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rr*. J.A RZPORT NO. 2213 FINAL REPORT ON -JPC LOR O.OT~ BOOK Job No. 171--<51 ril* No. 141-27.1 April 27. 1948 R. R. Knlaht RESEARCH DEPARTMENT P1io*pht* Dhriilop 2215 '(u"K fW I0-ILizlA Monsanto Chemicals COMPANY ' CONFIDENTIAL TRAN 011867 WATER PCB-SD0000001029 HXP3R? HO, 2215 FIXAL RJPCFT m THIS ROWT AND THE INFORMATION CONTAINED HEREIN IS THE PROPERTY Of TH MONSANTO CHEMICAL COMPANY. ABOCLOR DATA BOOK Job Ho. 171-401 Fll# So. 141-27.I RESEARCH DEPARTITEBT - PHOgpgAB DIYIglOH - Annirtoc, Alabena a***4*********** Raport 9obittd - April 87, 1948 Cbaaiata: A.M. Illanbur* B.R. Kflleht Prepared by: R.R, Inlgbt Xlghtaaa oopiaa wars nada of this rapart and dlatributad at follova: . Ho. 1. Raswaroh 7Ut Ho. 2. R J.. Jsakla* -O.B. Dargia Bo. 3. R.R. Cola - B.3.Haathorly Ho. 4. V.T. Durratt -F.P. LaBalia Ho. 9. H.F. SiflTir Ho. 6. G.A. Hoetemlt * Ho. f. X.P. Ruofcar Ho. 8. X&gmr X. Hardy Bo. 9. J.F. Raavaa Bo. 10. JJ. Raorat Bo. 11. AJI. XUanborg Bo. IX. V JL. Eal#* . Bo; IS. Paul Lopia ~8o. 14. P.0. Beal*ssaa lo. 18. ' He. IS. Ho. 17. Ho. 18. . Tblfi If oop7 Ho. J3 COMPANY CONFIDENTIAL ' TRAN 011866 WATER PCB-SD0000001030 SSTSARCH DOTAJmsifP - HIOTPlL.Tr DI7HIW MCSflANTO CHUOCAX COT-TP/vHT Anniston, Alabama A ROC L OR DATA BOOK General Lafornatloa on properties of Aroelors, Aroelor process dU, uses f Apoclon, sad physiologies! effects of Aroelors. FORK-.) 0TO A* a turn of present Lag the available data on Aroelors to the in terested personnel within the k'onsanto orgenliation, this looaeleaf notebook la belne compiled, , Moat of the dote has resulted free* work carried out with In our onn organization. Literature references, however, will be cited In all oases throughout the compilation in order to allow acre date lied infor mation to be obtained by the user, . The following detailed outline le for facilitating the location of data in the book and to assist in properly inserting new data sheets. Each Aroolor is to be given u series number for location under the headings. This scheme at present Is as follows: Aroolor 1221 _ 100 series Aroolor 1232 - 200 series . Aroolor 1242 500 series Aroelor 1248 400 series Aroolor 1254 500 series Aroolor 1260 - 600 series Aroolor 1262 - 700 series Aroelor 1268 - 900 series Aroolor 1270 - 900 series . Aroolor 1271 - 1000 series Other Diphenyl Aroelors - 1100 series ` Aroolor 446S - 1500 series Other ,HlAh Boiler Aroelers 6100 series ` Aroolor 8442 - 2400 series Aroelaar 5460 - 2500 series Aroolor 5468 2600 series Aroolor 5468 - 8700 series Arcelor 2565 3000 series Related Compounds - 4000 series TRAN 011869 COMPANY CONFIDENTIAL THIS REPORT AND THE INFORMATION CONTAINED HEREIN IS THE PROPERTY OF THE MONSANTO CHEMICAL COMPANY. WATER PCB-SD0000001031 -2 - Th* peg* pertaining to the solubility of Aroelor i463 In rerlous solTents would be of this type "IAJ - 1300". In oases where the lnformotion for ell Aroolora can be compiled cm one sheet, eueh ee refreotIts indloea, the pare will be Inserted under the general heeding and will bear ooly the Dumber for the fLret Aroelor, for example, lAh - 100, I. GBHSKAL WOP^iJTIEl 07 ,.ROCLOR3 A. Physical Properties (a) General Phyaloal Constants 1, Formula and molecular nelpt 2. 3peolf lost Ions for Manufacture (b) Danalty and ipeoiflc Orarlty (o) Cubloal Coefficients of Srpanalon . (d) Vapor Pressure and Rote of Preparation (0) Speolflc Hast end Heat Cepeolty (f) Thenaal ConductlYlty (g) Viaooslty ' (h) RefraotlYe Index , . (1) Heats of Vaporisation - Other Thermodynamic Properties (J) Solubilities (k) Flash and Flame Points (1) Liiacellnneoua B. Ilsotrical Propertlss (a) Dielectric Constanta (b) Power Factors (a) Dielectric Strength (d) Volume RealatiTlty (e) Dipole Xausnts (f) Ml soellaneoua COMPANY CONFIDENTIAL 011870 WATER PCB-SD0000001032 3 II. KSmiDs or mahgfactori* A. Eeaeanto Proe8 1. Ree Ifcterlale 2. Chlorlaetle 3. Dirt illation 4. 3torege and Chipping B. German Proceed . C. Other Processes III. 03K3 OF AR0CL0R3 ,, A. Eleetrloel Field 1. . Transformere 2. Cepe alter e 3. Coe ting for 7ire 4. Other aeee B. Fernishee C. Plaatlolsers D. Hydnsulle Fluid 3. Fire Retardante F. HeetLag aodluB I 0. Mlseellensotts &. . digest loss for new Uses IF. HITOOT-OOICAL ifTSCTS 1. 3kla Teste E. ( 3yste*etie Teste ' i p~ram miHO aroclors COMPANY CONFIDENTIAL . TRiN oiuu WATER PCB-SD0000001033 THIS REPORT AND THE INFORMATION CONTAINED HEREIN IS THE PROPERTY OF 4 THE MONSANTO CHEMICAL COMPANY. The book 1 subject to revision sad ehanges as various data ara located. Graphs and diagrams will be Inserted when possible and new graphs drawn as Information 1 oorapiled. No Indices of Motions la planned ,ut this tins, but later re visions may Include such page if the volume of Infoxmitlon warrant It. Contributions of new and supplementary data ere earnestly so licited. Any dlaorepanclea In the existing date or advioe aa to a better means of presenting the Information will be greetfully acknow ledged. Address all correspondence to the group loader In oharge of the reeearoh on Aroclors at Phosphate Divisi on - Research Department, Annlstoa, Alabama. R. H. Knight rs 12/2/4? COMPANY CONFIDENTIAL TRAN 011872 WATER PCB-SD0000001034 rr i.. STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTOM, ALABAMA Ptf# N. PRODUCTt_AcMlar,JUn. GRADE; Herular _________ ____ CODE NO.: i04Q-C2S-rW)q AUTH0&MRr 4 6 1946 PROD. DEPT. NO.; _________________ SUPERSEDESi^ftjhBCmt^tiyw R#LJ* | A4UIl ) |f APPROVED BY (Initial*) i12eAE ruiauA Umia^m iZmlZadA _________ _ Control Specification Consumer Specification Crude Arooler 11211 Tp, Or. at 68*0, Aoldltf, rvz. riaOH/pja. C Aroclor 1221! Oolor Acidity, me, JfoCII/c7n. Op, Or, ot 60/l3.S*C Chlorine coo tout Viscosity at 100*F* 1.150-1.160 40.8 40 ,'iTTU max. 0,01 max. 1.143-1.150 20.3-51.5,: 36-41 3 NOTES: Copied tey rs 4/8/48 COMPANY CONFIDENTIAL TRAN OUS73 WATER PCB-SD0000001035 - r. \ ftAmAMD SPECIFICATION - OF Mow sawto Chemical Company PHOSPHATE DIVISION ANN 1 STOW, ALABAMA Pag a Ne. ____ PRODUCT: Aroolor LESS CODE NO.: 1040-23<wy&-f>q GRADE SeruXatf PROD. DEPT. NO-i _____ ____ ___ ftL*J'eJ A iVEi | APPROVED BY (Initial*) SUPERSEDES:. ImSasfelilia. y.F*R. FA*8* Control Specification Consumer Specification OnM AroeLar L1S21 "Jp. Or, at 68/15,8*0* Aimr, g* Haan/e** .`.roe lor 12381 Color Aoidlty, rv, RcOH/j'S, 7p, QT, at 65/15,5*0 Clilcr Lna content Tiaooaitjr at 100*7* 1,840-1.545 <,0 ,5 00 ~P5U aaz, ,01 nx. 1.235-1,540 51.5-5J.5 46-49 303 NOTES: copied *7 re 4/B/4S COMPANY CONFIDENTIAL TRAN 011874 WATER PCB-SD0000001036 3TAHDM 3PSC UlGATICIf cr MOW3AHTO OKMICAI COMPAfCr Pre>4u%; Chlorlaatsd Sighac-yl, dltlU8 Cods Ho. 1040-E40-73-09 Ond i Azooior 12&S ................ . _ ^ Dot t Author!:' Jung 21, 1940 3ap>trsi!a Spool! leatloa D&fcod July g 1954 Tolerable Lindt * fypiael Value 3p. Or. at 65/18.5*0. Color, RJA. Aoldity, M^s NaOH/pa. Tlesosity at 54,4*C. 1.538 to 1.868 0.5 l&scimuB .01 ifexlmUH 47 to 50 Soeondg 3yboli Uolrerwl Ajir0#t %f Approvtd w A. B. Oortor ' ~SET*? 'WmmiWt Mw A. 0Bbl. ??. lorksTEi!* e r Appro? i By Bobrt S, Seatherly *' "IKsa gar AuthorIsod by 7. M. Oarothaw _________ ` m x Blrooio? Copied By y* 4/8/4 COMPANY CONFIDEN* IAL TRAN 011375 WATER PCB-SD0000001037 TEAJDAflD SFSC1FICATIOT . OF . mcroawtc amacAL company Product; ChlorlaatM Dlphaayl, Slgtlllad Sods Ho. 1040"2S-75~0f Oraflct Axoelor 1848 - Data AailisriMd i'ua# El, 1940 Suparaadei 3pLfl%ioB Dstd Toly 3, 1934 Tolarabla Limit,* Typical Tala# 3p. Or. at 63/15.5*0, Color j W , Ability, MgraN&C^7pi Tiaeosity at 54.4*0. 1.404 to 1#414 0.5 Maxima * .01 Maxima 69 to 76 Oaoosssts Oaybolt Baiws^L Aroelor 1862 Op. Sr. at 90/15,5, Color, IJP.A. Aoidity, % HaOH/g, Tlsacaity at 98.9C, . 1.572-1.585 1.0 Ifexiarai .01 Maxima BS-100 933 Co Wo. 1040-310--76-09 Approrad by A. . ter%m _ ' Chlaf Ohaaiai Approrad by Ida. A* 0*laal. Jr.____ lif !br% S, faatharly -----------------------S&BffSTiF tottorta#! by J. H, Carat hara ; _ _ - ^7aie#j_ j ^f Cpl4 ty rs 4/8/48. ^ COMPANY CONFIDENTIAL TRAM 011876 WATER PCB-SD0000001038 3TAJ-CARD SPECIFIC TIDE MDK3AHT0 CHSJCAL COUPAWT Producti Aroolar 1254 ________________________ Code Ho. 1040-290-75-09 10/s/ilQrade; DleleotrloDate Authorised Supersedes! 6/gl/iO Color, AFHA So&le Conditio* Speolflo Gravity at 53/15 .0*0 Acidity, Ug. lUQH/o*. Inorganic Chloride*, ppm. 3*ybolt Tlsooslty at 98.9*0, boo. Dleleotrlo Oonetant et 100 "C Resistivity at 100*C, obsv-ca. at 000 volts Refreotlve Index at 25*0 D1 tilling Maps, Observed, 10% Observed, 50% Observed, 90% Pour Point . 7ater, ppm. Ivaporatlcn, 6 Hra. at 100*C Corrosion Test-Chanf.e In weight Acidity after teat Inorcanl'e^STorldas after test Condition after lest Color ' afSer test TM t/u/is 100 llax. Clear 1.495-1,506 .01 0.10 Ubx. 44.3-47.8 4.15-4.38 Above 500 I 10 1.5370-1.6390 360-385*0 355-36**C 36*-373*C 8 to 1* 35 llax. 0.4% 0.0% 0.01 0.10 Ubx. Clear 130 Ilex. COMPANY CONFIDENTIAL TRAN 011877 WATER PCB-SD0000001039 g-DUCURD TPECincm cr Monsanto chjmicai, cowpajct Produot: Axoolor 1X60 On d a: Dl# lsotrlo Cod# No. 1040-290-78-09 Date Authorlxed U/18/41 Supersede: 1/50/86 Color, AFEA 3o*l Condition 3p#lfi Or#Tltjr at 90/15.5*0 Aeidlty, Ugn. KaOH/ga. Inorgenlo Chloridee, ppn. Saybolt Vieocmlty t 98.9*0, m, Dielaetrle Constant at 100*0 Resistivity at 100*0, oh*-ca. at 500 volte Refractive Index at 8*C Distilling Ranee, Observed, 10* Observed, 80* Obaarrad, 90* Poor Point Water, ppn. Evaporation, 6 Etra. at 100*0 Oarrodon T*st-Ctenge In weight Aeldlty after taat Inorgnnlo thlorldea after taat Condition after teat Oolor -- *1Ffcar taat 100 Idax. Clear 1.550-1.860 .01 0.10 Max. 75-60 3.6-3.8 Above 500 X 10 1.6455-1,6465 370-377*0 377-380 *C 385-400*0 86-34 55 Ikx. 0.2 * 0.0* 0.01 0.10 Max. Clear 150 Max. re 8/11/48 co c0NFIOENt'AL TRAN 011878 WATER PCB-SDOOOOO01040 SPECIFICATIOS3 TCR SOLID DI3TTLLB) AR0CLCR3 KMIBf APPBABMC^ t CpTffl mu FOTTTT ACID 1*0. jfeJleQg/fl| CPUS 5% TDIUBBt KKLTTSO POIOT TOTAL CHH3BHg wee wee 0 Oo 50 0 t) m WTO 18T1 3bit to -yellow eryetalllae powder 'Jilt to grey or 110t yellow crystalline poofter Ohlte crystalline powder Prsetisally white 110* fluffy 130--160-C. 0.00 Max. 22S-J2S3-C. 280-300-C -- 00 APH& *1. 00 Aim * 304-0. Mia. 69.5 TO.351 >r~ Cfl4 by re 4/8/4 O *0 WATER PCB-SD0000001041 Cj M STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON, ALABAMA Pag* No. PRODUCT: ..Araalor 44fiB tailor I GRADE: ___ ___________________ . ---- CODE NO.: ldfldLaQ=ga.a DATE _____ AUTHORIZED: Qetnbat. &1 iqaa PROD. DEPT. NOj _____________________ HiLiJei n*F. ;.| APPROVED BY (Initial*) 9s944 __ SUPERSEDES: Am 6 3. 1944 P.L.) fl.l.T.l E*A,B, Control Specification Coiuumv Specification Appeoraaot : Color, loftonlB Point U.3,r*M.) Aaid ifusber (L^rtaon/rn.) CryntoJL Unity eleor, 11;^h% 7llcw# brittle routs 2,0 rax* 60 - 66*0, o - * V. No. *P*. * naluta color Unit to 2.0 moslraam Is momoa#a beoau liir>notloa records show that all lota produced la 1944 bare bod s eolor of 1 Jb. NOTES: Copied by r 4/8/40 COMPANY CONFIDENTIAL TRAN 011880 WATER PCB-SD0000001042 3TAffPARD gpgsmCATICH cr MONSANTO CHEMICAL COKPAJTT Product; Chlorinated High BoilerCod* Ho. !CX0--ta0?5-O9 Qrede: Arodar SidO________ __Data Author lx ed I5*jr 10, 1940 Supersede* Specifiostion Det*d December 23, 1932 Tolerable Limit* Typical Value Appearaae* Oolor, H .P .A. Crystallinity Teet Softening Point, A3TH . Acid Number ttgm HaOH/gm. Chlorine Clear, light yellow, brittle reela 2.0 maximum To peas teart 100 - 108.8*0. 59.0-00.6% Approrad by A. B. Gerber -------- ---------flfcTTf SuSTet Approred by Btw. A. 0'Beal, Jr, .... .. ....1?otE* Manager Copied by re 4/8/46 Approved by Robert 3. Weatherly, 5/6/AO Seles Manager Anthorixed by J. R. Carothara, 5A0/d0 Chemical Director TRAN 0U881 WATER PCB-SD0000001043 loaiisiafe Cbaaieal Courpaay Anniston, Alabama Aneiar Test Mothods and Dasips&tiosg 3peelfio Qrsrltf of Axoolor* Total Chlorln la Aroclors 3cft#nlas Foist at Solid Aroolors DetermlMtiOB of Iron 1 Aroeler Fla ah and FIaw Foists Viscosity of* Liquid Areolar* Distillation Raaf?