Document bBDmwbED4KnKEZNDqKVdkvjko

U. /: RSPORT NO. 2213 FINAL RSPORT ON ^ROCLCR D.VTa BOOK Job No. 171-451 Fil No. 141-27.1 April 27. 1948 R. s, KnUht Monsanto Chemicals K4 hONS 05M*' RIFORT NO. 8818 mtL REPORT OR THIS REPORT AND THE INFORMATION CONTAINED HEREIN IS THE PROPERTY OP THE MONSANTO CHEMICAL COMPANY. AHOCMR DATA BOCK Job Ro. 171-401 Fllo *0. 141-87.1 RI3XABCB DBPARTOBff - PH03PHAJg PIY13I0W - Anniatou, Alabus e*e*e***a******a Report sutaalttod - April 87, 1948 Chealata: A.M. Sllaaburc R.R. K&lgit Prepared bp: R Jt. KnlRit IlC&teea ooplas aara Bade of tblo report and distributed aa follora: . So. 1. Raaaarob rUa Ro. 8. 11. Jaaklaa - O.B. Dorsla Ro. S. R.8. Colo -R.S. Weatberly Ro. 4. W.T. Ourratt - P.P. LaSalle Ro. 8. 1,7. Weaver Ro. 8. CJl. Hoelmalt . Ro. 7. X.P. Ruokor Ro. 8. Sdgar 8. Hardy ' Bo. 9. J.y. Reerea Ro. 10. 7 J. Reevea Hp.ll. AJi. Zlleaburg Ho. U. Rjl. XBl#t . loi 18. Paul Lefia Ho. 14. P.O. Bealgaus Ro. 18. ' Ro. 16. Ro. 17. Ho. IB. Thla la aopy Ro. HONS 057948 nrsARGH DEPAimsifr - raoTPii.TE Dxrniar craaacAL comiTT Anniston, Alabama AROCLOS DATA BOOK (tautil informtloe on propartla a of Aroelore, Aroolor process data, uaaa of Aroolora, and physiological affaeta of Aroolora. Y0R3.I0HD Aa a aaana of praaantln; tba avallabla data on Aroolors to tha In- taraatad paraoanal within tha Kancanto organization, this looaalaaf notebook la being oorapllod. , Host of tha dots baa rasuited from nark carried out nlthln our on organization, literature references, bowersr, will be sited In all oaaaa throughout tha compilation In crder to alio* nora detailed lnfor- ntlon to be obtained by the user. . The following detailed outline Is for facilitating tba location of data in tha book and to saalat In properly Inserting new data sheets. Zaoh Aroolor is to be given a ssrles number for location under tha gsnordl headings. This sehaas at present la as follows: Aroolor 1231 100 series Aroolor 1333 300 series Aroolor 1343 900 series Aroolor 1348 400 series Aroolor 1394 - 900 series Aroolor 1340 - 400 series Aroolor 1343 700 series Aroolor 1368 a. 800 series Aroolor 1370 TOO ssrles . Aroolor 1371 - 1000 series Other Diphenyl Aroclors - 1100 ssrlss ' Aroolor 4448 - 1900 series Other .High Boiler Aroelors 3100 ssrlss ` Aroolor 9443 - 3400 Ssrlss Aroolor 8460 3900 series Aroolor 9468 * 3400 ssrlss Aroolor 9448 * 3700 ssrlss Aroolor 2949 3000 ssrlss Related Compounds - 4000 ssrlss HONS 057949 THIS REPORT AND THE INFORMATION CONTAINED HEREIN IS THE PROPERTY OF THE MONSANTO CHEMICAL COMPANY. to* page pertaining to the solubility of Aroolor 4465 In serious aolTants souId be of tblo type "IAj - 1900". In east* wbara the lnfornatlos for all Aroolora oan be ooisplled an ona sheet, aueh aa refraatlse lndlosa, the para will bo Inserted undar Mia general headli* and will bear only the Dunbar for tba flrat Aroclor, for exaapla, IAh - 100. i. onraui. mormrai or ;jiociaR3 A. Phyaloal Propartlaa ' (a) Oaaaral Phyaloal Constanta 1. formula and molecular nal#>t 2. 3paoIflostions for wanufaotura (b) Density and Tpeeifle (Parity (0) Oubleal Coafflaianta of Expansion , . (d) Taper Prossura and Rata of Ttraparatlon (a) 3poeifio Boat and Beat Capaalty (f) Theraal Conductlslty (g) Tlaooslty ' (b) Refraetlse index . . (1) Haata of Vaporisation - Other Theraodysamla Propartlaa (J) Soiubilltlaa (k) Plash and Pinna Points (1) Ulseellansoua B. llsotrloal Propartlaa (a) Dlalsotrlo Constanta (b) Poaor Taotare () Dlalsotrlo Strength (d) Volune HesistlTlty (a) Dlpola ltoanta (f) Klsoallaneoua 057950 0HS - 3- iz. methods or masctactohiA. Bonsunto Frossss X. ns* tutorials . 2. Chlorination 3. Olst Illation 4. storsgs an! Shipping . - B. Gsrmaa Froosaa 0. Othsr Proossaaa III. 03B3 OF A8WI/CR3 _ A. Elaotrloal Flsld X. Transfonmars . 2. Capasltcra 3. Coating for 7ir* 4. Otbssr nsss B. Tarnlahaa C. Plastiolsora D. Hydrsullo Fluid 3. Firs Rstardaats F. Boating nodluB l 0. HI ms11ansoua B. . Suggsstlona for as* Haas XT. HmiOLOOICAL KFTXT3 X. Skin Taata 8. ' Srstsastlo Tssts t^rsmn mmo /iroclcrs MOWS 057951 4 The book lo subjeot to revision and changes as various data ara looatad. Graphs and diagrams will bs lnsartad hsn possible sad saw graphs draan as Information la conplled. No ladlsaa of aaotlons la planned ut this tins, but later re visions my Include such pajree If the voltuee of lnfornutlon warrants It. Contributions of new sad supplementary data ara earnestly so licited. Any discrepancies la the existing data or advice aa to a batter Mans of presenting the lnfornstlon will be greatfully acknow- lsdgsd. Address all correspondence to tbs group leader in charge of the reaearoh on Aroclors at Phosphate Division - Research Department, Anniston, Alabana, R. R. Knight 12/8/4T HONS 057952 m u > STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON, ALABAMA Pm* n*. PRODUCT! _____ laai GRADE: nwalat CODE NO.: .mjaufUK. JSthoUBKIIi^ PROD. DEPT. NOj ----------------------- _______________ SUPERSEDES: BL7| A^**| 7,T,n,| T,A ^, APPROVED BY (Initial*) yi7AA. t.-:*-.*__________________ Control Specification Conranor Specification Crude /uroelor 11211 ip. Or. at 88*0, Aoiditr, ir;, nadVm. Aroolor 1221: Color Miaur. mt. Racii/ni. ip. Or. ot 6B/19.S*C. cniorln* ontoo* TlaaoaltT a* 100*F. 1.1904.160 ao,9 40 /iPHA aaz. 0.01 nax. 1.140-1 aso 20.3-21.5,: 30-41 *3 NOTES: Copied *r r* 4/8/46 HONS 057953  \X' t* ; STANDARD SPECIFICATION .............. OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON, ALABAMA Pa* N*. PRODUCT Aroolor 1238 CODE NO.! 1040-230-75-09 GRADE: . affd*r .... PROD. DEPT. NOj __________________________ SUPERSEDES: rwKiBtattTi 7F|R| 7ApB APPROVED BY (Initial*) 12-11-4* 12-IBU6 11-19-4* ig-ta-aa Control Specification Conramar Spodfication Orud* Aroalor nstt ip. Or. at Aaiaity, no. NaOR/ou Aroolor I2Si Color Aaldlty, w*. RoOH/m. 3p, dr. at B/.5*0. Chlorlaa bobtom nwoatty at 100*r, 1.*40-1.448 <.0.8 90 APII. nax. .01 MX, 1.235-1.840 31.5-83.9 44-49 SSI NOTES: Ooplad *r r* t HONS 057954 SIMTOMB) 3PS0 OTOATIOi 'W ipngMfto cHancAi cohabt Product: CUorUti Clnhiyl. ilrtlllil Q*d*i Aioolor 1248 1 Cod* Ho. 1040-840-73-09 D*t* Authcri**d Tan* 21. 1940 3np*r**d** 3p*oUlostIon Pt*d July a. 199* Tol*nU* Llalta Typical 7*In* 3p. Or. nt 68/18.8*0. Color, AOldlty, Kg* N0H/X TlMOalty *t S4.4*C. 1.SS8 to 1.348 0.5 Hkxlnua .01 Jfexlaua 4? to 80 3*ond* Oajtolt Cnitoraal W--* ty- * " wmd *7 Uhagy Approved tr Bobrt a. tottorlwd *1 0u^Zl UimtST Copl*4 8/ M 4/8/48 HONS 057955 <ammm aracmcmai . or ' MCWaMCTO CHBMXCrtl COtiPAHT . Produot; Chlorinate] Diphanrl. dlatillad Coda Bo. 1046-860-70-04 ammi Aroalor 1648; Data Aatfeorlsad Tuna n. IMP Siparaadaa Spaalfloatlon Datad Jklr 3. 1854 Tolarabla Haiti Typlaal taino 3p. dr. at 60/15.3*C Color, 1JP4. Aaldltjr, H&tHaC^ga Tlaoori.tr at 84.4*0. 1.404 to 1.414 69 to 76 Saeoata Saybolt Uaiaaraal Aroolor UK Dp. dr. at 90/lfl.8*C, Color, HJP.A. Aildltr, Kpt BaOR/ga, Tlaaoaltr at 96.9*0. 1.578-1.585 1.0 Aibaa .01 HaTtmia 66-100 90S Coda Ho. 1040-310-76-09 Approtad by A, B, Cartar x .. cElif(3E535f Asnrorad b id*. A. 0*1181. Jr. -------------- "fgEtKaagar Approved tf Kobrt So I--ttr; Authorlsad HI. H, Carothari '____ Chmdeil Diraetar Coplad Ip ra VS/46 0I*S StMCAHD 3P1CIFIC ,TXMI . or MoiraAino cHaucAL compact ' Produoti Aroolar 1254__________________________ Cod* Mo. lOiO-a80-75-09 Ond>i Dleleotrla Data Authorized 10/8/41 9operaodeai 6/81/40 Color, AIB4 3oalo . Coadltloa Speolfla Orarlty at <0/10.0*0 Aaldltr, M*. MOQB/Ok Inoroanla ChiorIdea, ppa. Sarbolt Tlaeoalty at 98.