product wos known to be satisfactory. Analytical Specification for Pure Benzene Appearonoe: Clear end colourless. Density at 20*c.; 0.876 Diet111Inc range; first 5 within 0.23*c. 9 - 95/. " 0.25*C. 95;. - end " 0.23*c. Solidification point; .lot leso than 5*C. Bromine consumption: Not more than 0.5 911. bromine per 100 c.e. Sulphuric acid test: Not more than 0.15 9a. KzCr,07 Carbon disulphide: Shall be free fran C3*. COMPANY CONFIDENTIAL TRAN 01193. STLCOPCB4025150 Difficulty la the synthesis was still beinr experienced, due to rapid eorroslon of the copper-nan^aese reaction coll, operating at SOOd. ,\ smell scale exnerlnental apporotua usin." a fused silica coil had been .made, but had not beon developed for production use. In addition to diphenyl, about i% each of 1-3 and 1-4 terpheayls are produced by the process, These are se parated, chlorinated and used in sealing Tarnishes; present production is about 4 tons per -nonth. No use Is made of ehlorterphenyls as paper lmpre^nants, since the materials are resinous and tend to crack; moreover the permittivities are lower then those of the chlordlphenyls. The erude diphenyl is next purified by distillation. During this process the terohenyla remain in tbs residue. They are extracted in the following nanner:- The residue is dissolved in hot benzene, filtered, end the 1-4 isomer obtained by fractional crystallization. The crude product is distilled in vacua, yielding 1-4 tsrphsayl with Belting point of 208*C. The 1-3 isomer, remaining in solution in benzene, is more difficult to isolate. The solution Is clarified -.rith activated char coal, filtered, und the benzene evaporated. The residue Is distilled to yield 1-3 terphanyl v;lth siting point 80-84C. (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*C., agitated and chlorine passe.. in. The addition of ehlorlae la continued for 100 houi-e at a rate of 130-135 kg/hour during which tine the tem perature It raised gradually fron 110*C. to 150*C. The and point of the chlorination la deteroined by measuring the density of the product. To remove hydrogen chloride formed in the process, dry air la blo through the liquid for 2 hours snd this hy drogen chloride is recovered. The produet is transferred to another vessel snd treated with 1/251 of solid sodium hydroxide, heeted end agitated. The sodium hydroxide Is allowed to settle out snd the Clophen drawn olf from the top, transferred to another vessel to which fuller's earth end soda ere added and the liquid redistilled. The stllle for this process ere ges heated. COMPANY CONFIDENTIAL TRAN 011935 STLCOPCB4025151 3. Trcpcrtlc a . (1) Capacitor Inrrcactljg grades. A urjBor7 of the physical and chemical >ro-rtie of the capucltor liapregjw ting trades of Clophen la riven In Appendix II. There are six gredeo of capecltoT lwpregnant, A33. A40. etc. up to AflO, the 3, 4, 3, etc. indi cating the number of chlorine radicals combined -,1th the dip'ien:. 1. Tech grade eonta lue a proportion of the adja cent homologuea not exceeding 20/,. Grade '.30 has the highest value of permittivity. Theoretically the hirbest value obtainable -.'lth a chlorinated diphenyl Is 9.0, and a grade haring a permlttlTlty ol` 7.0 has been prepared, but Is chenicelly unstable, and rery sensitive to aolsture and Impurities. The most commonly used grades are a50 and A60; ASO Is the most stable grade and has the Iciest dielec tric loan. Crada A60 Is considered by 1,0. to possess the optimum ooablnetlon of non-inflanrhabillty, stability and viscosity. As with Nibrsn, It io considered that no addi tives are required since the substances are stable in use,, provided that the capacitor* are efficiently sealed against tho air. Kicufil of Zurich are the only users of A30 and A40. The foHoning table shows tho variation in oapaeltance and pov;er factor with temporuture for a Clophen impregna ted paper capacitor. Tho ijnprec&Q&t is A30, tho dielectric is Gchoeller and Hoesoh "A" finish reg tissue (density 1.2 - 1.25) with a thlofcnees of 10 a; froouoncy of measurement is 000 c/s. Power faetor shows a maximum vslus of 0.052 at about 4*CS while capacitance foils off by 9oae 20(Z at temperatures below this critical value. Variation