# of Arooiors TTraporat lots Tact of Liquid Aroalors RafreetiY* Xdx of Liquid Aroolcra Raaiatirity of Liquid Aroolor Dleleotrio Caaartent of Liquid Aloclort Acid Nusbsr of Liquid Aroelor Color of Aroalor - SPA Soal Color of Aroalor - AHiA soal Aoid Kuaber of Solid Aroolor* Pour Polat of Liquid Aroolor laorgaaio Chlorlda la Aroelors TJatar Oonfcaot of Liquid Aroclors 14-10-48 14-15-48 14--17--48 14-21-48 14-84-48 14-2^-48 14-51-48 14-32-48 14-84-48 14-35-48 14-36-48 14-42-48 14-43-48 14-44-48 ,14-46-48 14-47-4 14-48-48 14-6S-43 COMPANY CONFIDENTIAL TRAM 011882 WATER PCB-SD0000001044 Monsanto Charaioal Company Anniston Method No. 14-10-4 Opeolfio Gravity of Am el or a The temperature at wMeh the gravities of liquid Anoolors ere taken varies with the vlsaoeity of the liquid. Note the temperature it which the gravity la to be taken for the Aroolor under teet and heat the sample to 10C. above thet tempera tiffs, Pour the hot sample into the steam or hot water jacketed hydronater Jar provided for this test. Stir veil with an accurate thermometer and adjust the temperature to the desired point by controlling the steam or hot veter feed to the Jacket. Continue stirring until the temperature remains constant for half a minute. Alice the hydroaster to sink into the liquid, then reed the hydraaeter scale at the point of the lower meniscus and record with the teaperature. Report the speolfic gravity to the nearest 0.001 unit. WATER PCB-SD0000001045 t Manaiito Cherries!. Company Anniston Method No. IV-13--48 3JBJSCT: Total Chlorlns In Aroelors U:iHOD: Volhard Titration following Peroxide fusion Chlorine In Aroolors may be dstsmined by fusion of the sample 7?ith sodium peroxide in s Burgeae-Parr fusion eup, extracting the fusion nlth r*eter, aeidifyinc the water extract with nitric acid, and nreeipibating the ohlorlne by addition of an exoess of sHrnr nitrate. After filtration, the excess of silver nitrate la determined by ti tration against potasalun thiocyanate, using ferrlo ammonium sulfate as indicator. Apparatus Ifca fusion cup used is the 3ur<?es*-Perr Sulfur Bomb No. 3 for flame ignition. A lead gasket is used. For Ignition, the bomb is sus pended through e 1-&/16" round hole in a 1/0" tranaite Dlste, This allows the fuelon eup to extend through the date for about 5/8 inoh. Ignition le effected by strongly heating the bottom of the fusion oup with the full flame of a Keker burner for two minutes. The bomb, gsoalcete, and tbo sodium peroxide ere obtained from the Parr Instrument Company, LJollne, Illinois. Charge for Fusion The fusion mixture is made up of about 19 rxsaa (one natal oeoop) of sodium peroxide sod 0-3 grans of finely powdered aena. auger. The reagents should be free from chlorine, or a blank run and corrected accordingly. He fusion mixture is mall mixed by plaaing the ingre dients in a snail glass stoppered bottle and shaking Timorously. A measuring, spoon for the sugar la convenient. 'JOLID AH0CL0R3t The non-cry eta Ulna type are neirfced in the form of smll pellets. Tfease are preiered by heating the <iroelor until e con sistency is reeohed as will permit dropping it from e glass stirring rod onto a tinned surfacs (a can top), aaoh drop forming a pellet. ,/heo tool these pellets can be removed from the surface by inserting a spatula under the. *4 grams are used. The pellets are brushed into the bottot of tbs fusion cun sad the fusion mixture plaoed on top of them. After titfiteolnc the lid, the charge is reedy for fusion. The crystalline type Aroolors ere welched In the powJared form, i4 grams being used. They are charged in the same Banner ee the honcryetalllne type. COMPANY CONFIDENTIAL TRAN 01138^ WATER PCB-SD0000001046 Total Chlorine la Aroelors 3 Caleulotloa of Chlorine Content , Dub tract tbs volume of KETTS required from the to luma of KCTJ3 required to tltrata the amount of standard AgRO, solution used. Thle will g^v^ the volume of KER3 equlYalent to the chlorine In the sample, Multiply the voluvw so obtained by the chlorine value of each ml. of KCRS and divide by the weight of sample taken. For example? If 50 ml. of silver nitrate solution is equivalent to 61,4 ml. of KCN3 solution and the value of 1 ml. of KENS solution t* .003 770 pram Cl; then if it is found that 0.3 <~r*ra of sample shows a ECNl titration of 10.4 ml. tha percent of ohlcrine is: (61.4 - 10.4) I .003770 X 100 . ^,09% C1 3 In oase the fusion mixture or other reagents oontaln ohlorine, the amount mat be determined and deducted fren the ahlorlne found. 3olotions Required standard AgNOf Solution: Dissolve ZZ nrans of silver nitrate In each liter of mter. Protect the solution from light. standard ICN3 Solution! Dlasolvs 10 'rams of ICN1 in 1 liter of -vater. Ferric Iron Indicator! Use a saturoted solution of ferric amnoniua alum, about 50 g. per 100 ml. of water. Pure Nitric Acid: Stock acid suffioes provided it is colorless. It can be boiled ln.a beaker until color less if neeeasarr using 600 ml. HN03 and 300 ml. of ne. Standardization of Jolutlons ;elgh 0.3 and 0.13 rrtus portions of pure dry KaCl into seperets 600 ml. beakers. Add 200 ml. of distilled mater to each and 10 ml. of pure 50> nltrlo meld. '.Then solution is complete, add 30 ml. of standard A&fOg eolation fre* pipat. Stir veil and filter through an asbestos mat on a perforated porcelain plate, using suction. Wash filter and transfer the flltrsts back to ths beaker in the same manner as when working with e earn-la. Titrate the filtrate# with standard ICR3 aolutloc, usim ferric Iron, Indicator. Tha vmlua of 50 ml. of AgSD^ eolation in terms ct ICRS solution is found by subtracting tha ml. of ICRS aolution in titrating tha 0.3 gram of HaCl frees twice tha number of ml. of ICT3 eolation used in titrating tha O.lfi gram of HmOl. comply WATER PCB-SD0000001048 Total Chi or in* ia Aroclars -4- Thta valus la eheclcsd by titrating 30 *1. of A^0S solution addsd to 400 ad. of water ajid 10 ml. of pure 50> W09 with KOns solution. This titration should agree rary cloaaly (1 0.1 i*l.) with the Talus found from the titration of NaCl. The titration must be made slowly to arold drainage error. 3Lnoe pore NaCl contains 60.662 Cl by theory, the value of the XClfS In terms of ohlorlne may be found by dividing the weight of ohlorlne In the fJsCl taken by the ml. of KEK3 equivalent to the silver nltrete required. Sxajaplt Two 0.3 gram portions of NeCl ehcrw KEN3 titrations of 13.11 and 13.13 ml. ' . Two 0.15 gram portion* of RaCl show SONS titration* of 57.28 and 37.24 ml. The JCDN3 equivalent to 50 ml. of AgNOj 1* then (37.28 37.24) 13.12 or 61.4 ml. By titration of 50 ml. of AgN0# against KCWT eolutlon. It la found thnt 61.36 ml. are required. Thla agrees within .04 ml. of the velue obtained from the NeGl titrations. The ohlorlne value of the KCNS la then, .6066 X .3 divided by 61.4 13.12 or .003770 grew* Cl per ml. of KCN3. The ohlorlne velue may also be calculated from the tltration'of 0.15 gram of NeCl. 0.6066 X .15 divided by 61.4 - 37.26 rives .003770 gnm 01, pwr ml. of KEN3. Precaution* 1. The fusion materials have explosive properties If handled improperly; consequently ear* mat be taken to use safe proportions, to seenre a good mixture free of large lumps, and to croperly neat the cover of the fusion eup. The fusion mixture anot be kept away from -star or moist sir, either of w) ieh vwy ignite the charge. The fusion mixture should not be ground to reduoe lump*. 2. The method a* described Is not applicable to volet lie organic easepounds anises precautions are taken to avoid lose of sempls during weighing. Iffact of Tarloblee . 1. On account of the high chlorine content of may of the Aroelara end the mall mount of sample taken, great accuracy la required In weighing, transfer, end mixing of the sample. The plpet end buret for mmmri&r th standard solutions wart be very dean to avoid drainage errors. COMPANY TRAN 011887 CONFIDENTIAL WATER PCB-SD0000001049 Total Chlorine is Aroolore 3 2, fusions whlob show black carbon denositaa on the corer and aide of tho fuaioa eup may or may not "ire the full ohlorine content. If a oarbon deposit Is found, a second fusion should be made usinp a mailer sample or reducing the amount of super in the choree or both. . 3, The temperature at whioh the atenderd solutions are standardized should be K>ted. In case rooa temperature* tary from this ta.ivperetura, appropriate roluae corrections ehould be made. 4, The fusion mixture materials should be essentially free of ohlorine. T e ohlorine content may be determined by natcinr e bleak fusion, that le, without addition of sample, end titretlap in the usual may. yit* el. of AgNO# may be added instead of 50 ml. portions of A^03 solution in like rolumes of solution and nitrlo acid. Heferenoee Beamirti: Determination of Organic Ha lore a, Ind. Enp. Chera., Anal. Ed., _6 332 (1934). r.'iB; ea 1-29-43 Copied by ra 4/20/48 COMPANY TRAN 011888 WATER PCB-SD0000001050 Uoamste Chauiasi Company Anniston Method Ho, 14-17-40 mTSST; METHODl -ioftanlnp Point of Tolld Aroolora Ball and Rln^ This method la a modification of the A.I.T.?:. standard method of teat far softening point of biturelnoue materials, eerie? designation: E 2S-397, Th method differs from the standard method In that the rlnca are larger than specified. A two ring support Is also uoed in order that two tests nay be made simultaneously. Apparatus The apparatus oonsists of ths following: () Two tapered brssa rlrvs, 3/0" inside die. at bottom, 11/16" inside diameter at top and 1/4" deep: thickness of mil 3/32". (b) Two steel balls, 3/8" diameter .'eight:**, 3,45 to 3.35 prane soh. (e) A 800 ral. Qriffln lor: form Tesker. (d) A rinc support for ths two rings ha Tine braes elate exactly me inch be low ths plate supporting the ring, (e) A 300*C. A.3.T.K. low distilla tion thermometer graduated 1*C. Preparation of tha Staple The sample shall be melted and stirred thoroughly, avoldlnc overheating or incorporating air bubbles in ths mass and than ooured into the ring so as to leave a slight excess on cooling, 3lnce the Arod or s shrink oonsiderably on cooling, the rlnr should be 'tell filled, nearly to over flowing. A little of the excess should b drawn over the top of the ring at several points so as to prevent tha oooled Aroclcr rroa dropping out of ths ring. In the same my, tha second ring. Is filled with a standard Arcelor of known softening point, Tha standard Aroelor should have a softening within at least 10 to 15*of tha Aroelor'being tested. The rings while being filled should rest on a clean een lid or on a brass plate whioh has been aralgansted to prevent the Aro&ar from ad hering to it. The Aroelor In the rinse should be fully oooled and hardened before preceding with the test. Procedure s 1 Add wool eolation (essploy water for soften lag point between 0-90"C, glycerin for between 00-200*0., mineral oil for above 200*0.) to the beaker until the surface of the solution ie 2" above the plate holding the rings when tha ring support is suspended In the beaker. Place the rins containing the Aroolcr to be tested end th standard Aroelor on the ring support. Fine a ball cm. the center of the upper surface of the Aroelor in each ring. On spend the thermometer so that the bottoa of the bulb 1 level with the bottom of the rises and Just aidwoy be tween the two rings. COMPANY CONFIDENTIAL TRi* n. WATER PCB-SD0000001051 Softening Point of lolid Aroelcr# - 2 - Plaoe beakef and apparatus on 6 Inch round hot nlute and heat ut such a rate that the temperature la nleed 5C. each minute. The temperature recorded by the thermometer at the 1 no tent the Aroolcs* touohee the bottom plate lo reported ea the softening point. The heat ing la continued until both /croc lor a hate dropped to the bottom -lata, lfo corrections are made for emergent stem. Hot os 1. The standard Aroclor le run along with the sample under test In order to compensate for "variations In rate of heating, dilution of glyoerln, nod thermometer variations. . The softening point of the etaodard sample is determined by making several determlnatIons using fresh elyoerln and oarefully checking the rise In temperature of the glycerin eo that It le aa near aa possible to 5*C. per minute. 3. The glycerin nay be ueed repeatedly for the testa after rmdoval of the Aroolor. 4. Benzol la used for cleaning the rings and balls. 6. ater ean be used instead of glycerin for softening points up to 90*C. 6. For softening points above 100*C, -ell boiled glycerin should be used. The usual glycerin le not satisfactory above 125 to 130*C, ' it bolls with lose of meter while the tereoerature remains practi cally constant. It la well to hare a supoly of hlgh-bo 11 lag glyoerln on hand to ba used only for eofteeing points above 100*C. 7. Air bubbles oa tbs rings and balls during the test should be avoided aa far as possible. 