<*C, aao. Dloloatrla Ooaatant at 100*C RealatlTlty at 100*0, olaa-nai. at 000 valla RafraotlTa Index at 28 "C 01 atHllng Raaaa, Otaervad, 10# Obeerred, 009< Obaaraad, 90# Foot Foist . Malar, ppe. , Ivaparatlaa, 6 Hra. at 100*0 Oorroalon Toat-Chaaeo la aoliOit Aaldltr altar toot Inorganlo Chlorldaa __ after taat Coodltloa after fcoet Color ' after taat ' 100 Hex. Clear 1.490-1.000 .01 0.10 thx. 44.0-47.0 4.18-4.80 Above 000 X M* 1.6370-1.6090 800-805*0 800-364*0 364-878*0 8 to 14 88 hex. 0.4# 0.0# 0.01 0.10 Max. Clear ISO Ifcx. 8/11/44 HONS 057957 9'EmDAHD iwemoATiar cr 1CW3MIT0 BBMPAl COMBAT Produet: Aroolor I860 Cod* Ro. 1040-890-75-09 Oroda: Dleleetrlo__________ ________ D*t* Authorised iiAB/41 9upr**d**: 1/80/3* Color, An* 3oaio Condition Spoolflo Gravity st 90/18.8*0- Aaldlty, *01 BaOB/pa. Inorgenla Chlorldoo, ppn. Snytolt Tliaaelty at 98.9*0, aoo. Diolootrio Constant * 100*0 Resistivity at 100*0, ohkaa. at 900 volts Refreetlva Index at 88*0 Dlstlllla* Range, Obaarvod, 10$ Obasrvsd, 80$ Ohsarvad, 90$ Poor Foist DfetiPf pp* . Kvaporatlon, 6 Bra. at 100*0 Oarroados Teet-Ohange in might Aoidltr after test Znorgnia Chloride* after test Ocndltlon after teat Color after teat 100 tin. Clear 1.980-1,960 .01 0.10 Ikx. 78-60 8.6-B.8 Above 800 X 10* 1.6488--1.6**8 370-877*0 377-838*0 388-400*0 86-34 35 Iks. 00.*0$$ 0.01 0.10 Iks. Clear 180 Iks. ra 8/11/48 HONS 057958 aaciwcflnga icb soup wanajp ataman ___ "W1" imtiiim <. cmm acid no. HOLD HT l.Ms<H/te colon Si TOWi num WDB mu (moans UB 1269 1270 1271 TIMts to /allow 7stslllas poster . ' '.kits to grwr or U#t psllos crystallite poster TThlta crystallite US-160*C. 225-835*C. 286-300*C 0.06 Ihx. - . Practically whits Ugl* fluffy poster - ' . BOIRk go AF3A Htx. 904*0. Min. 68.0 TO.Si MGNS Copied My rs 4/8/48 u m ' STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON. ALABAMA pm* n*._____ PRODUCT: i^t----------------------CODE NO.: DATE ------ PROD. DEPT. NOj _____SUPERSEDES: ftai.SLJHi-- n,LJ.) P.I*| APPROVED BY (Initials) g.TM --* -- C.3.3.1 ____Ifl.ArfA--------------------- Control Coniumar Spedficabon Specification AjpenuN s Color, loftanla* Point /laid .luabar (UffiaOlVcfU) CqrstalUiitr clear, lipjit 7*1100, brittle raaln 2.0 rax. 60 - 66*0. 0 - .09B No, spaa. * Raisins aolor Unit to 2.0 nozlranm la raaomanftad beoauaa laspa*tloa raaorda show tint all lots produoed in 1944 bar* bod a aolor of 1.8$. NOTES: Coplai by r 4/8/48 HONS 057940 ' 3TAMDARD 3PBCinCATICW . <* 1PH3AHT0 CHEMICAL COHPAHT Product! Chlorinate Hlah Boiler Code Wo. 1040-480-78-09 (Sedai Aroalar 3480 Date Authorlead Boy 10. 1940 Sunereedea Specification Dated Deecofeer S3. 1931 Tolerable Limit Typical Tblne Appearance Color, H.P.A. Crystallinity Too* Softening Point, ASCII An Id Humber M0i NaOH/ga. Chlorine . . Clear, light pelloa, brittle realm 2.0 martlam To paaa teat 100 - 108.5*0. 0 - .05 89.0-80 .8)1 Approved bp A. B. derbar - Chier cheaiee Approved bp dr. A. O'Wealb Jr. Darke Manager AsDroved bv Robert 3. Weatherly. 9/8/40 Sales Mnagur Authorleed by 7. H. Carothere. SAO/40 Chanleal Director Copied bp re // HONS 057961 UonsMto Cbonleal Company Anniston, Alabans Aroclor Test Methods and DasignetIona 3peelflo Orarlty of Aroolora Total Chlorlna la Aroolora softening Point of Solid Aroolora Dotonlaatloa of Iren la Asoolor Tlaab and Tlaaa Polata Vlsooslty or Liquid Aroalcra Distillation Range of Aroolora ITraporatloa Toot of Llqald Aroolora Refractive lades of Uqnld Aroolora Resistivity of Liquid Aroolora Dlalootrlo Constant of Liquid Apoelers Aeld Huaber of Liquid Aroalor Color of Aroolor - HPa seals Color of Aroalor - APBA Seals Aoid takar of Solid Aroolora Pour Point of Liquid Aroolora Iaorepalo Chlorldaa la Aroolora Rater Content of Liquid Aroolora 14-10-48 14-15-48 14-17-48 14-81-46 14-84-48 14-89-48 14-51-48 14-58-48 14-84-48 14-35-48 14-96-48 14-48-48 14-43-48 14-44-48 .14-46-48 14-47-48 14-48-48 14-63-48 HONS 057962 Itanaanto Chonloal Company Ann1*ton Hathod Ho. 14-10-48 Spaslflo (frarlty of Aroolara Tha tanparatura at whloh tha crsTltlaa of liquid Aroolora ara takaa arlaa with tha Tlaooalty of tha liquid. Rota tha taqaratua at whloh tha eratlty la to ba takaa for tha Aroalor undar taat and haat tha aampla to 10*C. abora .that taaparaturo. Pour tha hot aampla Into tha ataaa or hot aatar jaekatod hydroaatar jar prowldad for thla taat. Stir wall with an aoaurata tharmoaatar and adjuat tha tonpontura to tha daalrad point by oontrolllnr tha ataam or hot watar faad to tbo Jaokot. Contlnua atlrrlng until tha tamparatura ramalna aonatant for half a lalnuta. Allow tha hydroaatar to oink Into tha liquid, than road tha hydroaatar Mala at tha point of tha lawar aanlaeua and raeord with tha taaparatura. Roport tha apaelfle entity to tha naaraat 0.001 unit. HONS 057963 * Monmb to Chemical Company Anniston Method Ho. 14-13-48 3CBI5CT; Total Chlorlna In Aroclara 1XTH0D: Volhard Titration follonlag Peroxide fusion Chlorlna In Aroalora nay bo datamlnod by fusion of tha sample with sodium paroxldo In a Burgesa-Parr fusion oup, extraetlnc tha fualon with water, aoldlfylmg tba aatar extras* with nltrlo acid, and nraalpltatlag tba ohlorlne by addition of an axoaaa of silver nltrata. Aftar filtration, tha axoaaa of silver nltrata la datamlnod by ti tration afplaat potaaalon thiocyanate, using farrlo ammonium anlfata aa lndloator. Apparatus Tha fualon oup uaad la tha 3urRWe-Parr sulfur Bomb Ho. 3 for flame Ignition. A land gasket la uaad. for Ignition, tha boab la auapandad through a 1-&A*" round kola In a 1/8" tranalta olata. Thla alloaa tha fualon oup to axtand through tba olata for about 9/8 inah. Ignition la affaetad by atrongly heating tha bottom of tha fualon oup with tba full flaaa of a Maker burner for two mlnutea. Tha boab, idakata, and tha sodium peroxide are obtained from tha Parr Inatruaant Coupany, Ubllne, Illlnola. Charan for fualon Tha fualon mixture la mada uji of about 19 grama (ona natal aeoop) of aodlua paroxldo and 0-3 gran* of finely powlered sane, sugar. Tha reagents should bo from from oblorlaa, or a blank run and corrected accordingly. Tha fualon mixture la mall mixed by plaela* tha Ingre dienta in a Mali glass atoppered bottle and shaking rigorously. A mesouring spoon for tba sugar la oonranlaat. SOLID AliOCLORl: Tha non-cryate 11Ids typa ara weighed In tha form of small pallets. Thaaa ara prepared by heating the Aroelor until a oonslatenoy la reaahad aa will permit dropping it from a pleas stirring, rod onto a tinned aurfaca (a ran top), oaoh drop forming a pallet. .{hen eool thaaa pelleta can bo roasted from tha aurfhee by lnaertlnn a spatula under thM. .4 grama ara naad. Tha pallata ara brushed Into tba bottom of tho fusion oup and tba fusion mixture placed on top of thM. After tltfOMlng the lid, tha charge la ready for fusion. Tha crystalline typa Aroalora ara welched lu tha powdered form. j4 jpama being uaad. They ara ebargad In tho same manner aa tha aon aryetaUlna typa. HONS 057964 . Total Chlorine la Aroelor* a LI'UID AHOCLOR3: .20 to .SO arena ara weighed by dro-rtng from a Stirring red onto a place of thin haulspherically shaped glass, or 1/2 rslntla eapaul (Oelatln Capaulsa No. 00. United Drug Company, Boatoa - 3t. Loula), whleh baa bean juat rravloualy tarad, and which rsraaloa oa the balaaea. It la aeeaaaary to heat the more vlaeoas Aroelora to "dropping" oonalateney. Tha plaoa Of glass than eaally alldaa off the bt-lanoe pea Into the fualoa oup. Oorar with the fualoa mixture.. The following quantities of a-bfila, auger, and AtflO, are uaed for the respective ohlorlne contents! 01 Cintent 0* - 30* 90* - 48* 48* - 88* 88* - 88* 88* - TO* Procedure ' weight of Sample O.S grams 0.3 prams 0.3 graas ' 0.8 wwna O.S grams . Amount sugar 0.8 g. 0.3 g. O.S g. O.S e. 0.3 g. AgHO, 80 nl. SO nl. so nl. 78 al, 100 al, Place the fualoa oup, ehleh oontalna the irenered sample aad fualon mixture, la the tranalte ifpiltlon plate aad apply the full flaae of the Ueker burner to the bottom of the fualoa oun for 2 minuter. (CAUTION: Do not atand too near the fualoa during Ignition. The uae of a aafaty ahleld la reoommandad.) Than raraora tha flame aad tool under the tap. ".Then eool remora sera* oap. Thorou^ily rlaae the oup oorar with water, collecting the rinsings la a olaaa 400 ml. beaker. Qian plane tha fUalon oup oa lta aide la the beaker and oorar with a matoh glass. 