In ctpaeltanes and powcr-factix with tamperatige for a Clophen-Impregnated capacitor. Temperoture CC.) Relative Capacitance Power Victor -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 (max.) 20 1.10 0.006 40 1.10 0.005 60 1.10 0.004 00 1.11 0.005 No evidence was obtained from 1.0. on the use of any type of eddltlve with a view to depressing the temperature at whleh the change of state oeeurs. COMPANY CONFIDENTIAL TRAN 011936 STLCOPCB4025152 The method adopted for evaluatin'* the vmter content in oils such es Clophen is described In Appendix III. It is also applicable to such solids as Nibren. Tngelhardt stated that no source of failure had been ex perienced durLnr the -stile period of production of Clopben, which is about 17 years. Consequently no improve ments or nodiflcations had been made or found necessary during this period. (2) Transformer-coolin'? rx3de (Clophen T64) . No detailed lnfaratlon -ms sought on this material, since it is unnuitable as a capacitor imprsgnant and is only used as a ooolant for tranuformers and phase shifters. A sumaury of its physical and chemical properties is Given in Appendix 17. It has a lorn viscosity, is modsratsly stable under electriesl stresses and has the distinct ad vantage over mineral oils of being non-inflammable. Tbs principal users of this product are A.E.O. and "lenena, but it la understood that, as with other chlorinated com pounds, conservatism ond prejudice among customers have prevented its wider use. No stabilisers are added to the muter in 1 as their function of absorbing hydrochloric acid would be defeated by the formation of "chloride salts", which in turn become elec trolysed. It was said to be vary important to avoid con tamination of Clophen T64 which may occur in transit and for this reason the use of leather for raskets mist be avoided. 4. Methods of use, precautions, etc. No detaile were obtained on the method of impregnation used by I.G. for the construction of test-specimens of Clo phen- impregnated capacitor. This v*s partly coused by the non appearance, after the first day. of Efegelhardt, but it is not considered likely that any novel processes are involved. Tot information on the precautions necessary in the use of Clophen, see Teetion II. 5, above. re 11/19/4? COMPANY CONFIDENTIAL TRAN 011937 STLCOPCB4025153 IH-A-b - 5 DC ,r'-3n - H.I.O.'j. final Report "o. a?3 Iter* flos. 1, f, 22 and 31 Pf x It Clopben la mode In several rr-des, viMeb correspond closely with their U.3. counterparts, A.50 belnp the .xude moat connoaly used for capacitors. _ Lxcept for rery rare use by ",lemons and ITalake for special orders, Clophea bos not been uood la Germany for snail capacitors of tbe teleoomrunioatIon type, but It hcs been used extensively by olenens-'chuckert for pov/er ospocltors. It le Interestin'- to note that the Gemnn forees used Clopben laprecaoted and filled tubular capacitors node by Dueotl, of lillan, who obtained the lmprecnont from I.G. The prejudice apslnst Clophen vra, bowover, bolnp. gradually overcome and several manufacturers were eont enrols tine an extended uae of this notarial. Gome of than con sidered It to b equal to or possibly hotter than mineral oil for opera tion ot power frequencies. rs 11/24/47 COMPANY CONFIDENTIAL TRAN 011938 STLCOPCB4025154 III-A-b-50 Prom - B.I.0.3. Final Herort rTo. 833 Item Nos. 1, ?, 22, and 31 Paf#a. 98, 99 (2) Clophen The only chlorinated Lapreraant used by CienensSchuckert la Clophen, supplied by I.G. In power factor correction end hlph voltage applications It la 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 hare been tried and found unstable. *1.80, A.?0 and A.80 ure too viscous to allow for (rood impregnation and have lower permittivities. Although the vlaooalty of A.50 at room temperature la much ereater than that of oil, the viscosity ofc Impregnation tempernture is sufficiently low to rive no trouble in attaining thorough impregnation. A routine cheek on conductivity is mode on each drum of Clophen, and formerly if the conductivity were too high, the Clophen was treated with powdered chalk to neutralise the free acid. As the result of continual pressure on I.G. over a period of years, the