8. The rate of rlaa of temperatiye of the glycerin ehall be uniform for eech minute after the first 3 minutes of heat lag and not averaged over the period of the teat. FABtea 1-51-4,8 Copied by rs 4/20/48 TRAN 011890 WATER PCB-SD0000001052 Monsanto chanlcel Company Anniston Uethod No. 14-21-45 3DBJTSCTi De tend nation of Irua In Aroolora Iron Ln Aroolora may be determined by ertreetinc a banzai solution of the Aroelor with dilute hydroohlorlo acid until further extractions hew do appriselable Iron content. Tha Iron in the combined extracts is then-determined by dlehraaate titration. Procedure Transfer 3-10 grans of saaole to a dean separatory funnel of about 150 ml. oapeaity. Add about 30 ml. of baazol and shake until the sample is ln solution. TThen solution is oomplete, add 10 ml. of 1:1 iron-free 331 and shake for about 2 mlnutee. Let stand until se parat Ion of the two layers is complete, then drew off and preserve the ecld extract. Add another 10 ml. of 1:1 3C1 end shake again. Draw off tha ecid layer end combine with the firet artraot. Continue until HC1 layer la clear. Determine the iron by neual dlohronate titration method. FAB tom 1-31-48 Copied by re 4/21/443 TRAN 011891 WATER PCB-SD0000001053 Monsanto Chonioal Coap&ny Anniston Method Uo, 14-24-48 OtJBJECT: Flesh and Flame Points .'JhTIIDDi CleTeland Open Cup The fluah and flame polnta of Aroolor shall b determined In the . Cleveland Open Cup Tester, following the procedure described in A5T5J' v D 92-33. Apparatus The oup shall be supported by a aatal plate 1/4" {.633 cm) in thlok- ness and 6 inches (13.24 cm) in width. The plate shall be of braes, oast iron, wrought iron, or steel. In the center or the olate there shall be plane depression 1/88" (.07V on) in depth, end of Just sufficient diameter to fit oup. Thera shall be a circular opening 2 3/16" (3.30 cm) in dlametor, out thru the plate, o enter Uv with the oenter of the shore mentioned depression. The plate shall be covered with a sheet of hard asbestos board 1/4" in thickness, and of the same shape as the aetal plate. There shall be cut in the center of the as bestos board a circular hole just fitting the cup. Heat mey be supplied from any convenient source. The use of a rae burner, alaetrle heater, or alcohol lasp la permitted, but under no oiroumsteneee are products of oom- buetioh or free flame allowed to oorae up around the eup. The source of heat shall be centered under the opening in the plate and shall be of a type that will not produce looal superheating. If a flame heater is used, it may be protected from drafts or ezoessive radiation by any suitable type of shield, that does not project above the level of the upper surface of the asbestos board. The thermometer shall conform to the requIrenaats of thermometer Ho. 8. (Tee A3TM table of thermometers). . Procedure The thermometer shall be suspended or held in a vertical boit ion by any suitable device, the bottom of the bulb shell be l/4 1*. (.635 cm) from the bottom of the eup, and above a point half uay between the center and book of the eup. The eup shall be filled with oil to be tested in such a ranner that the top of the meniscus is exactly et the filling line at root temperature. The surface of the oil shall be free from babbles. There shall be no oil above tbs fiUlnr. line or outside of apparatus. The test flame shall be approxinsitely S/S" (.897 cm) In diameter. The test flame shall be applied as the temperature read cm the thermo meter reach Meh successive 5*f mark. The flame shall peas in a straight line, (or os the oLreuaference of a olrcle having e radius of at least 6 inches.) across the oamter of the eup and at right angles to the diameter pasting thru the thermometer. The test flam Shall, while pessing across tbs surface of the oil, be in the plan of the upper edge of the eup. Tbs time for the passage of the teat flam across the cub shall b apre-oxl- mtely 1 second. COMPANY CONFIDENTIAL TRAN 01 18 9 2 WATER PCB-SD0000001054 Flash and Fimas Polite Z- Th oil shall be h a ted at a rat* not exeeedinr SO*'!1' oar minute terar>era tur rise till a point ia reached approximately 100*F below the probable flash point of the oil. Thereafter the rate of heat lor shall be decreased and for at least the last 50F before the flash point is reached the rote shall be not less than 9T. or more than 11*F per minute. < The flash point shall be taken us the temperature reed on the thermo meter when a flash appears at any point on the surface of the oil. The true flaah roost not bs confused with s bluish halo which sometimes surrounds the test fleas. After detenalnlnc the flash point, the heating shall be continued at the specified rat of 9*F to UF per alnote, and application of the teat flan aha] 1 b# made at the specified intervale until the oil iipaltes arid con tinues to burn for a period of at least five seconds. The method of application of the flame shall be the sans as for flash point. The tem perature reed at the time of the flame application, which causes burning for a period of fiva seconds or more, shall be raoorded as the flute point. The flash point and flams point tests shall be made ia a room or com portment free from air drafts. The operator shall avoid breathing over the surface of the oil. It is desirable that the room or compart ment nay be darkened sufficiently so that the flash nay be readily dis cernible. . Note Aroolors 1X48, 1X54, 1260, and hi-her chlorinated Aroclors do not have a diatinot flash or flame point below their boiling temperatures. Copied by rs 4/21/48 COMPANY TRAN 011893 WATER PCB-SD0000001055 Monsanto Chsmloal Coapajjy AnalatOB Mat hod No. 14-29-48 'STBJlXTi Ylaooalty of Liquid Ax emigre ITETgpD: Saybolt Universal, A3TM D 88-44 Ylacoaity la a measure of resistance to flow. It Is measured by tha tint necessary for s ohoaen volume to be foroad thru tub# of chooen leacth and internal diameter, By theory the viscosity of fluid la related to th# average dlatano# beV.teen its moleoulee and to their averse apood and their size. Apparotue Viscosimeter assembly with oil tube, beth, raoeiver, thermometer*, rtralaer, timer, and pipet to meet all requirement# of ASTBJ D 88-38. The viscosimeter now in uaa It made by Krebs lies, and LXg. Co., New York, purchased froa Kail Qreiner Co., their 2-tube capacity 862, One tube - on left hand - ha# been certified by the Bureau of Ttanderd*. Procedure The vlsooslmater la set up in aeeordanoe with manufacturers direction# using No. 20 motor oil for tha bath. The procedure and method of reporting results are those described under A3TM D 86-44. Care of Apparatus Both; At conclusion of test, open the contact points until 1 or TnoEea apart so as not to put undue strain m t ha mo e tat lo control when bath cools. Put a few drops of oil in motor cups occasionally. Keep outside of beth wiped free of oil or Aroolar. Cower with hood when not in use. Usintsln proper lewel of oil by oooaelonal additions thru hole In front. 'Then oil blackens, dimantle, clean heaters, tubas, sad r if lose, then refill with fresh oil. Oil Tube: While still hot, ranowe all possible Aroclor froa gallery with pipet. Than cooled to 70-80*, fill tube end gallery with beassne, drop thru orifice into besker, drain -wllery with plpet, repeat with acetone, end wipe dry with absorbent paper la such a - ay that fibers cannot fall into toab, Repeat until clean. Occasionally cower the leather plunger with sired thin paper (eopyB COiVirANY confidential TRAN 0UB9<t WATER PCB-SD0000001056 Visooel ty of Liquid Aroclcrs - 2 - I sheets) and rwb vail* of tuba before uainf' cleaning fluid. Thi* keeps mil* polished. Carer oil tubes with lid* when not In use. Or If loe t orifice. foroeps. clean. Do not pass wires, stria,is, pipe cleanerB, etc. thru the If hair falls across orifice, renore nitb lon handle If the orifioe beoortes dogged, dismantle sppcrotus to Calibration Check tha timer occasionally for 60 second oeriode. Check bath ther mometer from time to time. Check performance of Tlscoaimeter oerlodlcally by running a reference sample of Aroelor on whioh careful deter minations hare been amde. Available for oolibration is also an oil standard, celled "Aloha 48", of the Amerloan Petroleum Institute. The oil is obtained from the Atlantic Refining Company, Philadelphia, Penneylvania. Because suoh oil standards ere eubjeot to o bangs they are aheoked annually. TAB:! 1-51-43 Copied by rs v 4/21/48 COMPANY CONFIDENTIAL TRAN 011895 WATER PCB-SD0000001057 KcfQMjafeo Chemical Coispany Anniston Method No. 14-31-45 tXTBJ?PTi Distillation ftanr# of Liquid Aroclore METHOD t A.D.T.U. D-20 with Uodlflet 11 on a Tha apparatus, oonalatlac of flask, condenser tab, shield, and ther mometer, la exactly the same as described under A.9.TJ1. tart D-20 "Distillation of Bituminous Material suitable for Hoed rreatment". Attaah a 6 lnoh auxiliary thermometer (0 - 130*C.) to distillation thermometer, Ploee bulb holf -say between top of oork end orobable ftTernce of dietillation range. Cover both thermometers with e 3/4" diameter r.iaae tube to Insure a uniform temperature correction for the exposed stem, berometrlo pressure and thermometer error. The procedure le chenged only to the extent that thermometer readings are taken when specified percentages (usually ID, SO, and 905-'-) of Aroolor have been distilled Instead of following the A.T.TJLI. proce dure of weighing tha distillate between specified thermometer readings. In testing liquid Aroolora, 100 rpxa. of sample are weighed into the distilling flask and distillate received in a tered flask or beaker resting on pen of a Torsion belanoe with 100 pram scale. Procedure 7eigh out 100 grams of sample Into the distilling flask. Aaeeeble apparatus as deaorlbed under A.3.T.M. D--20. Insert thermometer (A.3.T.U. high distilling 0 - 400*0.) thru occrk in the neck of the flask so that the top of the bulb la level with the loweat point of juncture of the tabu la tore and neok of the flask. Anply best to the flask supported on two sheets of 20 nesh wire amuse so that the first drop comas over in from 8 to 13 minutes. . Cpnduct dlstlllatloB at rate of 80 to 70 drops pea* start. Collect diefcillats in a 280 ml. beaker tared on a balance. Take temperature 9%, 99%, 99%, 97%, and dry. Corrections for energaat stem and pressure are applied to the thermo meter readings if required. Take correction reading* at first drop, 10, 80, 90)1, and dry. Report the temperatures to the nearest 1*C. '"xsavplei (Exposed stem in decrees) X (temperature difference in degrees) X 0.000158 degrees stem correct ion T^. The exposed stem is reed from the top of the cork. 'The temperature difference is the reeding of the thexsaometer minus the t@apereture of the auxiliary therucseter. TRAN 011896 WATER PCB-SD0000001058 Distillation Haaff of Li($ai<l Aroclor* - 8 O.OOOLB ^ k e baroeatric oorrootlon Tf T* aomal boilina point la degreea abaolate; A p ahaar.e la treasure from ?SO an. H4. The correction Is added If barometer la below normal end subtracted If the baroaetar is above normal. (Line Dour. 11 - "Thermodynamics tad Chemistry pp, US). Corrected Temperature Observed temperature Tl i Tb. ' TABtea 1-89-4S Copied by rw 4/28/48 ccr^pM.Ni y CONFIDENTIAL TRAN 011897 WATER PCB-SD0000001059 Monsanto Chealoal Scraps ay Anniston Method No. 14-32-48 CUBJTCT; Evaporation Teat of Liquid Aroolara maOD: 6 Hours Heating ot 100C AST: 06-39T - Modified Procedure './elgh oa a rough balanoe about 30 roma { .5 pa.) of the wall mixed Aroolor Into aa accurately tared tin box, 35 cm. die. X 33 on. de@p (3 ox. QlU-style ointment box, deep pattern), Fleher fl-620. Let stand until box and sample are -t roon temperature, then welgh accu rately. Place the box in a ventilated oonTectlon oven maintained at 100*0. 1 1* for 6 hours. Remove, cool in deslooator to rooa temperature end accurately reweigh, From the lose In Wight calculate the evaporation In per cent. Report to aeoond decimal place only, Notes 1. Be sure box is st room temperature whenever exact weight ia taken. . 2. The oven aboulfl not contain other Mmole e which mi^ht Interfere with evaporation. * 3. Beeauas the evaporation lose Is sensitive to temperature, the eir bath must be closely maintained at 100*C. FAB:oa 1-29-4C Copied by ra 4/23/48 CO,VlP/tl\fY CONFIDENTIAL TRAN 011898 WATER PCB-SD0000001060 Monsanto Cheaieel Company Aanlatan Method No. 14-34=48 . ggBJKT: RefreotlTe Index of Liquid Aroolare METHOD: Abbe Refreotoraeter___________ _________ Refractlre Index The refractive index of any median la defined aa the ratio of tha Te locity of light la aLr to tha velocity of light la that ndlua, It la meaaured by th rotio of the alna of tha incident eacl bo tha alne of the angle of refraotion. The deaaar tha nadiua, tha -Teeter 1* ttm refraction toward the normal (higher refractlTa index) . Beoause the rafraotlTe ladaz la oharaoterlatle of aeoh aubetance, It la useful in Identifying lipids end verifying their purity, In determining the bolaoular structure of organic compound a, end In some quantltat It analyaaa of aixturea. Aa applied to Aroolor testing rafraotlTe Index prorldea a verification of oompoaltion and purity. Apparatus Abba Refraotometer with aooessorlea, Baueoh and Lomb, Cat. f350, Serial No. 377. Calibrated to read directly in terms of refreotlve index of tha D line (eodlua) at a temperature of 20*C. Prooadura Operators ahould be fasiliar with tha Bauaoh and Lamb "Direction tar Use" and practice tha manipulation aa there deecrlbed before attempting determination* on Aroolor. Tha abridged directions below pro-ride a working outline but at the expense of omission of essential explanatory details which are contained In the B. end L. directions. Screw thermometer into Its socket in rmter Jacket of upper prim. Open prime end cheek their condition. Clean If they are soiled, streaked, or spotted. 