50-7 al. will be la the beaker from rinsing tha oap, and thle la auffleieat to deeoapoaa the charge. Renore the eup aad rlaae well. .1100 deeompoaltlon la aomplata, rinse off oorar-glass and add pure SO,, with stirring, until add la present In ezeeaa to the extant of about 10 ml. (About SO ml. of aold are retired.) Add axuetly 80, 78, or 100 ml. of standard sllrar nitrate solution from a plpat (depandlag upon chlorine present) and stir to effect coagulation of allrer nitrate preolpltate. filter with auction through an asbeetoe pad oa a 1-1A" perforatad poroalain plate aad wash beaker and filter 4 times with mail portions of 00Id rater. Allow the filter to drain 00aplataly batwaan waahlnoa. Transfer tha flltrata bask Into tha 400 al. beaker and rlnae. the flask twlos, addin.- tha rinsings to the beaker. Add S al. of ferrle Iron Indiestor to the solution and titrate with standard KCN3 solution until a distinct plak tint la Juat obtained. HONS 057945 Total Chlorine la Aroolors -3- Calculation of Chlorlaa Content 3ubtraet tba Toluaa of XCTC required fro* tha volume of KCH3 required to titrate the amount of atendard AgSOj solution used. This will f^vq the volume of KOI3 equivalent to the ohlorlne la the ample. kultlply the velum so Obtained by the ohlorlne value of each ml. of KDJI3 end divide by the weight of aam-'le talma. Vor example: If SO al. of ellvar nitrate solution Is equivalent to 61.4 al. of H0HS solution ead the value of 1 al. of KB1I0 solution Is .009770 gram 01; than If It Is found that 0.3 Tara of sample glows a non titration of 10.4 al. the percent of shitrine la: (61.4 - 10.4) X .003770 X 100 . 01 la oaaa the fusion mixture or other reagents sontain ehlorlaa. ths amount aust ha determined and deducted fraa the ohlorlne found. Solutions Required Standard AgN0( Solution: Dissolve 22 qrans of silver nitrate la eaah liter of mter. Proteet the solution from light. Standard XCN3 Solution: Dissolve 10 <-ram of KC1T3 in 1 liter of -rater. Forrlo Iron Indloator: Dae a saturated solution of ferric amonlum alum, about 90 g. per 100 ml. of wetor. Airs Hltrlo Aold: Stock sold suffices provided It la oolor}.saa. It can be boiled ln.a beaker until oolorlees'lf necessary using 600 al. BM03 and 900 ml. of 1^0. Standardization of solutions .'sigh 0.9 and 0.19 gram portions of pure dry HaCl into separate 600 ml. beakera. Add 200 ml. of dlatlllod aator to eaah and 10 al. of pure 50$ nltrlo sold, '.then solution la complete, add 90 ml. of standard AtfK)s solution from plpat. stir wall and filter through an aabsatoe ant on a perforated poroelala plate, uelng suetlon. Hash filter and transfer ths filtrate bask to the beaker la tba same manner aa when working with sarnie. Titrate tha filtrates with standard KCR3 solu tion, using ferric Iron indloator. The value of 90 ml. of AtfR* solution In tans of KCR3 solution la found by subtreating the ml. of XOT3 solution la titrating ths 0.9 gram of Had from twlos tbs numbsr of ml. of KCR3 solution used In titrating ths 0.19 gram of maCl. HONS 057966 Total Chlorine la Aroelcra -4> Thla value la aheoked by titrating SO al. of AffOs solution added to 400 al. of water and 10 nl. of pur# 50>i taos with KCtla solution. This tltratloa should agree Tory alossly (1 o.l nl.) with ths Talus found Aron ths tltratloa of MCI. The titration must ba ends slowly to avoid drainage error. 3loos pars IteCl aontalas 80.68,1 Cl by thsory, ths valua of ths KCR9 la tarns of shlorlna any ba found by dividing ths wslght of ahlorlna la ths MCI takan by tbs ml. of KCK3 squivulant to ths sllvar ultrata required. Inaaplsi Tno 0.3 graa portions of HsCl show KCN3 titrations of 13.11 and 13.13 al. ' . Tno 0.15 gran portions of MCI shoo KEK3 titrations of 37.18 and 37.14 al. Ths XBM3 aqulvalsnt to SO al. of AgHOg is than (37.18 37.14) 13.11 or Cl.4 al. By tltratloa of SO al. of ArftDg against KOn solution. It Is found ttat 41.36 al. ars required. This agrass within .04 nl. of ths valus obtalnsd Ann ths MCI titrations. Tha ahlorlna valus of ths XCIW Is thaa, .SOM X .3 dlvldad by 61.4 13.11 or .003770 grans 01 par nl. of K0H3. Tha ahlorlna valua any also ba ealsulatsd fron tha titration of 0.1S gran of HaCl. 0.8066 X .IS dlvldad by 61.4 - 37.16 rives .003770 grans 01, par al. of HOIS. Precautions 1. Ths fusion materials hava axploalva properties if handled Improperly; consequently ears nnst be takan to use safe proportions, to assure a good alxture free of large lumps, and to properly uoat the aovar of tha fusion sup. Tha fusion alxture naot be kept away from Tatar or anlat air, either of a) lah my Ignite tha ebarge. Tha fusion' Mixture should.not be ground to redues lumps. 1. The method as deeorlbed la not applloable to volatile orgsnia bosspounds unlsaa presentlone ere taken to avoid loan of sample daring neighing. Iffset of Tnrlnblns . 1. On eaeaunt of the high ohlcrlne eontent of may of the Aroelora and the mail amount of annuls taken, greet aoouraoy Is required In neighing, tronnfnr, and nixing of the sample. The plpet end burst for meenrlnr the standard anlutlonn mot bn very eleaa to avoid drainage errors. ' HONS 057947 Total Chlorine in Aroolors -3- 8. ration! whloh show hitok carbon daoosltaa on the oarer and side of tbo fualon oup aty or may not clw the full chlorine eontent. If a oarbon deposit la found, a aaeond fualon should be made ualnp a mailer aanpla or reducing tba amount of sugar in the ohsrgt or both. S. Tba temperature at which the standard solution! are standardised should bo noted. In ease roan temperatures vary from this tem perature , appropriate Toluae correctIons should be made. 4. The fusion misters materials should ba essentially free of stilorlne. f: a chlorine content may ha determined by netting a blank fualon, that la, without addition of aanpla, and titrating In the usoal may. rive ml. of AgHOg may ba added Instead of 90 ml. nortlona of AtffOg solution In llko rolunee of solution and nltrlo aeld. Hafereaoea Baamidi: Datemlnctlon of Organic Halogens, Xnd. Eng. Cham., Anal. Ed., 4^ 998 (1934). r.\B:a 1-89-49 Copied by rs 4/80/48 HOMS 057968 Monsanto Chanisal Ctr^wny Anniston llothod Ho. li-17-4G `3PBTB0T: IglMOOt softening Point of -Tolia Aroolqrg Ball nd Hlnn This method U a modification of the A.3.T.I:. standard method of taat for softening point of bltunlnoua materials, eerie1 designation: S 28-997. Tha nathod differs from tha standard method In that the rings are larger than spaelfled, a two ring supiort Is alao noad In order that tao teats may ha made simultaneously. Apparatus The apparatus oonslsts of ths following: (a) Two tapered brass rlnra, 8/8" lnalda dla. at bottom, 11/16" Inside diameter at top und 1/d" deep: thleknass of sail 3/33". (b) Tm atael balls, 3/B" diameter weighing 3.48 to 3.33 crane saoh. (o) a 800 ml. Qrlffln low form 'taker. (d) A ring support for tha too rings haring a brass elate exactly one Inch be low tha plate supporting tha ring, (a) A 300*0. A.3.T.K. low distilla tion thermometer graduated 1*0. Preparation of ths sample She sample shell be melted and stirred thoroughly, aroldlnr overheating or Incorporating air bubbles In the ness and than oourad into tha ring ao as to laara a alight assess on eoollng. 31nee the Aroalora shrink considerably on eoollng, the ring should ho 'tall filled, nearly to over flowing. A little of the sxooss should be drawn over tbs top of the ring at several point a ao aa to prevent tha eooled Arealv from dropping out of the ring. In the same way, tha seeond ring la filled with a standard Arotlcr of known softening paint. Ths standard .Vroolor ahould have a softening within at least 10 to 13*of the Aroolsr being tested. Ths rings while being filled should rest on s clean ean lid or on a brass plate which hea bean amalgamated to prevent the Arodor from ad hering to It. The Arodor in tbs rings should be fully cooled and hardened before proeadlng with tha taat. Prooadura " Add sod solution (savior water for softening point between 0-00*0, glycerin for betweae 80-200*0., mineral oil for above 200*C.) to tbs beaker until ths surfoee of tha solution la 2" above ths plate bolding the rings whan tha ring support la suspended in tha banker. Place the rings oontainlng the Aroolcr to be tested and tha etandard Aroolor on tha ring aipport. Pinos a ball am the oefltsr of the upper ourfaee of tha Arodor in saoh ring. Ouepead tha thermometer ao that tha bottom of the bulb la level with the bottom of tha rings and Just midway be tween tha two rlogs. HONS 057969 Softening Point of Tolld Aroelcrs - a PImo beaker < apparatus on a 6 laab round hot olate and haat at aueh a rata that ths tamparature 1* ralaad 5*C. each minute. The temperature rasordad by tba tbamomatar at tba Instant the Aroalor touabaa tba bottom plots la raportad as tha softening point. Ths hast ing la aontlnuad until both Aroslors bara dropped to the bottom -lata. HO oorreotlons are nada for saargsnt atom. Hot an 1. Iha standard Aroalor is run along with tha sample under test In order to ocnpensate for verlutlona la rata of tor,ting, dilution of glyoarln, and tharmonater variations. I. Tha softening point of tba standard sample is determined by making several determinations using fresh glyoarln and earefuily cheeking tha rlaa la tamparature of tba glycerin so that It Is as near as possible to B^C. per minute. 