acid content had gra dually diminished, and it is now possible without chalk treatment to work to the same rejection limit of resietlvlty as for oil, viz. 1013 ohm..cm. at 20*C. Drums of Clophen falling to pass the conductivity test are returned to I.G., unless urgently needed. A certain elasticity is permissible In view of the hl^i standard sot. Apart from conductivity, further acceptance cheeks are specific ^avlty (1.54-1,55) and permittivity (5.0 5.2). Permittivity Is measured at 800 oyoies and 20*C, on a cohering bridge et low voltage. The acceptance standards for Clophsn A.50 are shown graphically in Appendix XXXIV. Clophen costs about 1 U. do pfg./kg., and is therefore much dearer then oil (30 pfg./kr.). This extra expense la offset, however, by the use of a special design whieh reduces tbe amount of Clophan required. An ad vantage claimed for this lapregnant is that is has a similar permittivity to paper (vis. 5). Other lmgreggants studied. As Clophen Is considered nearly ideal, no serious attempts have bean made to find superior materials or addi tives to improve Its performance. This attitude Is sup per ted by service experience, la which no failures have been reported. It la realised, however, that on froezlag dischargee nay ooeur in the oontraetion voids, whieh may result In decomposition of the Clophen and failure of the COMPANY CONFIDENTIAL TRAN 011939 STLCOPCB4025155 dielectric. Tests r;ere performed (see faction 17, 2, (3;: to check r/hetbor this degradation does ir faet occur, and no failure vsbs noted. Nevertheless, 1.0. supplied snail sartroles resembling Clophen A.SO but haring a lov;er melting point so thut this possible source of failure r. >uld be Investigated. Uepresslon of the temperature at which the dipoles baear* lmoblle should raise the maximum usable frequency and hence broaden the range of applications by Introducing those ror audio-frequency furnaces. Two of these I-C, .qamn'lea, v'lth references A.1S1! and A.162N, are, like Clophen, nude from benzene, but hare a lower chlorine content because of the presence of un additional alkyl group (CjjKan+1), and hence a lower density. Their advantage over Clophen ,`..50 la that the setting point (l.a. tamporotura of maximum dlepersion and of capacitance diminution) la lo-.Tored from -0*C. to -17*C. The permit tivity, vlaooelty and noo-influmnablllty resemble those of Clophon A.50, The viscoslty/temperoture curves of these two samples, K.7 mineral oil and Clophen A,50., are oompared In Appendix XXX7. ra 11/19/47 COMPANY CONFIDENTIAL tran oimo STLCOPCB4025156 III-B-2500 December 22, 1947 TO: FHOTM-.i'E. DIVISION 3JI\J: Arcelor 5460 as Used Ln T.thylcellulooe Lae.-.uer RE: federation of Paint and Vjraleh Production Clube Official Digest (October, 1947), Aroelora used as plasticizers and reslno impart excellent qualities to ethyleellulose. Uthylcelluloae la used ln lacquers of vuriouo types, the ethylcellulose acting os a long chain rolyner to inpart toughness and flexi bility and to Increase the speed of drying. dome of the prlnclpol uses for ethylcelluloee lacquers are for the ooetlng of high tension ignition cable; heat sealing lacquers for foil and puper where the slight discoloration which may develop ln nltrooellulose laoquers on heat aeallng ie not permissible; linoleum lacquers whore alltoll resistance la essential; textile printing.; printing Inhs, particularly ln multicolor designs wljero hydrocarbon solvent does not soften or blocd Into rreviously printed desirne; ulroroft lacquer for resistance to both hoot and cold ond to nuiok temperature ohan/rea; record lacquers, especially for home rccordera; and ln wood sealers where good saodlag and flexibility ere assent lei, A good pigmented ethyloellulose luequer but been node, based on the following formula: Ingredients Kthylcellulose N-22 Aroelor 5460 TlOj Menthylphenol Toluene Ethanol ftrta (by weight) 6.4 6.4 4.2 0.06 67.0 16.0 100.06 rh Copied by rs 2/2/48 Benlgput COMPANY CONFIDENTIAL TRAN 011941 STLCOPCB4025157 ?ron - "emo G.Y, Frankle/P.0. Psnl^nuj March 11, 1948 ' Soil-Poison Conoentrete As described below, tba *. materials sro formulated into a water emuleifloble soil-poison concentrate