91th lower fixed prim horizontal, place on it 2 or 3 drops of the Aroolor from a stirring rod - sufficient to fill the speoes be tween prises whan clasped together. Close prleas and look with look nut. Adjust tha instrument and mirror to reflect white light Into the re fra o- tosatar. No spots on air pocket's ahould he visible. Connect water Jacket to aouroa of constant temperature -rater, usually tha tap, and pasa water until the thermometer ha# been constant to OJI*C. for at least 3 slnutss at 28"C. Tha Aroclars flow more easily at 2S*C., henoe the choice of this temperature. - fith primes illuminated, rotate tha prisma by weans of the Index ante until the border of tha light and dark fields passes exactly thru tbe intersection of th cross balra. If the border line is fringed with color, rotate th# compensator until the color disappears. If th* boun-- COMr- 'ANY CONFIDENT/AL TRAN 011899 WATER PCB-SD0000001061 Refraetivg Index of Liquid Aroelor 2 dary is not stepp, adjust mirror until a distinct half ahado-? Is ob tained . If tii 11s op tha cross hairs are blur red, adjust eyepiece uaiil a eood focus is obtained, Secure final fins ad Justment by -isens of the slow motion sores. Head ths refract Its Lndex, estlrmtinc to the fourth decimal ->laoe. If the tsrapereturs of the water Jacket ie other than 25*C., correct to 25* by use of the,correction feotor, 0.00044 per *C. This factor Is applicable only to Aroelora 1248, 1254, L260, and 1262. It me found by careful asasureraect on each Aroclcr thru the ran me 10* to 50*C. The correction Is subtracted when the working temperature la below 25C. and added when above 25*0. ' Example: If U e refractive Index Is found to be 1.6422 at 15*0., the index corrected to 25*C. le 1.6422 - (10 I .OOOU) - 1,6578. Care and Calibration of Instrument Immediately 'after use, clean tbs prisma with swabs of pure cotton dipped In benzol, finally wiping dry with a soft doth. The Trlsms, especially tha upper one, tarnish and scratch easily. Consequently great care must be taken in cleaning. Before use the orlsma should always be Inspected and recleaned if necessary. 'Then not In use, the refreetonetar should he kept in its closed oass. For practice or for cheeking erfarmanoe, distilled water 1 o useful. Jeter has a refractive Index of 1.3330 at 20*C., with temperature eoeffieient of 0.0001. A test niece of speolel rlese of known refractive index ie supplied with the instrument for calibration and adjustment If neoesssry of the position of the Index era. Refractive Index of Aroclors - Typical ' Careful moaeurernants at 25C. have given ths following typical values for Axoclora. Aroelor 1848 Aroclor 1854 Aroelor 1860 Aroelor 1868 1.6295 1.6376 1.6460 1.6468 Substantial departures (over 0.0010) from these values should be in vestigated Lamediately as they - ^f.correct - indicate substantial error in the composition of the Aroelor or eostaaination with ether Materials. FAS:as 1-87-49 Copied by re 4/25/4 COMPM/y CONFIDENTIAL TRAN OIL 900 WATER PCB-SD0000001062 Eoamat Chemical Company Ajsnintoa Uethod No. 14-35-48 TJBPDCT; Resistivity of Liquid Aroalors METHOD; Resistance '-lea aura-meat 3 between Conductora Apparatus !Jogohr* Brldg: General Radio Company Type 544B, AC operated - 300 volt e, oorial No. 171, Th la Is a direct-current '/heetst one bride for measuring high resistances, bridge balance,belnr obtload thru use of a vacuum tube voltmeter. Range; 0.1 megohm to 10,000 megohms, (Covered by a dial aaJ 5-poeltiou multiplier switch. A reelstanee of 1,000,000 tie goha a can be detected. Test Eleotrodeas Two concentric nickel cylinders (or braes, nicks! plated) with feet. Obtained from General Electric Coapany. The Inner eleotrode has outside diameter of 2.8" and height of 3.25", with area of 184 sq. cm. The outer electrode hoe Inside diameter of 3" and like height of 3.25", with area of 198 eq. cm. The distance between electrodes is therefore 0.1 Inch or 0.254 ca. By theory the electrode constant, area/ length, is 191/0.254 or 752 where 191 la the average area. In proetlee the oell aonstant supplied by General Electric Coapany la ueed. For the electrode a now In use, the oell constant wee given as 815. Oleas Plates Pyrex, about 3-1/2" diameter with oonesntrio groove# to eesiat In a peeing the electrodes. Obtained from General Electric Company, Oven: Ceneo-DeKhotensky drying ovan with two holes In back wall for por celain tubes for lead wires. Holes must avoid oven heating elements which occupy 2" paths vertically and horizontally Intersecting at the center of the circular wall. < Lead '.'Ires: Provide 500 ohm Amphenol twin conductor cable to connect the electrodes In oven to the poets of the bridge. The rortioos emooed to oven temperature ere bared and then ooversd with naroeleln beads. Provide also a flexible lead to ground the bridge to e 'water pipe. Clean the leads, beads, end porcelain tubes oerlodloally. Aeeeably of Test Cell groovedThe glass piste ie placed In an 800 oe. beaker. The clean elec trodes are placed In the grooves of the glees olats with the connector poets directly opposite in order to give the widest possible seeing to reduce surface oon&totivlty. The cylinders should be very clone to equidistant. The apparatus should be dried for 2 hours at 100G. befor UBS . . Heat th sample to be tested to about 110*C. on a hot plat end oour . into the slsetrode assembly until the level of the liquid ie 1/4 to 1/2D above the electrode. Cere rust be used to sake ear that the COMP A\iy TRAN 011901 WATER PCB-SD0000001063 gJBJ~5ST: Resistivity of Liquid drooler a - Page 2, IffTHOD: Resistance Measurements between Conductors lip of the container, froni which the liquid la poured, la clean. Tilt the beaker In suoh manner that all air bubbles in the Aroolor will rise to the eurfaoe. Air oool to 103-104*C, ?)n without removing thermometer, transfer to the oven which la maintained at 100*C. and oonneot the eleotrodee to the two flexible \rires whloh lead to the megohm bridge, Then the Areclor oomes to temperature (100*C.), remora thernooeter, check cen tering of eleotrodes, ond precede to measurements. Measurement with Megohm Bridge ^` , Connect the two lead wires to the megohm bridge with the lead from the outer electrode to the LCT7 unknerm post of the bridge; the inner elec trode to the utnknorm post. Connect the 'TRWND post on the left aide to a water pipe. Swing the spring conneotor, piroted on the "0" post, to the LO / Dost. Connect the attachment oord to the 110 7 po.;er *ippiy /1th the Aroolor et 10C*C., turn the oontrol knob (CTTECIC-^Pon. .TE-C.'I'J^GE) to the CHECK position. Thre-i all 3 ewitotaea at the rear of the Panel to ON, Alter Z minutes bring the galvanometer pointer to zero by mean of the ZERO ADJU3T knob. Then turn the oontrel knob to CIl'tRGE for one minute. Turn the. mob tc OPERATE and return the galvanometer pointer to zero by adjustment of the LUU'IPLT BT snitch and the megohm dial. Read after one minute. Re pent the CHARGE and OPERATE positions for verification. The reeietlTlty of the Aroclor is the produot of the "multiply by" reading tinea the dial reading times the eleotrode constant. Report In units of 10 ohn am, rounded off to tiro significant figures. Example: "Multiply by" reeding: . Megohm dial reading Eleotrode Constant 100 5.4 mag. ohms 815 cm Resistivity Values for reslstlrlty are qualified by designation of temperature and voltage. These are 100"C. and 500 volts for the teat above. Like con ditions are used at Plant B. . COMPANY WATER PCB-SD0000001064 3JBJS2T: Resistivity of Liquid Aroolors - Pane 3 MTTHUD; Resistonoe .eaBiirsment a betv/een Conductors Caro of Apparatus The "Opera ting Instructions", General Radio Form 45S-B, Meh ecoompany the megohm bridge, recite detolle of installation, asasuramenta, uasa, and construction, illustrated by figures and circuit and 'Tirin'? dia^rramaNo attempt la made to reproduce such information here. The operator should acquaint himself with the contents of the O.R. manual and refer to it for maintenance of tubes and perts. ,Tien not in use the megohm bridge should be closed and stored in oablnet. Cleaning Electrodea - After the measurements are made the eleotrodes are remowed from the . tested liquid, and allo-ed to drain until the liquid stops running from the electrodes. .Thlle still hot they are placed In a baaker filled vrith benzene under a well wen 11a ted hood and allO'wsd to cool. -1160 cool, the eleotrodes ore removed from the bon2eoe and scrubbed with porwiered tri sodium phosphate end a benzene carbontetraohloride mixture (50-50 by volume). This acrubblnR can be done rrith either a bruah or the hands. The eleotrodea are then rinsed with acetone, followed by tap -wter and then distilled "/stir. Th# aleotro.lea should not be touched by the hands after the aoetone vre ah. After final rinsing the electrode are placed in on oven ot 120*0. for one hour or until they are used again. The gin as spacer plates are oleaned and handled in the sans manner as the eleotrodes except that they axe wrapped in lense paper before being plaoed in the oven. Calibration For a rough check on the condition of the bridge, one or more cartridgetype resistances of known approximate value should be kept on hand for periodic or emergency verification of the meter Itself. re 8/3/4S COMPANY CONFIDENTIAL TRtN 011503 WATER PCB-SD0000001065 Monsanto Chemical Company Ann If to a Method No. 14-36-48 ^BJTCT: Dlcleotr lo Constant of Llould Aroolor MrraCD: Measured at 1QQ*C. end LOOP oyoles 3cope This method applies to Mineral oils and oil substitute used for ineulotinp. purposes. Apparatus Cepeoitanoe Bridge Oathode Roy Nall Detector Oscillator Constant Tenpcraturs Oven Variable Air Condenser 1300 co. Pyrei Beater Genera 1 Radio Co., Type 716-AX General Radio Co., Type 707-A General Radio Co., Type 606-A Cenoo-DeKhotinsky #93000 General Radio Co., Type 334-T Procedure Electrode and beaker must be cleaned as directed under "Cleaning Appa ratus for Dielectric Constant", and be at 100*0. Heat A_rodor in the can to 105 "C. Pour over electrode until ole tea and oerania insulation are covered. Connect leads. 3tlr with thermometer outside oven until teapsTature reaches 101*; place In oven which has been oarefully adjusted to 100*0, At the time sample is placed in erven it a temperature should not have fallen below 90*0. Connect leads to capacitance bridge, observing that the lead from insu lated side of oondeneer goes to insulated terminal on bridge. Balance bridge oarefully according to direetioa under "Balancing Capacitance Bridge", Until Aroclor and oven temperatures have beooms identical the bridge balance will constantly shift. After oven temperature reaches 100*C,, maintain bridge balance until no pronounced shift is evident. Record reading of capacitance scale multiplied by multiplier setting. Dielectric Constant. Capacitance in Aroclor st 100C. Capacitance in air at 100*C. Balancing Capacitance Brldg ^t S S9 o Condensed procedure. Operator should reed operating instruction for Nall Detector for complete details. 1. Connect to power supply leads to oscillator end null detector. Ground the oscillator. 2. Turn on oscillator by pushing 3000 ohm, 10 miltiplisr, 100 eycl# frequency buttons. Adjust harmonic ontrol until oscillation begins as shown by closing of sect In oathode ray tub. TRAN 011904 WATER PCB-SD0000001066 Pago #2 Dielectric Constant of Liouid drooler - Test 14-36-40 3. On null detector turn brilliance knob to extreme left, the fooua knob to extreme rlgiht, gain control to extreme left, ereeo amplitude at mid-scale position, tba sweep frequency switch on iLn# aide. 4. Turn on power rwltoh, lighting pilot light, 5. 'halt fifteen seconds, turn brillianoe knob to extrema right. 6. Adjust foous and brilliance knobs until sharp fins line, 7. Connect external terminals on dataotor to output terminals cm oscillator, Switch sweep frequency to external side, 8. Connect detector terminals of bridge to imut terminals of detector, taking cars that the black wire (ground wire) of the lead goes to grounded terminal on both ende of lead. P. Set in control at ald-ecele and selectivity to extreme left. Turn sweep amplitude to extreme left, obtaining vertical line, "ilth 10. v/ith turning control knob obtain the maxlom lenrth of this line, keeping it always under 1/4 inch with ain knob. 11. Set sweep amplitude to ertrone left. 12. Set gain oontrol to rive vertical straight line of about 3/8 lnoh. 13. Balance bridge .by ad Justin" power factor and capacitance dials until only a dot ram in a on the screen vhen the gain oontrol is at extreme right. 14. Set sweep amplitude beyond ndd-polnt, and slightly displace the power-factor dial to obtain a tilted elipse. 15. Adjust phase control until this ellipse doses into a straight line inclined to the horizontal. 16. Bring power-factor dial beck to balance poeition, whioh should restore the horizontal straight line. Displace this control the same aaount in the opposite direction. This should again tilt the straight line but in the opposite direction. Adjust phase control until there la no tendency far. this line to open up when it la strung SO degrees from horizontal in both direct lone. 17. Throughout these adjustments the other bridge control (the company TRAN 011905 WATER PCB-SD0000001067 Pag* *3 Dielectric Constant of Liquid Aroclor - Teat l-*-36-48 capacitance Dial) tiuat b In balance poaltlon. If the ellipae rraiually opens whan the 1 in a la horizontal It my be brought back to the llna vra In by rsakltr alight changes in thia control. If oonfuaion remits, balance both controls again ns In (13) end re neat tb suc ceeding adjustments. This la tha position of bridge balance: An alteration of the power-factor control will tilt the line which does not open apprecia ble thru an angle of 30* to the horizontal both eya; an alteration of the oap&oltaooe dial opeoa the ell ipse but does not ohang# the inclination of the major axis. The apparatus nay be left In thia balanced condition, turned off by twitching off first the brill Ian oe knob of the detector, then the power ewltoh, then turning off the oac ilia tor. For auooeaelTe measurements the oontrola art not ohanged, the apparatus left in adjustment. Then the following steps define the procedure: . 