9. Tha glyoarln may be used repeatedly for tba tests after removal of tha Aroalor. 4. Bensol la used for cleaning tba rings and balls. B. '.star can bs used Instead of glycerin for softening points up to 90 *C. 6. rar softening points above 100*C, wall boiled glyoarln should be uaad. Tba usual glycerin la not satisfactory above 129 to 190*0, ' it bolls with loss ef water while tha temperature remains practi cally constant. It la nail to have a supnly of high-belling glyoarln on hand ta be used only for softsnlne points above 100*0. 7. Air bubbles oa tba rings and balls during the test should be avoided as far as posslbls. 8. Tbs rats of rise of temperature of tha glycerin shall ha uniform far aaeh mlnuta after tha first 9 minutes of heating and not averaged over tha period of tha teat. TAB:on 1-91-49 Oopled by ra 4/20/48 HONS 057970 Uoasaato Chetnloal Company Anniston Method Ho. 14-21-48 gQBJBCTi Determination of &un In Aroolara Iron in Aroolara may ba determined by extracting a benzol solution of (ha Aroolor with dilute bydroehlozlo aeld until further extreatIons shoe no' appreciable Iron content, rhe iron la the oonblned aztraeta le then .determined by dlohroaate titration. Procedure Transfer 3-10 grans of sanpla to a olean separatory funnel of about ISO ml. oopaolty. Add about SO ml. of benzol and shake until the sample la la solution. Shan solution Is oonplete, add 10 ml. of 1:1 Iron-free BB1 and rtiaks for about 2 minutes. 1st stand until aoperation of the teo layers Is soaplets, than dree off and preserve the aeld extract. Add anothar 10 ml. of 111 BB1 and abaks again. Dree off tha aeld layer end combine with the first extract. Condole until HC1 layer Is clear. Determine tha Iron by usual dlehronete titration method. - PABiea 1-31-48 Copied by rs 4/81/48 MONS 057971 Monsanto Chenloal Coopeny Anniston Method Ho. 14-24-48 JUBJBOT; Tinoh end flame Points mmUDi Cleveland Open Cup The flush sad flame points of Aroolor shall bs dstsmlasd la ths . Cleveland Opsa Cup Tester, following ths proosdurs dsssrlbsd la ASItl' v D 92-33. Apparatus Ths sup shall ba supported by a natal plats 1/4" (.638 on) la thlok- nsss sad 6 lashes (18.24 am) la width. Tbs plats shall bs of brass, east Iron, nroagit Iron, or stssl. Xh ths eontsr of ths ilate tiara shall bs plans dejreseloa 1/32" (.079 on) la depth, sad of Just sufflslsot diameter to fit sup. Thera shall be a elreuler opening 8 3/16" (8.80 ea) la dlaostor, out thru the plate, centerlnr with tbs ' Mater of ths above mentioned depression. The plate'shall be covered with a sheet of hard asbestos board 1/4" la tblekaesa, and of tbs sane shape as the aetal plate. There ahell be cut In the center of the as bestos board a circular hols just flttlnc ths sup. Heat may be bapnllsd from any convenient source. The use of a res burner, eleotrIs heater, or alcohol leap la permitted, but under no olrcumstances are products of atm- bustlod or free flams allowed to oone up around the sup. Ths souroe of hast shall bs centered under ths opening In the plate and shall be of a type that will not produce local superheating. If a flaas heater Is used. It nay be protested from drafts or excessive radiation by any suitable type of shield, that does not project above the level of the upper surface of ths asbestos board. Ths thermometer shall oonfora to the requirements of thermometer Ho. 8. ('lee A3TU table of thermometers). . Procedure The thermometer shall be suspended or held In a vertloal position by any suitable devise, ths bottom of the bulb shall be 1/4 la. (.638 oa) from the bottom of the sup, aad above a point half way between the eenter and bask of the sup. Ths sup shall be filled with oil to be tested la suoh a aanner that ths top of ths aenlseus la exactly at ths filling lias at room temperature. The surfaee of the oil shall be free from bubbles. There shall be no oil above ths filling lias or outside of apparatus. The test flaas shall be approximately 8/32" (.897 oa) la diameter. The test flame ahell be applied ea tha temperature read am the thermo meter reeohee eeoh euoeeeelve 8*7 nark. The flame shall pass la a etreight lias, (or cm ths clrouafarenas of e olrele having a radius of at least 6 laehaa.) serose the oeater of the sup aad at right ancles to the diameter passing thru the thoxmaaeter. - The teat flame shell, sblle Teasing eoroes the eurfaoa of the oil, be la the plana of ths upper edge of tbs cup. The tins for the passage of ths teat fleae eoroes the sup shall be approxi mately 1 second. HONS 057972 flash and Flans Points -2 - The oil shall bs haatad at a rata not oxoaadlnr 30*F nar nlnuta tem perature rlas till a point Is rsaehad ai-iroxlmately 100*F below tha probabla flash point of tha oil. Thereafter tbs rata of haatlw shall bo dodraassd and for at laaat the last S0F bafors the flash point la raaohsd ths ruts shall bo not loss than 9*F. or mors than 11*F par minute. Ths flash point shall bs tslcan as ths temperature road on ths thsroonstar ahan a flash ap-vsars at any point on ths aurfaea of tha oil. Ths trus flash nnst not bo confused with a bluish halo rrhlah sonatinas surrounds ths tost flans. After determining ths flash point, tha besting shall bs oostlmsd at ths spsolflad rats of 9*7 to 11*T par nlnnts, and application of tho tost flaw shall ha nods at tlM apsolfled Intervals until ths oil 1unites sifd con tinues to burn for a period of at laaat five saaonds. The mathod of applioatloa of thn flame shall ha tha aana an for fladh point. Tha tanparatura road at ths tins of ths fleas application, which causes barnlap for a period of fire seconds or nore, shall be recordad as tha flaaa point. Ths flash point and flana point testa shall bs mads la a rooa or eon- partaoat free from air drafts. Tha operator shall avoid breathing over the surface of ths oil. It la dealnbls that tha roon or eonpert- nsnt sap bs darkened sufficiently so that tha flash nap be readily dis cernibis. . Hots Aroalors 1848, 1834, 1860, and hl~har ohlorlnatsd Aroelcrs do not have a dlstlnet flash or flana point below thslr boiling tempsraturea. TABson 1-86-43 . Copied by rs 4/81/48 HONS 057973 Monsanto Chsmieal Co^any Analaton Uethod Ho. 14-89-48 'AIBJUCTi Viscosity of Liquid Aroolcrs tnanaPi aayboit universal, ahem d 88-44 Tlseoslty la a maaaure of raalatasea to flow. It la aaasurad by tha time necessary for a ebosan volume to ba forced thru a tuba of chosen lancth and lntamal diameter. Bjr theory tha viscosity of a fluid la ralatad to tha oversea dlatanoa betieen lta molecules and to thalr average apaad and thalr slza. Apparatus Vlsooslaetor assembly alth oil tuba, bath, rasaWar, thermometers, atralaar, timer, and plpat to Aaat all requirements of Agm 0 88-38. Tha vlasoslaeter now la aaa la aada by Kraba Klee. and Ufa. Co., New Tork, purchased fxoa Kail Orelnar Bo., thalr 8-tuba capaolty #888. Qua tuba - on laft hand - hat bean eert Iflad by tha Bureau of itaadarda Proaadura Tha Tlaaoataatar la aat up la aeoordanoe with manufacturers dlraotloaa ualag Ho. 80 motor oil for tha bath. Tha proaadura and Matted of reporting raaulta are thoaa daaorlbad under A3IH D 88-44. Cara of Apparataa Bath; At eouelualon of teat, opaa tha aoobaet pointa until 1 or 8 TaaEaa apart ao aa not to put undue atrela on thamostatlo control ahan bath ooola. Put a few dropa of oil la motor oupa oeoaaloaally. Heap outside of both wiped free of oil or Aroolar. Cover alth hoot whan not la uaa. Ualatala proper level of oil by oeoaalonal addltlona thru hole la front. 