corrylnc almost 30 par cant by weight of uctiva lnrxedlcnts. Arocior L24 Trlohlorobenzane (ilxed Isomers) Pentoeblorophenol Isopropyl alcohol Toluene or Xylene Gterox GE" San tone rse 3 Pasts 33.3V 33.5 10.0 3.3 16.7 1.5 1.5 100. Of, * Other non-ionie typa emulsifyla- amenta such ae Triton Ntt or Span and Tween oos be used to rsnlsce the Storox SE. Copied bp rs 4/2/48 COMPANY CONFIDENTIAL TRAN 01 l STLCOPCB4025158 Chemical Abstracts por;inLr u ;e of AnocLom Vol. 41 Paga 60o7 ni-H-io U.S.P. 2,425,973 to Andersen and Coalahan, (Hercules Porter Company). Foundry eores sprayed vrith 1%' solution of chlorinated naphthalene in hydrocarbon solvent she? creator scrotch resis tance thnn untreoted cores. Cl2 content remains from 40 - 80.' Cl* . Partleulurly rood for use ilth .1 eastinr9. rs 12/2/47 COMPANY CONFIDENTIAL TRAN 0119*3 STLCOPCB4025159 17-10 Ftjui - 3.1.0,3. rIns 1 Report ''o . ?y;Iten Mos. 1, 7, Z2 ecd 31 " Parcs - 10 and 11 huch less trouble hee been experienced with eblord 1 -henyl than with ohlonuaphthalene, prcbubly beeauje the former, bein? liquid ln- volvee leee phyical dontuct Ln dlspoeel. '' (2) Preventlog. Very thorough washing of ell arees of the skin likely to be contaminated with solid, liquid, or fumes hee always beon the basic principle ln prerantlon of skin troubles, and In still looked upon as fundamental. ."hen fatty soaps eoaaed to be oTalloble, because of the di version of fats to food, it became essential to Insist upon ths iiss of barrier er shims, of which the beat nes one named "rvun.30", reads at Trommersdorf. This hss now been replaced, for lack of supplies, by an alternative soda by I.G., named "f'lTITAL*, whleh Is considered inferior to 'ulmbo but satisfactory. The FIssnn firt put up a special powder named "rCT'TFTLHJLV'tS" to act as s barrier, but this ma found to be inefficient except to allay irritation on skin oraas exposed to fumes only. For this purpose it still finds use at Leverkusen and et the Hydra.lerke faotory at 3erlln. A special point ie .`hade of fume extraction, and the minimum uir speed away from the operator is 1 astro per seoond. To cheek the efficiency of the precautions, a thorough exami nation is made every 4 weeks of every worker coming into contact with chlorinated hydrocarbons, and sines the enforcement of the precautions, no deaths or symptoms of Internal injury have occurred. ~>lnoe superfatted soaps have ceased to ba available, a cleansing composition containing Alehlor-methane has bean devised. This Is so powerful a detergent for chlorinated materials that barrier creams are considered unnecessary, but it is uncomfortably irritant to many aklns. (3) Cura. .'hen severe attacks of ehloracne ond internal sickness were encountered, in the early years, when the properties of chlorinated materlols were not well understood, extensive rest periods had to ba prescribed, together with e senerous diet, entire absence of further contamination, and long periods in the open. Tines precautions have been taken to minimise the effects, only s few mild eases of ehloreens have been t. Tbeae have been treated with a solution of acetic and salicylle acids ln methylated spirits. COMPANY CONFIDENTIAL STLCOPCB4025160 ! 4) Conclusions and Facomnende t lo no . 1.5. oonsldor that neither ;cxiclty nor 9i<ir. affection need now h any deterrent to the use of chlorinated naphthalene, and that chlcrdlphenyl la If anything less troublescrw. Certain people, notably those -1th fulr skln.-i, show distinct nllorgy, and or boot diyertcd to other -;or'< not lnvolvlnr contact. Corupuloue cleanliness of the skin (Including tbe face, neefc, and arms) and of the clothlnr (esoeelally iindcrrornent9) la essen tial and noeds strict enforcement. .'ashing v;ith hot vt?r and good soap la sufficient, so lon^ as the soap Is superfatted since tho skin becomos sensitive to irritation by alkali, 3arrlor cream should be used on thooa parts of the skin which oome Into contact with solid or liquid material, and the aren of contact ahould be minimised by tho use of protect It# clothing and ftlotoj wiiero possible. Areaa of the akin wnloh ore contacted by furaoo only, end particularly those chafed by olothiag (e.r. the nook