1. Conneet all lends as previously directed lncludlnr that from mill detector to bridge. 2. Turn on oscillator by outhing 100 oycle frequency button. 3. Turn on null detector, wait 15 eeoonda then turn on cathode ray tuba. Turn sweep amplitude to oxtrems left end adjust brilliance to obtain a fins vertical line on screen. 4. Briar this line to a dot by adjustin'* the two bridge control*. Initial adjwtaent Is facilitated by having "Gain" control to laft. Whan final adjustment is obtained this knob oust be at extreme right. 5. This dot reneining unchanged shows condition of brld-s bslsnos. Cleaning Apparatus for Dielectric Constant The condenser is removed from the tested dleleotrio and allowed to drain while still in the oven at 100*C. The condenser is then placed, while still hot, in a beaker at benzans under a wall ventilated hood end allowed to ooel. It la then thoroughly washed with powdered trieodlua phosphate end e 50-50 mixture of benzene end carbon tetrachloride followed by an acetone rinse. The operator should ba very careful not to touoh the natal plntea of the oondenser .after this point. Tbe oondenoer is then rinsed thoroughly with tap water followed by distilled water end dried on a clean paper in an oven st 1B0*C for at least one hour or until It is again used. nab 3/1/48 TRAN 011906 WATER PCB-SD0000001068 ffoamnio Chemical Gompeaj Anniston L^sthod No. 14-42-48 'XTBJT.CTT: AoId Number of Liquid Aroolora IT.'TMJOD: Titration with Alkali using Fhenol Red 2222* Th Aoid Number la the weight la milligrams ef odium hydroxide re quired to neutralist one gram of . roc lor to pH 7,6, It thus includes any hydrochloric acid, ferric chloride, and other inorganic or organic oonatituente having teid characteristic#. It corresponds to the Neutrelizat ion Number of ATT!! Designation DIOS except that the letter is expressed la ttnu of KOH instead of KftOH and has a somewhat higher (phenolphthaleln) end point. Procedure To 100 ml. of adjusted (pH 7,6) solvent containing lad icetor slonly add 0,1 H NaOT dropwiss until th color corresponds eonroxisately to pH 7.6 when compared aceiast a suitable raferenoe solution. Readjust if necessary to maintain pH 7.6. Add SO grams (tig.) of Liquid . Aroolor and ail well. Titrate from micro buret with 0.01 If NaOH until the original red oolor of th* solvent is restored. A portion of solvent in a similar container is useful reference In determinin'- the end point. The match is governed by estimation of th* intensity of red because the hue is not exactly reproduced on eooount of the yellow oolor introduced by the Aroolor, 1 ml, of 0.01 H He CO 0,4 I!gn, HsQB. Calculate In t ems of Mm. NaOH per gsa. of sample.*" Report to 4 decimal nlaoee. 0,01 Ftjfad! 11.1 m g. of nple IteOII/&l, Jtxaapls: If titration is 0.08 ml. for SO g. of Aroolor, the Acid Humber it 0.08 1 0.4/fcO 0.00064 Ugi. NaOR/gs, Report as 0,0006, Solutions' Required Solventi Itix 600 *1, of benzol, 200 ml. of A alcohol and 200 ml. of ac#t>a# Add ml. of 0.2 phenol red solution. Fheaol B4 Oolutioa, 0JB; T 0.1 i. of toy indicator in a small bee tear add ussetly 2.0 ml, of 0.1409 NaOH. Itir to diflve and dilute with 5A alcohol to 50 ml. Reference Buffer pH 7$t Dissolve 0.41 g. and 0,69 pa, IfagltPQ,* (both ashytiroue) in WO ml* of wster. Add 0.5 ml. of 0.2,.' pbwaol red. lolutios is u**d for reference is edjustiap. th* solvent if Lel^tt pH 7.6 oolor standard is sot avellnhls. company c 0nf>dential TRAN 011407 WATER PCB-SD0000001069 Aeid Wumber of Liquid Aroolara - B - Standard 0.01 K NaCH: 6 ml, of .5 K NsOS to 250 ml. vol. of 5--A 1- eohol. Protoot at all times from atmospherie C0a, . Not a ' 97 usltLg 200 ml. aeetons La solrent Lnetoad of 200 ml. a 100 gm, eampla of 1254 ssaj bo taken for analysis. FABtffli 1-00-46 Copied by re 4/23/48, Cn,?r-MPANY C0NFiDENT/AL TRAN 011908 WATER PCB-SD0000001070 Uaaaanto Chanicsl Company Annlstcc Method So. H-43-48 3JBJXTi Color of Aroclor on N.P.A. teals L'LTTKL : Rallies Pootcet Comcorator 3oo pa The method is applicable to Aroclors 4445, 5460, or others baying N.P.A. colors in the range 1 to 5. Procedure "am the Aroclor is necessary to obtain pouring consistency. Till the test oup of the HsIIIrb Pocket Coraperutor, Model 605, with Aroolor, insert oup In the comparator, and ooetpore against the oolor disc (No. 620o-40, Lubricating Oils and Petrolatum) which has N.PJk. oolors from 1 to 5 In one-half steps. Report color to nearest 1/4. Clean the test oup with s mixture of CCl* and benzol, with final rinse of benzol. AOIK color number# coincide with National Petroleum Aesocletlon oolor number (1915). The relation of the N.P.A. eolor numbers to othsr oolor scales is tabulated below: NPA Color Nos. (1915) NPA Names Union Petro leum Co. 1A 1/2 3/4 11-1/2 22-1/2 5 3 -3/fc 4 4-1/2 S 6 7 5* " Lily white Cream white 0 - H Extra pale Extra lenon pale I J Lesson pel* K Sxtra aran** Orange pale Pale Light Red Dork Hed L U n 0 p Claret Red s A3TO Color Noe. Loribond Ans]Lysis ueoRed Yellow Blue 200 510 -- 1 0-.12 1.5 0.60 2 2.5 2.5 4.6 3 6.9 3.5 9.4 4 14.0 4.5 21.0 5 35.0 6 60.0 7 60.0 8 166.0 0.6 1.1 1.7 2.4 8.0 26.0 27.0 32.0 45.0 50.0 56.0 93.0 60.0 106.0 64.0 - .55 .55 .55 1.80 FABtea 1-26--45 Copied by re 4/27/46 COMPANY CONFIDENTIAL WATER PCB-SD0000001071 itoaa&at-e Chemical Company V Ann 1 srtoa Mathod No. 14-44-48 ZPBJgCTi Coloi* of "'later Thite" Aroelor L3TIDD; CofrrparisoB against A.P.H.A. loala 3oopa , The method 1* applicable to Aroolor* 1234, 1260, or otter a haying oolor Iim than N.P-A. #1 ( " .atar \rhlt%") . A.P.H.A. "tandarde These oolor standards are sold solutions of potassium chloropletlnata and oobaltous ohlorlds. Tha unit of color is that produced by 1 me. of platinum per liter. Tha ratio of oobalt to platinum nay be varied if neoaseury to matoh the hue. Because the hue of Aroolor 1254 am! 12 60 seems best mate hod without cobalt, this has been omitted in the preparstIon described. Dissolve 1.245 g, of potassium ch loro pin tinate (KPtCl4) cootainii^ 0.5 g, of platinum In water with 100 ml, of oonoentrated hydrochloric acid, and dilute to 1 liter with distilled water. This solution has a color of 500, Prepare standards from 10 to 100 in steps of 10 by diluting 1, 2, 3 ml. etc. of tha above solution with distilled vnter to 50 ml, in standard high farm Nessler tubes. Protect the tubes from evaporation. Refer to peps 13 of "Standard Methods for the Examination of .'atar and Sewaga" eighth edition (1936) for details of standards containing cobalt. Published by American Public Health Association, 1790 Broadly, New York. Procedure Fill a match Inc Nessler tube \*ith Aroolor to a height equal to that Ln the standard tubes. Compare with standards by looting vertically downward through the tubes upon a white or mirrored surface placed at such an angle that light Is reflected upward through the column of liquid. A color tubs support (Fisher #7-065, 30 ml.) is convenient. Laanaueh as tha proportions of the standard color solution in tha compari son tubes are such ae to represent an aliquot part of a liter, the readings are dlreet as parts per stllllon. Colors up to 100 are recorded to the nearest 3. Direct comparisons are satisfactory up to 100. Above this the sample should be diluted with Carbon tetrachloride (saxiann A.P.H.A. oolor, 5), end tha oolor obtained to nearest 10 by multiplying by the dilution ratio. FAB tan 1-30-45 Copied by rs 4/27/48 COMPANY CNFiDENTlAL TRAN 119l WATER PCB-SD0000001072 tonsanto Chemical Company Annlstcu Method No. 14-46-48 "UBJSCT: Add Number of Tolld Aroclara and Heavy Liquid Aroclars IETROD: Titration with Alkali ualnr, Phenolphthale In Procedure Dissolve 50 grams of the Hjoolor la 50 ml. benzene In a 400 ml. baifcar, warning to hasten aolntlon. Add 50 ml. 3A alcohol, 200 ml. distilled ' water, heat to boiling, add 1/2 ml. ljl phanolphthaleln aolutioa, and tltrata, la tha case of tha dl at Iliad Aroolcrs with 0.01 N sodium hy droxide aolutlon, to a faint pink oolor whioh la permananT for at least two mlautaa after vigorous stirring. A reagent blank should be run oo> ourrentiy. Tha aeldlty of tha aampla is calculated as milligrams of eodiun hydroxide required per gram aampla. Calculations Using 0.01 N NaCR, Add No. ml. titration X 0.4/samnle weight For 50 gn. ~ Aoid No. (ml. tit, ml. blank) I 0.006 Using 0.1 R NSCE, Add No. - ml, titration X 4.0/aamnle nslfht For 50 gra. Aoid No. - (ml. tit. - ml. blank) I 0.06 Apparatus 10 ml. burette in .05 divisions. Conversions 1. To obtain Neutralization Number In terras of XOII, multiply the lold Niuriber in tarns of NaQH by 1.408. Inverse faotor Is 0.713, 2. Uultlply tha Aoid Number by 1000 to obtain the paxta of NaOH re quired to neutralize one million parts of Aroolar. Thus Aoid Nunfeer of 0.0006 la equivalent to 0.6 parts of NeCfi par million nerta of Aroalor. S. Tha large Mount of aatar used causes sharper .separation of the aqueous layer from the non-aqueous layer, thereby making the endpoint ore easily distinguishable. If the titration ia carried out against vary light background or In a fluorescent light, the and point la easily seen* 4. Aside fran free sold ss s cause for NaCB consumption, ferric chloride which is usually present in call amounts, also consumes NaOU in neu tralization to phanolphthalein. It tbarafore follows that an Aroolar of vary lorn acid number rust be also extremely low in ferric chloride. FAB tom 1-26-45 COMPamv TRAN 011911 WATER PCB-SD0000001073 Monsanto Chemical Company Anniston Method No. 14-47-48 ^JBJSCTi Pour Point of Liquid Aroolore MPTnOD; A.3.T.M. D-97-39 The pour point of an Aroolor la the lowest temperature at which the material sill flow when It Is chilled under certain prescribed eondltlone listed in AJTU D 97-99. Apparatus Apparotua consists of test Jar, thermometer, oork. Jacket, disk, gasket, and bath as described under A. j.T.13. method 097-39, The thermometer Is'the A.O.T.M. Cloud and Pour Test, ranee -30 to 50*C. Present ermeretue Is the nil Orelner Co. IfcBl 2234 einr.le unit with Qr2242 test Jar. Procedure for Aroclor follow 097-39 in all respects except that the centigrade scale is sub stituted. Only on outline follows: Add 40 al. of Aroclor to test Jar. Adjust thermometer to center of Jar with beginning of capillary 1/0 inch below surface of the Aroolor. '..'arm the Aroclor without stirring to 46*C. lh a bath at 46-48C. Cool to 32C. In air or niter bath at 23*C. Trans fer the Jar to the Jacket of the cooling bath which Is maintained at 0 to 3*C. Beginninc ut a temperature 8 to 10 degrees chore the pour point, at each lnterral of 2C., remore the test Jar from the Jacket and tilt Just enough to determine if there is movement of tbs Aroclor. This Inspection should not retire more than 3 aeoonde. '-'ben movement is not fromptly apparent, the test Jar should be held in a horizontal position for exaotly 5 seconds as noted by a stop watch. If movement occurs, imedlately return the test Jar to the Jacket, Repeat test for flow at the next temperature 2C. lower. Continue the test In steps of area degrees centigrade (14,12,10, etc.) until the Aroclor show no movement when the test Jar is held horizontally for exactly 5 aeoonde. This is tbe #olid point. The pour paint le the previous temperature, 2C. above the solid point. The pour point Is thus the lowest temperature et wHTcE" the liquid will flow or pour under the test oonditlone. Technicians must familiarize themselves with D97-39 which gives complete details of apparatus end procedure, reproducibility of results, effects of thermal history, etc. The directions above are inadequate except as s working outline. The bath twopereture is controlled by adding dry Ice to acetone for pour points bi>low 0*C. FABtca - 1-30-4S Copied by rs - 4/27/48 COMPANY CONFIDENTIAL TRAN 011912 WATER PCB-SD0000001074 ifensMt Chemical Coapaay Anniston Method Ho. 14-4S-48 ^TBTECT', The Testing of Aro'olara for Inorganic Chlorides iaiTTODs Solutions Required "Headerd Chloride Solution: DiseolYd 0.650 grume of pur# sodium ahlorids is suffioient weter to man but exactly 500 ml.; 1 ml. then contains 800 raicrofxa.'as Cl. Pipett 25 ml. of this solution to a 500 ml, flask and (rake to the mark to plTe s 0.00115 U NaCl solution, 1 ml. of which eontalas 40 Biorof^rsmt of Cl. PmmrvQ is a Pyrex bottle. Caution: The weter used in preparation 'suat be chloride free by the Tyndall Beam teat; the 0,00113 y solution should not be kapt orer 1 month. Silrer Hitrata Solution 10: Dissolrt 5 rrams of ailrer nitrate crystals In 40 ml. of water and add 10 ml. of ooaoentrated nitric said. Chloride frea distilled *'ater. Apparatus Required Lalfertts 10 ml. color tubes (13 an. 1 100 ran). Test tub# rack with a black urfae at the base for uniform comparison (Rot#: we are using black gasket rubber ever the entire board that sup ports the baee of test tube a dux Inc ooraper ison.) Box, About 7" long and 4" wide. This box contains holes In top and notched in the bottom to hold Laraotte color tabes. It is just hlgi enough to allow 1/4" of test tabs to extend through the holes in the top. The box should b# painted a net bleak on the lasid and on top and should contain enough hoist to aocoaodate nt least seres tubes. Method Clean all flasks, tebi9 sad pipettes to be ueed. Thsn rins* with dilute nitrlo esld then with chloride free distilled mtr. Add 5 ml. chlerid free water to e 250 ml. Erlenmeyer flesk, heat to boiling, M 800 of the Arcelor to b tasted, *ieh has been heated to 100C, shake rigorously for 1 aiaute, cool in coalin?:* pea. Carefully d*aant worn of the water extract to a aeperatory funnel. ^eeh with pure ethyl ether (chloride free). Transfer 10 ml. of the *ihr washed extract to & 10 si. Lsl&it color tub# after riaaise tub* with portion of street. Frpre standards by diluting, exactly I si. of the 0.00133 M 1*01 solution to 100 ml. In e COMPANY CONFIDENTIAL IR*N 011,1 WATER PCB-SD0000001075 Tb Tart Lag of Aroeiorf for Inorganic Chloride . z ,, voluaetrle flask, Oa ml. then contain 2 miorograra of Cl. Transfer 1, 2, and 3 al, portions to 10 ml. tub. Lake to the 10 ml. mark with Cl fre SfiO. Piece standard end sample In light free botx from whloh only the top of tube are erpoeed add 0.5 al. of the silver nitrate to aoh tube compare La a specially prepared test tube rack. The comparison is to be Bade quiokly and from a constant source of light , preferably day ll^it froa a window away from the sunlight . Comparison ie easier when other souroe of light are shielded from the comparison rack. Look dlrcetly into the top of the tubes and compere. Bote tbe known solution ?