'Thu oil blaekaaa, dlonatle, elaaa heatera, tubaa, and arlflaaa, than refill with fresh oil. Oil Tuba: Mills still hot, move all possible Aroelor from gallery with plpat. Shea aoolad to 70-80*, fill tuba and aallery with beanos, drop thru orlfloa Into beaker, drain -ellery with plpat, rapaat with aaatoaa, and wipe dry with absorbent paper la suoh a "ay that flbara eaaaot full into tuba. Repeat until elaaa. Oooasloaally aover tha leather pluarer with sized thin paper (*eopy" MOHS OS 7974 Tlsoosltp of Liquid Aroelcrs - 2 - boot*) and swab walla of tuba barora using oleanliyr fluid. TUi kssps walls pollshad. Corar oil tubas with lids whan not In uas. Orlfloa.: orlfloa. foroops. olaan. Do not pass wlras, strings, bins oleanars, ate. thru tbs If a hair falls aerOds orlfloa, ra-iors with lone handls If tba orlfloa beeoosa oloeced, dismantle apparatus to Calibration Chaok tbs tlasr occasionally for 60 saoond uorlods. Chsok batb theraometsr froa tins to tlaa. Chaok performnoa of Tlseoalaetar osrlodloally bp running a refarenoo sampls of Azoolor on whloh eoroful dateralastIons bars boan made. Available for oallbratlon Is also an oil standard, eallsd "Alpha 46", of tba Amorloan Petroleum Isstltuts. Tbs oil la Obtalnad from tba Atlantia Raflnlnc Company, Philadelphia, PannsylTinla. Because sueh oil standards ars subjeot to obaage tbsy aro ohsekad annually. TAB:am 1-S1-48 Copied bp rs 4/81/48 IConsanto Chmloal Company Anniston Method Ho. 14-81-48 AIBJ.'WTi T)latllletlon Banre of Liquid Aroalara MBTOCDt A.3.T.H. D-30 with Bodlf lootlono Tho apparatus, consisting of flask, oonflonser tabs, shield, and ther mometer, la exactly tha aaao as dsaarlbad under A.3.T.M. tost WO 'Distillation of Bituminous Keterlels sultabla for Hoad Treatment". Attaob a 6 lnoh auxiliary thermometer (0 - 190*C.) to distillation thermometer. Plata bolt half Tty bstnaan top of sork and probable average of distillation ranna. Corsr both tharaonatars with a 3/4" dlanatar glass tuba to lnsura a uniform temperature aorraetlon for tha expoaad ataa, barometric praaaura and thermometer arror. Tha prosadurs la ohucad only to tha extent that thermometer readings ara takan whan apaalflad pereeatagse (usually ID, 90, and 90fc) of Aroolor hata baan diatlllad lnataad of followin'; tha a.t.TJ:. proce dure of weighing tha dlatlllata batwaan apaalflad thermometer reading. In tasting liquid Aroolara, 100 ;wu. of aaapla ara welched Into tha distilling flask and dlatlllata roeelvad In a tarad flask or bsakar resting on pan of a Torsion balanos with 100 gre seals. Proaadnra ' /sigh out 100 grama of aampla Into tha distilling flask. Assaahla apparatus as dsaarlbad under A.3.T4I. D-SO. Insert tharmoaatar (A.T.TJI. high distilling 0 - 400*0.) thru ocrk In tha naek of tha flaak so that tha top of the bulb la level with tha Iowaat point of juncture of tha tabulators and naek of tha flaak. Apply haat to tha flaak supported on two sheets of SO meah wire puss ao that tha first drop oonee over in from 9 to 19 alnutes. . Cpnduat distillation at rata of SO to 70 drops par mints. Colleet distillate la a 890 ml. beaker tared on a balanos. toko temperaturn rsadlncB at 1*. 3f, 9*. 1051, SO*. SO*. 40, 80. 60, TO!'.. 00?, 90?, 93',:, 98?, 94?, 97*. and dry. Corrections for emergent atan and praaaura are applied to the thermo meter readings if required. Taka eorreetlon readings at first drop, 10?, 90?, 90)1, and dry. Report tha temperatures to the nsere at i*C. example: (Hzposed atom In degrees) X (tamparatura difference In dagraaa) X 0.00019S - degrees stem aorraetlon - Tj,. The exposed eten la read from tha top of tha cork. The tamparatura difference la the reeding of tho thermometer nine tha temperature of the auxiliary thermometer. HONS 057976 Dlatlllatlon Raafa of Llipild Aroelora - 2 - 0.00018 A k m baroaatrle oormotion Tfc nomal boiling point la dograoa abbolata; A jf obaara la praaaura fron 780 an. Kg. - Ttao oorraatlon la addod it baroaatar la boloa nomal and aabtmatod If tho baroawtar la aboaa nomal. (UaoOounall - "fhamodjraaaloa aad Ohaalatery* pp. 119). Corrootad Tempantura Obaarred taaparatura ritTg. VABtm 1-89-40 Coplad by ra 4/28/48 057977 HONS Monsanto Chenloal Company Annleton Method No. 14-38-48 'JPBJTCT; Evaporation Test of Liquid Aroolora ECmoD: B Hours Heating ot 1QQC. A3B* D6-39T - Modified Procedure /let on a rough balance about 90 grans ( .9 gn.) of ths well raized Aroalor Into an accurately tarad tin box, 99 in. dla. X 99 ora. deep (3 os. 3111-stjrle olntnant box, deep pattern), fisher #1-980. Let stand until box and saapls ere ~t roan temperature, then weigh accu rately. Place the box In e ventllatad convection oven maintained at 100*C. 2 1* for S houre. Remora, cool In desiccator to room teraperature and accurately rawalgh. Prom the loas In weight calculate the evaporation In per cant. Report to aeoond deolnal plaoc only. Rotes 1. Bs sure box la at xooa temperature whenever exact weight la taken. 8. The oven abouXd not contain other samplaa which might Interfere with evaporation. 3. Because the evaporation loas la ceneltlve to temperature, the air bath must be closely maintained at 100*C. ' FAB: cm 1-29-40 . Copied by rs 4/83/48 HONS 057978 Monsanto Chenleal Conpany Anniston Method No. 14-04-48 . ' aPBJtCT; Refraotlse Index of Llaulfl iiwi. MsTHOD: Abba Rofreotoastsr ___________ BaftraatlTa Index Tha refrmotive index of any medium la defined aa ths ratio of the veloolty of light In air to tha veloolty of light la that nadloa. It la nsasurad by tbs ratio of ths alna of ths lnsldsnt angle to tha sins of tha angle of rsfraatlon. Tha danssr tha aadlun, tha -raster la tin rafraatlon toaard tha noxnal (higher refraetlv* ladaz). Baoausa ths refraetlve ladaz la oharaotarlstis of aash aubstanoa, it la uaaful in identifying liquids and verliying thalr purity. In datamlalng tha nelssular atruatara of organle oonpooads, and la sons quantitative analyaaa of alzturaa. Aa applied to Aroolor testae rafraatlra ladaz pro vides a verlfleatlon of ooapoaltlon and purity. Apparatus Abbs Hafraotonatar with aooaaaorlea, Bausoh and Laab, Cat. fSSBO, tsrlal Ro. 577. Calibratad to road dlraotly In tarns of rafraotlTa ladaz at ths D lias (sodium) at a tanporaturo of 20*0. Prooadura - Operators should bo fanlllar with tha Biuaeh and Laab "Directions for Bee* and prastlso tha aanlpulatlon as there dsaerlbad before attcnptlng dataxnlaatlons on Aroolor. Tha abridged dirsotIons boloa provide a sorting outline but at tha ozpaaso of onisalan of essential explanatory details whlah are soatalnad in ths B. and L. directions. Sores thaxnoneter Into Its eoeket In wntsr Jaoket of upper urine. Open prims and shank thalr ooadltlon. Clean If they ars soiled, atraakad, or spotted. 91th loser fixed print horlaontal, plaoa on It 8 or S drops of tha Aroolor fron a etlrrlag rod - sufflelant to fill tbs soaoea betsaan prises shen elanped together. Close prints and look with look not. Adjust ths lnatrunsnt and mirror to reflast shite light Into the refrao- tonatar. Ro apeta on air pookata should be visible. Oonneet water jeeksS to oouroe of ooaatont temperature voter, usually ths tap, aad poss eater until tha theneoMter has teen sonstent to 0 J*C. tot at least 9 alaatea at 89*C. Tha Aroolors flow norm easily at 89*C.t hsnsa tha oholes of this tanparatura. - With prlsna lUunlaatad, rotate tha prims by neons of ths Index mi until the border of the light aad dark fields passes sxaetly thru tbs Interaaotloa of the arose hairs. If ths border line is frln'-ed with oolor, rotate ths sonpsnaator until ths oolor disappears. If ths boua- MGNS 057979 Refraotlve Index of Liquid Aroolors - 8 - dorr la not sharp, adjust mirror until a diatlnet half shadow la ob- taiaad. If tha llaa or tha oroaa hairs ars blur rod, adjuat eyemleoe until a good fooua la Obtained. Secure final fine adjustment by means of tha alow notion aores. Road the refraotlve index, eatlmtInc to tha fourth deelmal mlaoa. If tha temperature of the water Jaokef la other than 89*0., oorreet to -3* by uaa of the.correction factor, * 0.00044 par *C. ms factor la applicable only to Aroolors 1848, 1894, 1860, and 1868. It was found by careful jceasureasat on each Aroalor thru tha ran,re 10' to 80*C Tha eorreotlon is subtraoted whan tha uorklnr tanparatura is below 89*C and added iriian above 89*0. ' Kxample: If tie rsfraotlTs index is found to be 1.6438 at 19*0., tha index oorraetad to 88*0. la 1.6488 - (10 X .00014) - 1.6978. Cara and Calibration of Instrument Immediately after uoa, clean the prints with swaba of pure cotton dipped in bensol, finally wiping dry with a soft olcth. Tha mrlwta, aspoolally tha upper one, tarnish sad scratch easily. Consequently ^eat ears mat bo taken In alaanlne. Before use tha prisma should always be inspected and reeleaned if necessary. 