adjucent to tho edg of the clothlnr,) need protection by a suitable soothing powder. here fumes are generated, thoy should be drown oway from tho operator nt on air speed of at loost 1 netre per seond. It may be found essential to hare two ducts, one at floor level end one overhead,, with exhaust in two dlreotlons simultaneously. In ease the procautions are belnr eroded, or lest there should bo acne idloaynoraay, monthly medical Inspection Is desirable. ro li/24/47 COMPANY CONFIDENTIAL olm5 STLCOPCB4025161 rr-3-icc from - The Journal of industrial Hygiene 3nd fo'icolo^y Volume 20, Number 2 February, 193R :t>rp:ioi.ocici. cr^oo: ej nr i.rvruo ok rt.n REX'LTING FTiOr: RXt'OXHT TO CVTTAIN cin.oRm-.no inn)Roc.a!BOfn Chlorinated hydrocarbons, particularly chlorinated ntiohthclenea tjnd ehlorlnutad diphenyl, h:>ve been used extensively In certain In dustries. Their uoo In the manufacture and nreoen.tion of many types of oleetrlcul eoulpment Is constantly lncreaeinr. ,ilthou"h it Is known that some of thene compounds cause sene, only recently hes the possibility of nore seriouo oyatenic effects been recor^laed. The precent paper describes t) natholo-lcal chanres obserred in rots tbr.t had teen exposed to various chlorinated no-hthalcne com pounds and to chlorinated diphenyl. Compound Cr (chlorlto tod diphenyl) as administered to two "rouxi of anlmols In low concentrut ions. .ji aTcrj^e concentration of 0.37 rants. por cu. m. vju9 employed 16 hours dally for 134 days In the first experiment. In the neeond expsrinnnt (enployinr on OTcrure sir con centration of 0.93 .mens, por cu. n.) the animals -'ere exposed P hours dolly for 143 days. The prenent experiments demonstrate that chlorinated noobtholene compounds and chlorinated diphonyl ore capeblo of raroducing marked liver darnels in the nh ite rut without demonstrable nicrooeo-lc chun^cs eppetrinc in the other1 orr,~na. Furthermore, the characteristics of the liter lesions reeultlnr from comparable anounts of any '-Iren com pound are the seme, re.-ordlcos of the method of odnlniatrutlon (Inha lation, feeding, or subcutaneous lnjeotlon). Of the various chlorinated hydrocurbons tested, oblortn ted di phenyl rate eTidence of boinm the most toxic. j"hen administered by Inhalation in tcry low concent ret ions (overact 0.37 to 0.93 m'Tns. per cu. a.) liter cell ehan'-cs -.vere very pronounced after the first exposure period. The most striking chanpe was the byalinlzetion of t the cell oytopleem (sea fir. 6, plate III). Such cellular alterations were essentially unebanred after a 2 month recovery period. In these enlmele snail eublethal doses of Curbon tetrachloride and alcohol uni formly produced extensive liter necroeis and was hirMy fatal to them (fir*, l and 2, plots VII). Chlorinated diphenyl fed in all doses nrodueed similar but more marked liter injury lsee fl*. 5, piste III). In large doeee thle eorapound wee hitfily fatal. Tha litar ebonras In animals dyin?. after short exposures mere lnccrsolcuous and consisted mainly of swelling of cells and active regeneration (eee fig. 4, plate III) Uoweter, animals removed from exposure before being futelly COMPANY STLCOPCB4025162 2- poisoned, wabssquently developed hysllne degeneration of liver calls similar to that produced by proloarrd jdmini*trot ion of wall doses of th1 eompound. Thus tho results of the Taient study, as ell as certr. In field studios that hove been n*jd* (1) suyest that the solution of the in dustrial hazard Involved Is dependent largely on e reduction of the air ooncentratIon of these compounds to a level that -illl not oroduce liver daraore. The present experiments Indicate that lo-.rer air con centrations must be obtained In the cose of the more highly chlori nated naphthalene oomoounds and chlorinated diphenyl then for tricolor-- BDhthalenen If u safe environment far "rorlcmen is to be assured. He- cuuse of the pronounced toxio effect of snail doses of carbon tetra chloride on the 1 Ivors of anLnuls already Injured by exposure to chlorinated naphthalenes and ehlorlnatod dl-dienyl.. Its ace as e sol vent for thooe compounds v/^uld anneor to be very hazardous. ra 2/3/49 COMPANY CONFIDENTIAL TRAN 0119*7 STLCOPCB4025163