&lch nost nearly antchsa the -mter extract estimating to the nearest whole aiotofpras. The extruot blank and the distilled -rater should show no turbidity. Calculation Divide tbe ohlorlde content In mlcrorren of the known solution whloh mutohee the extract by the weight of the Aroeior represented by the ertraot to obtain the chloride content of the Aroeior In p.pja. . In the prooedure described, the 10 ml. extrect represents 40 -ran of Aroeior (I/O of 200 g. taken). The three known contain 2, 4, and 6 Aerogram of Cl, thng rerreoantlng O.CO, 0.10, end 0.15 p.p.m. retpectively. Values should be reported to the nearest 0.025 ppm. Precaut ion Because of tbs sensitivity of this test, eerious errors may result through very elicit ooataaination .or Inattention to detail. All equip ment must ba eorupalously cleansed, tbe diatllied water abeolutaly ohlorlde free and testing doae away froa fumes of S31 or chlorine fume. re 4/27/4,8 COMPANY CONFIDENTIAL tr*n 01191. WATER PCB-SD0000001076 Ueasaato Chemical Coapany Anniston liethod He. 14-65-48 SUBJECT; '.ater Contact of Liquid Aroolors U&THCO: Tltrat lop with Karl Fischer Raftrant Outline The Aroolor is dissolved In a mixture of benzene and methanol whloh has baen tltratad with Flohar reagent to the characteristic end point, Piecher reagent is a solution of iodine, sulfur dioxide, and pyridine. Iodine is consumed as long as any water Is cere sent. The solution is a<?ain titrated to obtain the water oontent introduced by the Aroclor, Solutions and Apparatus Karl Fischer Reagent: Weigh into a flask: 264 prana of pyridine, Barrett E~A or Eastnan 214-41, and add 61 /Trans of liquid or gaseous sulfur dioxide. Add the liquid eulfur dioxide directly fro* the inverted cylinder by attaching to the outlet Yalta a glass tube extending into the pyridine. Sulfur dioxide gas oen be bubbled Into the pyridine until proper amount is added. Store in a glass stoppered bottle. Transfer 65.6 grans of the pyridine-SO mixture and 134 si of absolute methanol to a 1 liter Florence flask. Cool thoroughly in an ioa water bath. Add 16.9 grans of iodine, stopper, cool again before shaking. Alternately cool and swirl until the iodine is in solution. Hakes 800 si of reagent. Store in glace stoppered bottle. Let stand 84 hours before using. Then fresh, one si of reagent is equivalent to about 0.0003 we. of water. Aroclor Solvent: Mix 8 parts dry benzol with 1 part anhydrous methanol. The dry benzol Is prepared by shaking the oosnercial grade with anhydrous oaleiua chloride, decanting into a flask and distilling, rejecting the rirst loyi to cone over. Keep in glass stoppered bottles with ttlnisan exposure to air. tfioro Burett 10 ml. x 0.08 si. Koch automatic with glass stoppered reservoir. Ick and KTebs #460. Equip reservoir with a moisture guard tube oontainlng Drierite or a similar dehydrating agent. Procedure Heat a lean BOO al. narrow south Irlenweyer flask in an oven or on hot piste until thoroughly dry. 9weep out for 10 alnutee or until cool with air which has been thoroughly dried by passing thru tubes containing 8 mmefa Drierite. Disengage the flask from the aspirating train and inmedlately close with a paper oap held by a rubber bead. COMPANY CONFIDENTIAL TRAN 0U915 WATER PCB-SD0000001077 I :i8kr Content of Liquid Arooiors - g - Hthout delay, transfer 100 al. of the benzene-ethanol solvent to tha flfl&k thns s Mil hole punctured Into the paper cap. Carer again with paper. Titrate at once with Karl Flsaher reagent to distinct red-brown end point which does not fade after swirling seTerml times. The Fisoher reagent is dispensed from the mleroburet the tip of which projects into the flask thru the puncture in the paper cap. At the end point any water content of the eolrent hse been reaoted, Ouperlnrpoee a fresh paper an Immediately. Obtain weight of the eolrent and we 11-core red flask cm a T'relon balarvoe or equivalent, ^ilokly Introduce with e dry pipette about 100 Tame of the slightly warned Aroclor to be tested. Cower at onoe end neigh epiln to obtain the weight of Aroolor to nearart gram, stake until the Aroclor le dissolved, II the mixture la cloudy, warm allgitly. If oloudlneaa persists another mixture should he prepared. Puncture a email hole in the paper cap for the Insertion of the buret tip end titrate with Fieoher reagent to tha lirat definite brown color, agitating with a castle swirling motion. The end point should merslrt through several twlrle. The end point may slowly feds through slow aoceea of ataoapherl* moisture in which ease it la restored by drop or two of reagent. If not so restored, the sad point may have been a files one or the closure is faulty, A definite end point Is Impossible if humid air la not well excluded. Proa the amount of reagent required and the weight of Aroolor used, cal culate the water content in p.p.au Oallbrotloa of Fieoher Peagent and ?tandard 7eter Solution Standard water solution in methanol: Transfer exactly 0.40 ml. of water frail a micro buret or a 1 ml. measuring plpet to a 100 ml. volume trio flask. Fill to the mart at onoe with anhydrous methanol and mix. One ml. of solution thee contains 4000 micro^rams of -atar in addition to any water which asy be present in tbs methanol. Transfer exactly 5 ml. of the above standard water solution (equivalent to 0.06 gytutf of water) to a 200 ml. TCrlenneyer flank which has been dried m& swept with dry sir. Close with paper cap and titrate with Fischer reagent in tbs asms manner a a the ample. The end *wint Is sharp, A methanol blank, found by titrating 5 ml. of the methanol used in waking up the rtazdsrd water solution to e like end point, must alvmye be subtracted froa this titration. Divide the mount of water taken by the net Fiadher reagent required to obtain the titer of the Fischer reagent in teen of water. Example 5 A 8 ml. aliquot of standard solution, equivalent to 30,000 aicrorxoKis of water, required 6.61 ml. of Fischer reagent while 5 ml. COMPANY CONFIDENTIAL tran oli< WATER PCB-SD0000001078 'Tatar Content of Liquid Aroelors - 3 - of the thaaal retired 0,35 of Flints? respect, 20,000/(6,61 - 0,55) - SO,000/6,06 3500 olcrofyana ^ter/ml. Reealibrations: Bedaost the Fiughar rea-ent deteriorates rapidly, it* titer mat ba determined for each days um. If the uju standard water solution ie used la reoaltbration as in the initial calibration, the titer of the Flasher rea^sat suet be calculated from its total water contact ( including that introduced by the methanol) , The total wsster i* the product of the initial rross titration and it* titer. This ia th* esamplt abov.% tha total water coat ant of 6 ml. aliquot ie 6,61 X 5300 a 21815 ralerograas. If on reoeiibration ?,3? ml. of Fischer reagent ie 21815/7.3? 2960 mlerogrsma of water per ml. Two or more calibration* should be made with agreement within 0.025 ml. Calculation of HgO empli 3tndardlzation of Standard 5,0 sol. Titrate 5 ml, slxtur 3,0 *ol. Titrate 5 ml. of methanol Tit of 3 ml, mixture A Tit of 6 ml. aafchwsol 9 ' A - B ml, rcagasst for SgO added 5/100 of .4 Dir id 5/100 X .4 by A - B * factor grama of BaO/ml. iii It i ply feotor X B girl nr, gm*. of 3,0 In 5 ml. of methanol. Add this wt. of 3,0 to ,0B already added giving 3,0 in 5 ml. (Total) Factor m_ 1,0 3t*d Titration " 1 ?!_ X srastpl Titeniio Tg ?* X 1,000,000 ppm 3*0 wt. iwipla ' : FABirn lg?-4S Copied by 1*8 4/E7/48 COMPANY CONFIDENTIAL TRAN OlHi' WATER PCB-SD0000001079 MuTC^IAL flTOBSR Proa PROPSHTIES OF BASIC fH/iL0T!AX" PfiOOCCTS Letter to !T,,C.!:./`M.T.Bolaer (Halowax Produota DIt. .Union Cert)id and Certxra Corp,,, 30 S. Forty-Second 3t., H.Y. 17, H.T.). latter dated Feb. 27 s 1946. Ho. 1000 Ho. 1001 Ho. 1013 50. 1014 Color* Flow Point (Itod. ASTO Softening Point) dff. t. White to Pel Straw r7bite to Pale Yellow Pal Yellow Liquid 194-201 247-252 P. --al--e T--ai--lr 277-203 S .eolfic Gravity at 77 dag. F. 1.19 - 1.25 1.53-1.59 1.65-1.71 1.73-1.81 P-rotratlon ("od. A3TT!) 200-e. load at 77 deg. 10-15 3-8 8-8 V Jcoaity (Saytolt Universal Second) Oxdtillation Ronp |AST0 der;. F. 33-37 at 77 da/'. F. 400-590 33-37 nrt 266 flt,. F. 600-650 31-35 at 266 deg.F. 41.5-656 33-37 at 302 da*.F. sPtPfio L =a*h Point (ASTi! Cleveland Open Cup) dec. F. 203 .284 356 3n Fir Point (AST!! Cleveland 0on Cup) der. F. Fn^er Factor at 1,000 ayalsa at 10 ayslea 338 Hone to boiling Hone to boiling Hon to boil tor ~ Lees than 0.2^ Leas than 0.2^ Leas than 0. 0 43 0.70? 0,7O< l electric Constant at 1,000 oyclaa at 10 cycle* 0 C. Roaistivity (*. *.) at 30 do*. C, -- 3-6 4-5 4-3 5-6 4-5 4-8 -- Over 107 - 108 Over 107 - 108 Over IO7-10a Copied by gseb V2/ia than 011918 COMP/rv CONFiDc,vnAL '/'L b-i L 1 WATER PCB-SD0000001080 From - Haiowex Products Division Union Csrblie and Carbon Corporation 30 East 42nd Street New York 17, New York Letter - VJ.C.U./J.M. Cole, Tech. Rep. 2A6/48 Zyrox 3007 (11-308) Q2TMERAL IHFCSllfcTICH Color 3p, Orsvity Softening Pt, . Stonier Viscosity saybolt Furol Viscosity Penetration at 50 deg. C. Penetration at 23 dec, C. Fla ah P%. Fire Pt. Co*bueti,bllitf Fracture Aoid Resistance-; Alkali Resistance , Volatility P.F. at 23 dag. 0. (1000 cyelea) Dial. Constant at 25 dag. C. (1000 cyalae) DC Resistivity at 25 dag. C. - Brora - 1.29 - 1.52 at 25 dag. C. -63-70 dag. C. - 20-27 at 150 deg. C. - 20-50 at 150 dag. C. - Approx. 73 (30 g. load) - Less than 5 ( 200 n, load) - Approx. 530 dag. F. - Nona to 500 dag. F, - 'ill not support combustion - Concholdal - Excellent - Ixcellent - Average for 24 hrs. at ISO deg. C. 0.56 'rag. /ail. cm. /hr. - Approx. .004 - Approx. 5.0 - Over 10 nag. mas. Copied by rs 4/2/48 COMPANY CONFIDENTIAL TRAN 011920 WATER PCB-SD0000001082 i WATER PCB-SD0000001083 NO. )> WATER PCB-SD0000001084 COMPANY CONFIDENTIAL Prom: B.I.0.9. Pinal Rapt. No. 093 APPENDU II. PHYSICAL AND CIO-IJC.AL FHOP'TvTr: T OF CLOPHTN OILS Item Nos. 1, 7, 22, & 31 Pa sea 108 - 109 (as quoted la I. G. Furben'a sales sheets) Property Clophen A30 Clophen A40 Clophen A50 Clophen A60 Clophen A70 Clophen A 00 Form .................... ............................ Colour.................................. .. .. .. 'Speciflo CTuYlty at 20C .. .. 3cll41fyLnc Point ............................ Flash Point* ............................ 5hrlnko/?o: ICO* - 20*C 50 - 20C .. .. .. .. Bsllin/t Point Limit at 12rna. of L-ercury .. ............................ Lose during Tvs oorut Ion \after 6 hours at 100*C) .. Liquid Liquid Nearly colourless Nearly colourless 1.35 1.40 -lot; --5*C 166* 193 (Pensky - Gortons) & 3>*/ 1.1*E V3^ 1.2E 165 - 195 100 - 215 o.co;. 0.03^: Volatility at 20*C ............................ (1mm. of liercury for 100 hours) licit ConductlTity at 40C (In Calorlos per metre per hour per *C) . Saponification Ho. .......................... ^0.009^ 0.095 0.0 Permittivity at 20#C .................... Di - ikdcwn StropTth............................ Ii.alotton Resistance In Ohm.on. V. small 6.0 <0.001 200k7/am. 1 X 10L3 <d .oos>: 0.091 0.0 V. smell 5.4 <0.001 200kV/cn. 1 X 1013 Liquid Liquid Nearly Nearly colourless colourless 1.55 1.60 12<` 30C 222 236* In an open crucible 6' 3?1.5*E 6T 3/ 1.9E Firm Nearly colourless Tina, crystalline ~hlte 1.7 1.72 - 1.77 50 *C >160*C 240 290 or -errer . (Penaky - Martens) s - er. - - 4K 190 - 230 195 - 25C 200 - 255 210 - 260 o.oey: ^-0.00951 <0.015: <0.009* 0.01^ <0.009^ 0.0 (2 hr3. at 125* <0.009yt 0.007 0.066 0.0 0.0 0.0 V. snail 5.0 <0.001 >2001Y/om. 1 X 10 14 V. SHSB11 V. small 4 - 4.5 3.0 < 0.001 <0.001 > 200kV/cm. - > 1 X 1014 >1 X 1014 0.0 V. small 3.0 - > 1 X 1014 Clophens are not poeHu t Ible and do not 3uonort combustion of materials Into v/hlrh they are Impregnated. 