'Than not in uaa, tha refraetomster should be kept In its olossd ease. Tor practice or for ohscklnp srfarraanca, distilled water is useful. ;ater has a rwfraetive index of 1.3330 at 80*0., with temperature co efficient of 0.0001. A test piece of special pleas of known refractive index la supplied with the instrument for eallbratlon and adjustment If neoessary of the position of tho Index arm. Refract Its Index of Aroolors - Typloal Careful measurements at 83*0. have given the f ollowlnc typical valusa for Aroolors. Aroolar 1848 Aroalor 1854 Aroalor 1860 Aroolar 1862 1.6893 1.6376 1.6460 1.6668 Substantial departures (ever 0.0010) fron theca values should be in vestigated immediately as they - >f-correct - indicate substantial error in tha composition of tho Aroalor or contamination with other meter la la. FABiem 1-27-49 Copied by re 4/83/48 HONS 057980 Honsanto Chemloal Company Anniston Bethod No. 14-38-48 JCBJtCTi Haslatlvlty of liquid Aroalora ICTHCD: aaalatanee Hensursmomts between Conductors Appsrstus Uegohn Bridge: Oanaral Radio Conrmny Type 344B, AC oparatad - 800 volts, aarlal NO. 171. Tbla la a direct-currant Jhantstcne bridge for menstvl^ high resistances, brldga belance.belnr obtalaad thru usa of a vacuum tuba voltmeter. Range: 0.1 megohm to 10,000 megohms, covered by a dial and 9-poaltlorn nultlpllar saltoh. A raalatanea of 1,000,000 mecobas eaa ba dataatad. Taat lleotrodsa: Two aoneaatrle niekal cylinders (or braaa, alakal platad) with foot. Obtalaad from Raarai Sleetrie Company. Tba Lunar alaotroda baa outalda dlamatar of 2.8" and height of 3.89", with araa of 1B4 sq. on. Tba outer alaotroda hna laalda dlunatar of 3* and Ilka height of 3.23", with area of 198 aq. on. Tba dlatanea batwean alaetrodaa la therefora 0.1 Inch or 0.294 cm. By theory the alaotroda oonatant, area/ length, la 191/0.294 or 798 where 191 la the average area. Da praatlaa the oell oonatant supplied by Oanaral Slaetrle Company la uaad. For the alaetrodaa now In uaa, the call oonatant waa given aa 819. . Olaaa Plate: Pyrex, about 3-1/2" dlamatar with eoneantrle cxoovea to aaalat In spaaing the alaetrodaa. Obtained from Oanaral Klaotrla Colony. Oven: Oeaco-OeKhotsnaky drying oven with two holaa in book wall for por- oalaln tubaa for land wlrea. Holaa muat avoid oven hasting elements whlah oooupy 2" patha vartleally and horlaontally lnteraaotlng at tha eaotar of tha olroular wall. . Lead ".'Ires: Provide 900 ohm Amphenol twin oonduotcr eabla to eomaet tlia alaetrodaa la oven to tha posts of tha brldga. The nortlona amosad to ovan temperature are bared and than oovarad with noreelaln beads. Provide alao a flexible lead to ground tha brldga to a water pipe. Clean tha lauda, baada, and poroalaln tubes periodically. Aaeamhly of Taat Call Tha grooved glaaa pinto la placed In an 800 oo. baakar. Tha clean alae trodaa era plaoed in tha grooves of tha glaaa olate with the connsotor posta directly opposite In order to give tha widest possible sTeeing to raduoa aurfaoe oomhictlvlty. The eyllndera should bo very clone to equidistant. The apparatus should ba dried for 2 hours at 10O*C. before uaa. . Hast tha aanple to bo tasted to about 110*C. on a hot olata and sour Into tha alaotroda assembly until tha lsvel of tha liquid la 1/d to 1/g- above tha alaetrodaa. Cara wist ba used to make airs that tha MONS 057981 SUBJECT: Resistivity of Liquid Aroolor a - Page 8. I METHOD! P-ealatanos Measurements between Conductors lip of the container, front whloh the liquid is poured, la clean. Tilt the beaker In suoh Banner that all air bubblea In the Aroolor will rlee to tbe aurfaee. Air oool to 103*104*C. then without removing thermometer, transfer to the oven nhleh la maintained at 100*0. and oonnect the electrodes to the two flexible wires whloh lead to the megohm bridge. Then the Aroolor oooee to temperature (100*0.1, remove thermometer, cheek cen tering of eleetrodes, and proeede to measurements. Measurement with Megohm Bridge _' , Connect the two lead wires to the megohm bridge with the lead from the outer electrode-to the LU7 unknown post of the bridge; the inner elso- trode to the unknown post. Connect the CROUND post an tbe left side to a water pipe. Swing the spring eotmeotor. pivoted on the "0" poet, to the LO'./ poet. Connect the attachment oord to the 110 7 po.ier mipply. (1th the Aroolor at 10C*C., turn the oontrol knob (OTSX3IC-0FCn .TE-C!rj?CE) to the CHECK position. Throw all 3 snltohes at the rear of the Panel to ON. After Z minutes bring the galvanometer pointer to zero by means of the ZERO ADJUST knob. Thai turn the oontrol knob to CILiROE for one minute. Turn the mob to OPERATE and return the galvanometer pointer to zero by adjustment of the UILTIFIZ 3T switch and the megohm dial. Read after one minute. Re peat the CHARQK end OPBKATE positions for verification. The resistivity of tha Aroolor is the product of the "multiply by" reading times the dial reeding times the eleotrode constant. Report in units of 10? ohm cm, rounded off to two slgalfleant figures. Example: - "Multiply by" reeding: . Megohm dial reading Slsotrode Constant 100 9.4 mag. obms 819 cm Resistivity 100' X 9.4 X 819 - 4.4 X 10S meg. ohm em - 440 X 10 ohm on Values for resistivity ere qualified by deal gnatIon of temperature and voltage. These are 100"C. end 900 volts for tbs test above. Like con ditions are used at Plant B. . NONS 057982 3UBTBCT: Resistivity of Liquid Arociora - Paga 3 ii^TrtjOi Raalstanca r'eaaurevents betvieen Conductors Cara of Apparatus Tha "Operating Instructions", Oeeeral Radio Tom A38-B, idiich accompany the megohm bridge, raelta datolla of Installation, measurements, uaaa, and ooaatruotlon, llluatrated by figures and olroult and 'rtriiw dlecramaN0 attempt la mad* to raprodnoa auoh Information here. Tba operator ahould aoquslnt himself with tha eontenta of the 9.R. manual and refer to It for maintenance of tuba a and perta. '.'hen not In uaa the megohm bridge ahould be oloaad and atored In oablnet. Cleaning SlactradaJ - After tha aaaaurananta are made tha elaotrodas are removed from tba . tented liquid, and allo-md to drain until the liquid stops running from tha elaotrodas. .nils still hot they are Placed In a beaker filled with benzene under a wall van 11ated hood and allowed to cool. Then cool, tha elaotrodas Ora removed from the benzene and scrubbed with pondered trlaodlua phoapbata end a benzene earbontetraohlorlde mixture (SO-SO by volume). This scrubbing can be done with either a brush or the hands. Tha eleetredes are than rinsed idth acetone, followed by tap mter and than distilled "mtar. The elaotrodas ahould not ha touched by tha hands after tha aoatona Bash. After final rinsing tha slaotrodes are placed In on oven nt 120*0. for one hour or until they are used again. Tba glass spacer plates are elaanad and handled In the sens mnner aa the elaotrodas axoapt that they are wrapped in lan.pc paper before being plaoad la tha oven. Calibration Tor a rough ohask on tba condition of tha bridge, one or more cartridgetype rsslstaaoas of known approximate value Aould be kept on hand for periodla ar amorganay verification of tha meter ltaelf. ra 4/9/48 HONS 057983 Uonaanto Chemical Company Anniston Hethod No. 14-36--40 OTJBOTi Dielectric Constant of Liquid Aroolor NglHCDi Measured at 1QQC. and 1000 oyolea 30OP0 This method applies to alaoral olio and oil substitute used for tin luting purpoaaa. Apparatus Capaoltaaoo Bridge . Cathods Roy Noll Dsteotcr Oaalllator Constant Temperature Oan Variable Air Coadaaaor 1900 ss. Pyxcx Bsakar Conors1 Radio Co., Typo 71B-AN Cenaral Radio Co., typo 707-A Oensral Radio Co., Type 606-A Cenoo-OeXhotlnaky *(99000 Cenaral Radio Co., Type 334-T Prooadura Blaetrode and banker must ba claanad aa lirastad under "Cleaning Aiparatua tor Dlslaotrle Constant", and bo at 100*C. Haat Aroolor in the can to 109*C. Pour ovar electrode until plates and oaraalo Insulation are oorared. Connsot leads. 