0 T - -V -I TRAN 01L9Z<t WATER PCB-SD0000001086 TABLE I Fron - United states Patent 2,070,268 Patented February 9, 1937 Pa-'e 2 o 33 > 2 O s> ro VJ1 Hydrocarbon corapoaltlons 1 Die- tilled i Di- blfth boiling corn- phenyl pounds 1--------2--------- 3--------4---------- 5--------6---------- Percent 0 0 80 60 50 50 Percent 100 100 20 20 50 50 Ohiorine content Percent 23.9 40.3 41.2 52.2 42.0 36.4 Properties of dielectric Viscosity aec. bolt at 210 F. 1oecIfle yraTlty at 65*/65* C. Dielectric constent K at. 100* C. (1,000 eye lee) 63 290 35.7 47.5 46.0 40.8 1.251 1.405 1.352 1.490 1.383 . 1.324 4 .25 4.98 4.07 4.56 4.84 4.89 Properties of chlorinated diphenyl 7--------8---------- 100 100 0 54.0 0 42 ,0 46.0 34.0 1.523 1.380 ___________ _J 4.30 4. Copied by rn 2/2/48 300, 2100 $-4 l cr (pi w & i WATER PCB-SD0000001087 I-A (J) - 500 Stability of Grado P Uycar and Teflon In Aroclor 1254- at 130*C and 45*C Short Form iieport No. 2179 File No. 141-27.1 . December 29, 1947 Notebook references: Smith 45137 Crade P Hyoar and Teflon Immersed in Aroclor 1254 Material Temp, Hours Oa In In ",'t. Jj Gain in Thickne as Grade P Hycnr Grade P Rycar Teflon Teflon 130*C 45C 130'C 45*C 285 285 285 285 68.6 26.3 Negligible Negligible 26 6 Negligible Negligible re 1/14/48 COMPANY CONFIDENTIAL TRAN 011926 WATER PCB-SD0000001088 I-A-l - 500 From - Memo P.C.B./R .L..T. 3/22/4B Aerovox Corporation New Bedford, Maasachu9etts DeteminLap; I'luoro9cence in *roclor "The ullroviolet lipht '; uoe for determining fluorescence in Aroclor ig manufoctured by Oeor'-o 7. Ckitc.s and Company, Franklin Square, Lone Inland, Mew York. It is a CH 4, 100 /att, G. E. Mazda Lamp with filter. "Our procedure 1s to pour a small amount of Aroclor into a 5" watoh class or a 5" Pyrex evaporating dish and observe for the decree of fluorescence under the CH 4 lamp, preferably In a dark room. If the sample has been contaminated with Mineral Oil it will ehow up as o streaky or milky fluoreaoence ee oompired to pure Aroolor. The fluoreaoence around the meniaeus of cure Aroclor ia not to bo oonfusod with tha fluoreaoence resulting froa contaminution. "This tost is qualitative end, os eucht is based on the experi ence of the person performing it. 'It keep standard sample for comparison. If there are any further Questions please fool free to contact us". Copied by rs 4/2/48 COMPANY TRAN 011927 WATER PCB-SD0000001089 COMPANY CONFIDENTIAL v '' I-B-10 WATER PCB-SD0000001092 WATER PCB-SD0000001093 . COMPAMy CONFIDENTIAL TV /# -* WATER PCB-SD0000001094 II-B From - B,1.0.3. Final Report No. 83 Item Nos. 1, 7, 22, and 31 Faros 12, 13, 14, 15, 16, 4 17 III. CHLORINATED D IFHTNTL 1. General. Chi or ice ted diphenyl is manufactured by I.G. Farben under tne trade narw of Clophen, Gone types are liquid and others solid at norraal tempersturea. They are used as impregnants as alternatives to hydrocarbon oils and tsaxes. Clophen shares with other chlorinated materials a high permittivity and hua the same dangers in handling, due to noxious properties. In addition to the grades suited to capacitor impregnation, a grade known os T64 is made by I.G. Ferben, suitable for trans former cooling. The total output of Clophan A50 and A60 for the years 193G and 1943 wae:- 1939 Type A50 21 tons ASO 132 * 1943 w A50 170 W A60 506 w The cost of the material in Germany 1s:- Type A5Q 1M. 50pfg. to U.!. 60pfg. per Kilogram " T64 1U. 20pfg. per Kilogram. The follov/in" is a list of the principal prewar consumers of Clophen :- Gienens-Gchuckert, Berlin. A.E.O. (Hydrawerk), Berlin. Hioafll (Brown Boveri), Zurich, Alathom, Paris. Ducati, Milan, Italy. Switzerland. It wee stated that no German capacitor manufacturer uses Clophen for the manufacture of small capacitora for radio and telephone purposos and where these have been used by the Ger man fighting services they were supplied by the Italian firm, Ducati. - 2. Manufacture. (1) The synthesis of diphenyl from benzene. Diphenyl is synthesised from benzene as shown in the figure, following:- COMPANY CONFIDENTIAL TRAN 011933 WATER PCB-SD0000001095 /5a --v'W'v---Condenser Distilling "J Column 500-650*Cn< 200 *C Two-stece Host Drchanger Reaotlon coil; 800 *C Synthet.ls of Diphenyl from Benzene The synthesis occurs in the vapour phase, at 000*0. and atmospheric pressure, in an electrically heated reaction coil of copper-nenganeoe alloy. No catalyst Is required. The apparatus, apart from the reaction coll, is of iron, and operates at the temperatures shown above, ,.bout 10,' of the benzene vopour Is oonvertod Into diphenyl In one passage through the reaction coll. The purity of the benzene is of Importance for the elec trical quality of the ultimate 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 infornetion could be obtained regarding any undeslroble impurities or the mechanism by whiah they cause poor electrical performance. Thiophene wes stated to be definitely harmful, and vague reference v*a made to "nitro-compounds", to "aliphatic hydrocarbons" and to "substances which could not be chlorinated". The pre iae nature of these materials was not known, but their absence we a ensured by obtaining benzene always from suppliers whose product woa known to be satisfactory. Analytical Specification for Pure Benzene Appearance: Clear and colourless. Density at 20*u .: 0,876 Distilling range: first 5f. within 0.25*C. S* - 95/. " 0.25 C. 95,", - end " 0.25*C. Solldlflcotlon point; Dot leso than 5*C . Bromine consumption: Not more than 0.5 gm. bromine per 100 c.c. .lulphurlc acid test: Not more than 0.15 9a, K2Cr2o7 Carbon disulphide! Shall b free from CS,. COMPANY CONFIDENTIAL TRAN 01193<* WATER PCB-SD0000001096 Difficulty in the synthesis was still being experienced, due to rapid corrosion of the copper-manganese reaction coil, operating at 800*U. A smell scale experimental npporotue using a fused silica coll had boon .Tiede, but had Dot beon developed for production use. In addition to diphenyl, ebout 5% each of 1-3 and 1-4 terphenyla are produced by the process. These are se parated, chlorinated and used In sealin'1: Tarnishes; present production is about 4 tons per month. No use is made of chlorterphenyla as paper lmprer,nants, since the materials are resinous and tend to crack; moreover the permittivities axe lower than those of the chlordiphenyls. The crude diphenyl is next purified by distillation. During this process the terohenyls remain in the residue. They are extracted in the following nenner:- The residue is dissolved In hot benzene, filtered, and the 1-4 isomer obtained by fractional crystallization. The crude product is distilled in vaoue, yielding 1-4 terphenyl with melting point of 208*0. The 1-3 isomer, ro/naining in solution in benzene, is more difficult to isolate. The solution is clarified with activated char coal, filtered, und the benzene evaporated. The residue is distilled to yield 1-3 terphenyl v/ith Tilting point 80-84 *0 . (2) Chlorination of diphenyl. For the chlorination of diphenyl a lead lined teasel of 10,000 litres capacity is used. It is charged "ilth 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 chlorine is continued for 100 hour's at a rate of 130-135 kg/hour during which tins the tem perature is raised gradually from 110*0. to 130*0, The end point of the chlorination la determined by measuring the density of the product. To remove hydrogen chloride formed In the process, dry air is blown through the liquid for 2 hours and this hy drogen chloride is rcoovered. The product le transferred to another vassal and treated with 1/2ft of solid sodium hydroxide, heated and agitated. Tile sodium hydroxide is allowed to settle oat and the Clophen drawn off from the top, transferred to another vessel to which Fuller's earth and soda are added and the liquid redistilled. The stllle for this process are gas heated. COMPANY CONFIDENTIAL TRAN 011935 WATER PCB-SD0000001097 3, Trcpeft le b ,, ' . (1) Capacitor Lmcremcting grades. A suEjcury of the physical and chemical >rooertias of ths capacitor irapregna ting trades of Clophen la riven in Appendix II, Thera are six gradeo of capacitor isrpr egnant, A39, A40, etc. up to AfiO, the 3, 4, 5, etc, Indi cating the number of chlorine radicals combined ",1th the diphenyl. Tech grade contains a proportion of the adja cent homologues not erceedlng 20?.. Grade A30 has the highest value of permittivity. Theoretically the hirhest value obtainable ",'ith a chlorinated diphenyl is 9.0, and a grade having a permlttlrlty of 7,0 has been prepared, but is cheniotlly unstable, and very sensitive to moisture and Impurities. The most eonnonly uoed grades are A50 and AfiO; A50 is the most stable grade and has the Iciest dielec tric loso. Oade A60 is considered by 1,0, to possess the optimum combination of non-inflammability, stability and viscosity. Aa with Nibran, it in considered that no addi tives are required since the substances ore stable in use,, provided that the capacitors are efficiently sealed against tho air. tllcufil of Zurich are the only users of <130 and A40. The following table shows tho variation In oapaeitance and povjcr factor with, temporuturo for a Clopben impregna ted paper capnoitor. Tho lmprecnant Is A50, the dielectric is Ochoellor and Hoeoch "A" finish reg tissue (density 1.2 - 1,25) with a thickness of 10 n; froouoncy of measurement is 000 o/e Power factor shows a maximum value of 0.052 at about M*CV while capacitance foils off by some 20? at temperatures below thia critical value, Variation in cc.pecltance and pcrwor-factcr with temperature for a Clophen-impregnated capacitor Temperoture (*c.) -60 -40 -20 0 4 420 440 460 400 Relative Capacitance 0.07 0.91 0.94 1.02 1.06 1.10 1.10 1.10 1.11 Power Vactor 0.035 0,024 0.013 0.048 0.052 (rasx.) 0.006 0.005 0.004 0.005 No evidence was obtained from I.G. on the use of any type of additive rrith a view to depressing the temperature at whleh the change of state occurs. COMPANY CONFIDENTIAL TRAN 011936 WATER PCB-SD0000001098 The method adopted for evaluatin'' the -.vater content In oils such ss Clophen is described In Appendix III. It Is algo applicable to 3uch solids as Nlbren, Tn^elhardt stated that no source of failure had been ex perienced durlnr the whole period of production of Clopben, which is about 17 years. Consequently no improve ments or nodificetions had been made or found necessary during this period, (2) Transformer-cool lac rrade (Clophen T64). No detailed infariation was sought on this material, since it is unsuitable as a capocitor iraprecnant and is onlyused as a ooolant fcrr transformers and phase shifters. A summery of its physical and chemical propertle s la civen in Appendix IV. It has a low viscosity, Is moderately stable under electrical stresses and has the distinct ad vantage over mineral oils of beln^ non-inflammoble. The principal users of this product are A.E.O. and "Siemens, but It is understood that, as with other chlorinated ecrrvpounds, consorvotism cad prejudice amonc customers have prevented its wider use. No stabilisers are added to the material as their function of absorbing hydrochlorlc acid would be defeated by the formation of "chloride salts", which In turn become elec trolysed. It was ssid to be very important to avoid con tamination of Clophon T64 which may occur In transit and for this reason the use of leather for raskets must be avoided. 4. Methods of use, precautions, ate. No details were obtained on the method of impregnation used by I.G. for the construction of test-specimens of Clophen-Impregnated capacitor. This was partly coused by the nonappoarance, after the first day, of Engelhardt, but it is not considered likely that any novel processes are involved. Tor Information on the precautions necessary In the use of Clophen, see lection II, 5, above. re 12/19/47 COMPANY CONFIDENTIAL TRAN 011937 WATER PCB-SD0000001099 m-A-t - 500 ^ron - R,1,0,0, Final Report Uo , P93 . ,Item flos 1 7, 02 and 31 PC x It Clophen la made In several rT-dos, which oorreapond closely with their U.3, counterparts, A.50 beinc the .mrude moat commonly used for capocltore. , I'iCept for very rare use by 'Ueraons and TTalske for special ordors, Clophen hca not been used in Oemony for amell capacitors of the telennmmin t nnt ion typo, but It hes been usod extensively by Rlenons-lchuctert for power oapacltors. It la interestin'* to note that the German forces used Clophen imprecated and filled tubular capacitors mode by Ducotl, of IJilan, who obtained the imprecnont from 1,0. The prejudice amainst Clo phen vrea, hoviover, belnr, gradually overcome and several manufacturers were oontemplstinc an extended use of this material, Gome of them con sidered it to be equal to or possibly hotter than mineral oil for opera tion at power frequencies. ra 11/2^/47 COMPANY CONFIDENTIAL TRAN 011938 WATER PCB-SD0000001100 III-A-b-50 FTora - B.I,0,G. 7Inal Report Mo, 893 Item Noe. 1, 7, 22, end 31 Pages. 98, 99 (2) Clophen The only chlorinated impregnant used by liemensGchuckert Is Clophen, supplied by I,,G, In power factor correction and high roltage applications it is consider ed practically ideal. The only type of Clophen used In bulk is A.50, pentachlordlphenyl, (corresponding to Aroelor 1254). A.30 end A.40 have been tried and found unstable, A.60, A,70 end A.80 ure too viscous to allow for pood Irapregnatlon and have lerver permittivities. Although the viscosity of A.50 at room temperature la much rreater than that of oil, the viscosity at impregnation temperature is sufficiently low to give do trouble in attaining thorough inrpregpna t ion. A routine check on conductivity is mode on each drum of Clophen, and formerly if the conductivity were too high, the Clophen was treated with povrtlered chalk to neutralise the free acid. Aa the result of continual pressure on I.G, over a period of years, the acid content had gra dually diminished, and it la now possible without chalk ' treatment to work to the same rejection limit of resis tivity as for oil, viz. 101*5 ohn..em. at 20*C. Drums of Clophen foiling to pass the conductivity test are returned to I.G., unless urgently needed. A certain elasticity is permissible in view of the hi^i standard set. Apert from conductivity, further acceptance checks ere specific gravity (1.54-1,55) and permittivity (5.0 5,2). Permittivity is measured at 800 oycLes and 20*C . on a Sobering bridge at law voltage. The acceptance standards for Clophen A.50 are shown graphically in Appendix XXXIV. Clophen costs about 1 11. 60 pfg./kg., and is therefore much dearer than oil (30 pfg./kr.). This extra expense ia offset, however, by the use of a special design which reduces the amount of Clophen required. An ad vantage claimed for this lapregnant is that is has a similar permittivity to paper (vis. 5). Other lmgregnants studied. As Clophen la considered nearly ideal, no serious attempts have been made to find superior moterials or addi tives to improve its performance, This attitude is sup per tad by service experience, in which no failures have been reported. It ia realised, however, that on freezing discharges nay oeeur in the eoatraetlon roide, which may result in decomposition of the Clophen and failure of the COMPANY CONFIDENTIAL TRAN 01 L 9 3 9 WATER PCB-SD0000001101 re 11/19/47 dielectric. Tests were performed (see 'Section 17, 2, (3)) to check T/hethor this degradation does in foot occur, and no failure wes noted. Nevertheless, 1.0. supplied snail samples resembling Clophen A.50 but having a lower melting point so thut this possible source of failure r. >uld be Investigated. Uepresslon of the temperature at which the dipoles beecrT* lrmoblle should raise the maximum usable frequency and hence broaden the range of applications by introducing those Tor eudlo-frequenoy furnaces- Two of these I.G, sonnies, with references A. 1621! ond A.162N, are, like Clophen, rode fron benzene, but hare a lower chlorine content because of the presence of un additional alkyl croup (CnH2n'fl) Qn(5 hence a lower denalty. Their advantage over Clophen A.50 is that the setting point (l,e. tamporoture of maximum dispersion and of capacitance diminution) is lowered from -G*C. to -17*C, The permit tivity, viscosity and non-inflammability resemble those of Clophen A.50. The vlscosity/temperoture curves of these two samples, K.7 mineral oil and Clophen A,50., are oompared in Appendix X)CKV. COMPANY CONFIDENTIAL tran oii9<*o WATER PCB-SD0000001102 III-B--2500 December 22, 1947 TO: PHO-SPlI-.n; DIVISION 5JBJ: Arcelor 5460 oe Used In Dthylcellulooe Lacouer RE: Federation of Paint and Varnish Production Clubs Official Digest (October, 1947), Aroclors used as plasticizers aDd reslno impart excellent Qualities to ethylcellulose. I'.thylcellulose Is used In lacquers of vurlouo types, the ethylcellu lose acting as 6 long chain oolyner to inpart toughness and flexi bility and to increase the speed of drying. Come of the prlncipol uses for ethylcellulose lacquers are for the ooatine of high tension ignition cable; heat sealing lacquers for foil and paper where the slight discoloration which may develop in nitrocellulose luoquere on heat sealing ia not permissible; linoleum lacquers whore alkoll resistance lu essential; textile printing; printing, inis, particularly in multicolor dosirna wlro hydrocarbon solvent does not soften or blood into previously printed designs; alroraft lacquer for rcaistunco to both heat and cold and to nuiolc temperature obanges; record lacquers, especially for home rocordere; and in wood sealers where good saDding and flexibility ere essential A god pigmented ethyloellulose lacquer has been made, based on the following fornula: Ingredients Ethylcellulose N-22 Aroolor 5460 T103 Menthylphenol Toluene Ethanol farts (by weight) 6,4 6.4 4.2 0.06 67.0 16.0 100,06 rh Copied by rs 2/2/48 Benignus COMPANY CONFIDENTIAL TRAN 011941 WATER PCB-SD0000001103 II 1-0-300 ?ron - fiemo G.Y, Frankle/P.Q. Bentrnug tbrch 11, 1948 Soil-Poison Conoentrcte As described below, the-e materials are formulated into a water emulsifinble aoll-poieon ooocentrete corryi&e almost 30 per cent by weight of uotive inpyediente. Aroclor 1242 Triohlorobenzene (Mxed leomora) Pentachlorophenol Isopropyl alcohol Toluene or Xylene Sterox SE* Santomerse 3 Paste 33.3V- 33.5 10.0 3.3 16.7 1.5 1.5 100. Of. * Other non-ionle type emulaifyin,'; events such ae Triton NH or Span and Tween oon be used to reoLece the Storox SE. Coplod bp re 4/2/48 COMPANY CONFIDENTIAL TRAN 011^2 WATER PCB-SD0000001104 Chemical Abstracts P03CIQLF, UCE OF AROCLOTn Vol. 41 Pago 6067 III-H-10 U.S.P. 2,425,973 to Anderson and Coalahan, (Hercules Povrier Company) . Foundry cores sprayed with 15^' solution of chlorlneted nophthalene in hydrocarbon solvent show /Treater scratch resis tance than untreated corc3. Cl2 content reneins from 40 - 80,' Cl2 . Particularly mood for use 'iltb '.1 cagtinr9. rs 12/2/47 COMPANY CONFIDENTIAL T RAN 011^43 WATER PCB-SD0000001105 n-io FTim - B.I.0,3. Final Report Mo. 0yj Ite-i Nos. 1, 7, 22 and 31 Faroe _ lo and 11 Much lees trouble hee been experienced with chlord 1 ohenyl thnn with ohloraephthalene, probably because the former, being liquid, lnvolvee lese physical Contact in d isposal. (2) Prevention, Very thorough washing of all areas of the akin likely to be contaminated with solid, liquid, or fumes has always beon the basic principle in prevention of skin troubles, and in still looked upon ao fundamentalo "/hen fatty soaps ceased to be ovailoble, because of the di version of fats to food, it became essential to Insist upon the nee of barrier creaius, of which the best was one named " ^CnrBO", mode at Tromraeredorf. This has now been replaced, for lack of supplies, by en alternative mode by I.G., named "MITIOAl", which is considered inferior to 'uimbo but satisfactory. The Flsann film, put up a special powder named " -'.CTTTELKTLVTRn to act as a barrier, but this '.mbs found to be inefficient except to allay irritation on skin areas exponed to fume3 only. For this purpose it still finds use at Leverkusen and at the Hydraworks faotory at 3erlin. . A special point is .mode of fume extraction, and the minimus uir speed away from the operator io 1 metro per sooond,, To check the efficiency of the precautions, a thorough exami nation is made every 4 weeks of every worker coming into contact with chlorinated hydrocarbons, and since the enforcement of the precautions, no deaths or symptoms of internal injury have occurred. Tinea superfatted soaps have ceased to be available, e cleansing composition oontoining lUchlor-methane has beon devised. This ie ao powerful a detergent for chlorinated materials that barrier creama are considered unnecessary, but it la uncomfortably irritant to many skins. (3) Cure. hen severe attacks or chlorecna and internal sickness were onoountered, in the eerly years, when the properties of chlorinated ranteriolo were not well understood, extensive rest periods had to bs prescribed, together with a generous diet, entire absence of further contamination, and long periods in tbe open. nines precautions have been token to minimise the effects, only a few mild cnees of chloraene have been met. These have been treated with a solution of acetic and selieylic acids In metbyleted spirits. COMPANY CONFIDENTIAL WATER PCB-SD0000001106 2- (4) Cone lu a Iona and Recommencetiono. 1.5. oonaldor that neither toxicity nor skin affection need now be any deterrent to the use of chlorinated naphthalene, and that chlordlphenyl is if anything 133 troublesome. Certain people, notably those -lth fuir skins, show distinct ollorcy, and are boat diverted to other work not lnvolvinr contact. hcrupuloue cleanliness of the skin (including the faoe,, neck, and arms) and of the clothinr (caned ally uuderrerments) I3 ossantial and needs strict enforcement. fashing v/ith hot vter and good soap ia sufficient, so long as the soap is superfatted,, since the skin beoo/nas sonoltlvo to irritation by alkali. Barrier cream should be used on those parts of the skin which oome into contact with solid or liquid material,, and the area of contact should be minimised by the use of protective clothing and glovca wbero possible. Areae of the akin wnioh ore contacted by fuiaoo only, and particularly those ohafed by olothing (e.g, the nook adjuoent to tho edc of the clothing) need protection by a suitable soothing powder. ".'here fumoo are generated, thoy should be drown sway from tho operator at on air speed of at loast 1 metre per secind. It may be found essential to hove two ducts, one at floor level, and one overhead, with exhaust In two directions simultaneously. In case the procautions are being, evaded, or lest there should bo acme idlosynoraay, monthly medical inspection is desirable. ro li/24/47 COMPANY CONFIDENTIAL TRAN 011945 WATER PCB-SD0000001107 IY-3-100 From - The Journal of Industrial Hygiene and foxlcology Volume 20, Humber 2 February, 1930 ;-ORp:ioi.oG7Cni cr^ooo in nr uvnic of rt..n RESULTING FROM EXPOXHE TO CERTAIN CiELORDIiTL'D HYNROC.dlBONR * Chlorinated hydrocorbone, particularly chlorinated nuohthclenes tmd chlorinuted diphenyl, hove been used extensively In certain In dustries. Tbelr uoe in the manufacture and nreoart.tion of many types of electrlcul equipment Is constantly lncreaeinr. Although It Is knovra thot some of tber.e compounds cause acne, only rocently hes the possibility of more serlouo oyntemic effects been recognized. The present paper describes tlw> pathological chonrcs observed in rots that had been exposed to various chlorinated no'htheicno com pounds and to chlorinated diphenyls Compound G (chlorine tod diphenyl) was administered to two ''route of anlmnla in low concentrut 1od3 . aH uvoruce concentration of 0.57 mgms. por cu. m. wug employed 16 hours dally for 134 days In the first experiment. In the second experiment (employing on overure air con centration of 0.93 mggis. por cu. n.) the enimal3 -'ere exposed P hours daily for 143 days. The present experiments demonstrate that chlorinated noohthalene compounds and chlorinated dlphonyl ore c&pablo of mroducing marked liver damage in the white rat without demonstrable mi croocotic ohjn"cs appearing in the other' organs. Furthermore, the characteristics of the liver leoione resulting from comparable amounts of any '-iven com pound ere the sumo, regordleos of the method of administration (inha lation, feeding, or subcutaneous injeotlon). Of the vurioua chlorinated hydrocurbona tested, ohlorln ted di phenyl gave evldance of being the ;oo9t toxic, '/hen administered by Inhalation In very low concentrations (average 0.57 to 0.93 m'-ma. per ou, n.) liver cell changes were very pronounced after the first exposure period. The moat striking Ghango ts the hyalinlzntion of t the oell cytoplasm (sec fig. 6, plate III). Such cellular alterations were essentially unchanged after a 2 month recovery period. In these animals small eublethal doses of carbon tetrachloride and alcohol uni formly produced extensive liver nacroslo and was highly fatul to there (firs. 1 and 2, pluto VII). Chlorinated diphenyl fed in snail doses nrodueed similar but more marked liter injury (see fig. 5, plate III). In large doses this compound was highly fatal. The liver ehon^es in animals dying, efter short exoosures vie re ineonsolcuous and consisted mainly of swelling, of cells and active regeneration (see fig. 4, plate III). However, animals removed from exposure before beinp' fatally WATER PCB-SD0000001108 -2 - poisoned, subsequently developed hyaline degeneration of liver cells similar to that produced by prolonrrd udmin lstrotlon of small doses of this compound. Thus tho results of the -recent study, as rail os certain field studios that hove boon mud (l) surest thot the solution of the in dustrial hazard Involved Is dependent largely on a reduction of the air concentration of those compounds to n level that will not oroduce liver damn re. The present experiments Indicate that lower sir con centrations must be obtained In the case of the more highly chlori nated naphthalene oomoounds and chlorinated diphenyl than for tricolor- D8phthalenes if a safe environment for workmen is to be assured, he- cuuse of the pronounced toxlo effect of snail doses of carbon tetra chloride on the 1 Ivors of an Louis already injured by czoosure to chlorinated naphthalenes and chlorinated diphenylIts use as e sol vent for thnee compounds vnuld apneor to be very bozardoun. ro 2/3/49 COMPANY CONFIDENTIAL TRAN 011**7 WATER PCB-SD0000001109