3tlr with tharmosMter outside oron until taaipsMtiira rsaehsa Ml"; place In ovan nhleh has boon oarefully adjusted to WO*C. At tbs tins aaaple Is plaeod la orea Its tsaparaturn Miould not hare fallen beloo 90*C. Connsot loads to eapaoltanoo bridge, obsarrlag that ths lead fron lnsulatad slda of condenser goes to Insulated tordinal on bridge. Balance bridge carefully according to direction under "Balancing Capaoltaaoo Bridge". Until Aroolor and area toapsraturea hare beoooa Identical the bridge balaaoa *111 constantly ahlft. After oean tenperature roaohaa 100*C., nslntaln bridge balanoo until no pronounsod shift is evident. Record reading of capacitance soale multiplied by multiplier setting. Dielectric Constant. Capaoltanoo In Aroolor at 100C. Capaeltanoa In air at 100*C. Balancing Capacitance Bridge Ooadeased procedure. Operator should read operating instruction for Bull Detector for complete details. 1. Connect to po*er supply leads to oscillator and nail detector, around the oscillator. 2. Turn on oscillator by pushing 9000 oba, 10 multiplier, 100 cycle frequency buttons. Adjust baraonle ontrol until oscillation begins as show by closing of sector In oathode ray tube. HONS 057964 Po #g . Dlelsetrio Constant of Liouid Aroolor - Tast 14-36-48 3. On null detector turn brilliance knob to aztrana laft, the foous knob to extreme right, gain eaitrol to extreme left, areas amplitude at ald-aoala position, tba sweep frequency switah on line aide. 4. Turn on power switch, lighting pilot llfdit. 3. -alt fifteen aeeonds, turn brllllanea knob to extreme right. 6. Adjust foeua and brilliance knobs until sharp fine line. 7. Connect external terminals on datsator to output terminals on oselllator. Switch sweep frequency to external side. 8. Gonnaet detector terminals of bridge to incut terminals of dstootor, taking ears that tha black wire (ground sirs) of tba lead goes to grounded terminal on both ends of lead. 9. Sat wain scntrol at mid-scale and scleotlrlty to extreme left. Turn sweep aaplltuda to extreme left, obtaining parties! line, '/lth 10. with turning oontrol knob obtain the caxlmn length of this line, keeping it always under 1/4 ineh with gain knob. 11. set sweep amplitude to extreme left. 12. set gain control to glee vertical straight line of about 3/8 inch. 13. Balanoe bridge .by adjustin'' power factor and oapaaltance dials until only a dot remeins on tha screen vhen tha gain oontrol is at extreme right. 14. Set sweep amplitude beyond mid-point, and slightly'dlsplaee the power-factor dial to obtain a tilted ellpse. 19. Adjust phase control until this ellipse elosec into a strelsbt line Inclined to the horizontal. 16. Bring power-faotor dial back to balance poaltlon, which should restore tha horizontal street line. Dlsplaee this oontrol the same amount In the opposite direction. This should cf^ln tilt the straight lino but in tha opposite direction. Adjust phase oontrol until there Is no tendency for.thla line to open up when it is swung 30 degrees from horizontal in both directions. 17.* Throughout these adjustments tha other bridge oontrol (the HONS 057985 Page #3 Dielectric Constant of Liquid nroolor - Teat 1 *-36-48 oapaeltaaes Dial) must ba la balaaoa poaltlon. If the alllpaa rrafi lially opaaa whan tha line la horizontal it may be brou"ht baok to the line agaIn by itaklcr alight ehangsa In thla eentrol. If oonfuslon reaulta, belanoe both eontrola asmIn na In (13) and renaat the sue- oeeding adjustments. _ Thla la the poaltlon of bridge balance: An alteiatlon of the power-factor control will tilt the line which doe a not open a ppree la bia thru an angle of 30* to the horizontal both ways; an alteration of the oapaeltanee dial opana the alllpaa but doee not change the inclination of the major axle. The apparatus any be left In thla balanced condition, turned off by aultchlng off flrat the brilliance Icncb of the dataotcr, than the power swlteh, than turning off the oac iliator. Por auccaaalTe aaaauramenta the oontrole are not ohanged, the apparntua left In adjustment. Than the folloalnr atapa define tho procedure: . 1. Connect all lands aa preciously directed Including that fro* null detector to bridge. 2. Tun on oscillator by bushing loo oyola frequency button. 3. Turn on null detector, wait IS seoonda then tun on catho'1 a ray tuba. Turn sweep amplitude to extrema left and adjust brilliance to obtain a fine yertloal line on aoreen. 4. Briar thla line to e dot by adjusting the two bridge controls. Initial adjwtaent is facilitated by having "Cain" oontrol to left. When final adjuatnant la obtained this knob met be at extreme right. 5. This dot remaining unchanged shows condition of brld-o belanoe. Cleaning Apparatus far Dielectric Constant The condenser la removed from tho tostod dloloetrlo and allowed to drain while at 111 In the oven at 100*0. The condanaar Is than placed, while still hot. In a bother of benzene under a wall ventilated hoed and allowed to ooel. It la than thoroughly washed with powdered trleodlua phoe|diate and a SO-SO alxttre of benzene end carbon tetraehlorlde followed by aa acetone rlnae. The operator should bo eery careful net to touob tho metal plates of the condenser .after this point. Tho oondansor Is then rinsed thoroughly with tap water followed by distilled water end dried on a dean paper in an oven at 120*0 for at least one hour or until It la again used. mb 3/1/48 HONS 057986 Monsanto Chemiool Conpany - Anniston Method Ho. 14-42-48 UBTDCT: Aald Wuabcr of !!.-,uia Aroclora tr.TUOD: Titration with Alkali using Phenol Hod Ooopc The Aold Nuabar is the weight In milligrams of sodium hydroxide re quired to nsutrallza ona gran of Afoolor to pH 7.6. It thus lnoludea any hydroohlorlo aeld, farrlo chloride, and other inorganic or or^anlo oonstltusnts having sold characteristics. It corresponds to tha Neu tralization nuabar of Aim Designation DIGS except that tha latter la sxpreaeed In term of ICQH lnatoad of NSOH and haa a aom-diat higher (phanolphthalaln) end point. Procedure To 100 al. of adjusted (pH 7.6) solvent containing Indleator slootly add 0.1 H NaQH dropwlse until the eolcr corresponds acnrozlmstaly to pB 7.6 when oonpared gainst a suitable referanoe solution. Readjust if necessary to Maintain pH 7.6. Add 90 gram (tig.) of Liquid Aroolcr and alz sell. Titrate Iron nlero buret with 0.01 It HaOB until the original red color of the solvent la restored. A portion of solvent la a similar container la a useful reference in determining tha and point. The natch is governed by estimation of the intensity of red because the hue is not exactly reproduced on acoount of the yellow color introduced by tha Axoclor. 1 *1. of 0.01 H HaflB 0.4 llgj. HatH. Calculate in tanas of Mga. NaCB per ge. of sample.** Report to 4 decimal places. "V-- t03r WJiaCB I fltj a 8. of aanpla gaon/iqi. Kxampls: If titration is 0.06 ml. for SO g. of Aroclor, tha Acid Number is 0.06 X 0.4/90 - 0.00064 Uga. NaOH/ga. Reoart as 0.0006. 3olutlcns Reoulred ' 3olvant I Mix 600 ml. of benzol. 200 ml. of 9-A alcohol and 300 ml. of acetone. Add 9 ml. of 0.2$ phenol red solution. Phenol Red Solution, 0.2$: To 0.1 mi. of dry indicator in a smSU. beaker add exactly 2.0 ml. of 0.1409 M HaOH. Stir to dissolve and dilute with 3-A alsohol to 90 ml. *~ Heferenoa Buffer pH 7.6: Dissolve 0.41 g. NaII,P04 and 0.99 trn. 9atHP04 (both anhydrous) in 100 ml. of water. Add 0.9 ml. of 0*2,. phenol red. Solution is used for reference in adjusting tha solvent if Lal'otta jB 7.6 color standard is not available. HONS 057987 Aold IfUMbor of Llijuld Aroelors - 2 - Standard 0.01 If Ha! 5 Ml. of .5 If NaOH to 290 ml. ni, of 3-A al- oobol. Protaot" at all tlaas froo atmoanbarlo 00a. . Soto ' By ualn* 290 al. aootons la aolTont lastood of 200 ml. a 100 9a. aaapla of 1294 aay bo takon for analyala. lUia 1-30-49 Coplod by ra 4/23/48, MONS 057928 Ucnaanto Chemloal Company Annlatoe Method Ho. 14-43-48 gPBTBCft Color of Aroolor on N.P.A. Teala iriTIICD; Halllne Poe'jat Comparator Tha mathod la applloabla to Aroelara 4463, 3460, or othara having H.P.A. oolora In tha ranee 1 to 5. Procadara '.'.'aim tha Aroolor la necessary to obtain pouring oonaiatenoy. rill tha taat oup of tha Halilna Pookat Comparator, Model 60S, with Aroolor, lnaart aup In tha oomparetdr, and oompara against tha oolor dlaa (No. 620O-80, Lutrloatlng oils and Patrolatum) whloh baa N.P.A. oolora from l to 8 in ooa-half atapa, Raport color to naareat 1/4. Claan tha taat aup with a mixture of CCI4 and benzol, with final rlnsa of bonzol. ACO: oolor nuabara eolnolda with National Petroleum Aoaoelatlon oolor aunber (1918). The relation of tha B.P.A. oolor numbers to othar oolor aoalaa la tabulated below: NPA Color Roa. (191B) 1/* 1/8 3/4 1 1-1/8 8 8-1/8 3 3 -V* 4 4-1/8 8 6 r 6 NPA Nhmea Onion Petroleum Co. m m - `. Lily white Craam white Extra pale Extra laaon pole Lemon palw Extra orange Orange pole Pale Light Had Dork Had Claret Rad ' - m - 0 H I J K L l! N 0 P B AlTU Color Noa. Lomlbond Analyale Rad Tallow Blua 800 810 1180 am -a am - 1 0.18 1.8 0.60 8 8.8 8.8 4.6 3 6.9 3.8 9.4 4 14.0 4.8 81.0 8 38.0 6 60.0 7 60.0 B 166.0 0.6 1.1 1.7 8.4 8.0 86.0 87.0 33.0 48.0 50.0 36.0 93.0 60.0 106.0 64.0 - - - .58 .58 .88 1.80 - PABtea 1-86--AS Copied bp ra 4/87/46 HONS 057989 Monsanto Cbemlenl Company ' Anniston Bsthod No. 14-44-46 JOBJgCTi Color of "7stsr Tbits* Aroclors METIPD; Comparison sgslnst A.P.H.A, Coals loop* Ths method Is applloabla to Aroolora 1294, 1260, or otters having oolor loss than R.P.A. #1 ('v.'aUr onto"). A.PJ.A. standards Tbaso oolor standards ars add solutions of potasslun ehloroplatlnato and oobaltous ohlorlda. Tbs unit of oolor Is that jroduesd hr 1 of platlaua psr lltor, Ths ratio of oobalt to platinum nay bo varied If noooooarjr to mstoh ths boo. Bsoouso tho has of Aroolor 1294 and 1260 aaona boat natohod without oobalt, this has boon cnittsd In tho prepara tion described. Dissolve 1.249 g. of potassium ehlaroplatlnata (KsPtCl*) containing 0.9 g. of platinum In water with IDO ml. of oonoomtrated hjrdroehlorle sold. Ml dilute to 1 liter with distilled water. This solution has s color of BOO. Prepare standards from ID to 100 in steps of 10 by dllutlnr 1, 2, 3 ml. ate. of the above solution with distilled water to 90 ml. In standard hlgt form Messier tubes. Protect ths tubes from evaporation. Refer to pare 13 of 'Standard Methods fbr the Sxamlnatlon of '.'ater and Sewage" elchth edition (1936) for details of standards containing oobalt. Published by Amerloan Public Health Association, 1790 Broadway, Row Tork. Procedure Pill a natehlng Ressler tube with Aroelor to a height equal to that In the standard tubas. Compare with standards by looking vertically downward through the tubes upon a white or mirrored surface placed at such an angle that light Is refleeted upward through the column of liquid. A color tube support (fisher #7-069, SO ml.) is convenient. Znamnueh as the proportions of the standard oolor solution in the compari son tubes are suoh as to rejresant an aliquot part of a liter, the readings are dlreot as parts per million. Colors up to 100 are recorded to the nearest 9. Direct eoaparlaoms are satisfactory up to 100. Above this ths sample should be diluted with Carbon tetrachloride (maxlaun A.P.H.A. color, 9), end ths oolor obtained to nearest 10 by multiplying by the dilution ' ratio. FABisa 1-30-49 ' Copied by rs 4/27/48 HONS 057990 KOaaanto Cbamleal Company ' Annlaton Method No. 14-46-48 TOBJBCT: Aold Umber of mild Aroelore ani HaTT Llculd Aroolor! METHOD: Titration with Alkali using Phsnolphthalsia Prooedurs Dissolve SO grama of the >^roolar In 50 ml. benzene In a 400 ml, bsaksr, naming to baataa aolntlon. Add SO al. 3A aloohol, 200 ml. distilled aatnr, haat to boiling, add 1/e ml. l phanolphthalaln aolntlon, and tltrata, In tba oaaa of tba dlatUlad Aroolora sltb 0.01 N aodlam hy droxide aolntlon, to a faint pink oolor nhlob la permanent for at laaat . tao mlnutaa aftar vigorous stirring. A reagent blank ahould ba ran soneurreatiy. Tba aaldlty of tba aanpla la oalanlatad aa mllllffam of aodlun bydroKlda required par gran aanpla. Caleulationa Using 0.01 H RaflH, Aold No. - ml. titration X 0.4/aamnla anight Tor SO i. ~ Aold No. (al. tit. - ml. blank) X 0.008 Ualng 0.1 N NhCH, Aold No. ml. titration X 4.0/samnla weight Tor SO o." Aold No. (ml. tit. - al. blank) X 0.08 Apparatna 10 aa. baratta In .08 dlrlalona. ConTaralona 1. To obtain Rautrallcatlon Sumbar in torna of xon, multiply tba Aald Rubber la taraa of KaCS by 1.408. Inraraa factor la 0.713. S. HaltInly tba Aold Rumbar by 1000 to obtain tba parti of NaOH re quired to neutralize oan million parta of Aroolor. Tbua Aold Hunker of 0.0008 la aqplvalsnt to 0.6 parta of RMB par million narta of Aroolor. 9. Tba larga amount of nafeu uaad oauaaa abarpu reparation of tba aqueous layar fron tba non-equeoui layor, tharaby maidup tba aadpolnt nora raally dlatlngulahabla. If tba titration la oarrlad out aalnat a vary light buokppround or la a flnoraaeaat light, tba and point la anally anon. 4. Aalda fron tree aold aa a oauaa for lhCH oonaunption, farrlo ohlorlda ahlab la uanally present In naall amount!, alao son aima RbOU la asutmllaatlon to phmolphtbalsln. It tbarafora follow* that an Arotlar of vary low aold number mat bo alao aztranaly ion la forrla ablorld*. TAB tan 1-8B-4B . Coplad by ra - 4/S7/48 HONS 057991 Monsanto Chemical Company Anniston Method No. 14-47-40 3DBJTOT! Pour Point of Haul4 Aroolori lamco; A.3.T.11. D-97-39 Tha pour point of an Aroolor la the lowest temperature at whloh tha matarlal will flow Han It la ehillad under certain preeorlhed aondltlona listed In A3TM D 97-99. Apparatus Apparntua eonalata of taat jar, thermometer, eork, jacket, disk, gaakst, and bath aa described undar A.~.T.1S. method 097-39. The thermometer la the A.3.T.H. Cloud and Four Test, ranee -38 to 30*0. Present eocaratua Is the Bull drainer Co. #CR 8834 single unit with Qr8848 test jar. Procedure for Aroclar Follow 097-99 In ell respecta except that tha centigrade seals Is eubstltutsd. Only on outline follows: Add 40 al. of Aroelcr to test jar. Adjust tharnonater to center of Jar with beginning of os plllery 1/8 Inch below surface of tha Aroolor. ','arn tha Aroolor without stirring to 46*C. Id a bath at 46-48*C. Cool to 38*C. In air or natsr bath at 89*C. Trans fer tha Jar to the jacket of the cooling bath which la maintained at 0 to 3*C. Beginning ut a temperatura 8 to 10 degress above the pour point, at each Interval of 8*0., remove the bast Jar from tha jacket and tilt Just enough to determine If there la movement of the Aroolor. This Inspection should not regilre more than 3 seoonds. '.man movement la not froaptly apparent, the taat jar should bo held la a hcrlacmtal position for exactly 3 seconds as noted by a stop watch. If movement occurs, lrcsedlately return tha taat Jar to tha jacket. Repeat test for flow at the next temperature 8*C. loner. Continue tha teat in steps of even degrees centipede (14,18,10, ate.) until tbs Arcelor dhows no movement whan the test Jar la bald horizontally for exactly 3 seoonds. This la tha solid point. Tha pour paint la tha previous temperature, 2*C. above tha solid point. Tha pour point la thus the loanat temperature at which tha liquid will flow or pour under tha teat conditions. Technicians must familiarize themselves with D97-39 which give# complete details of apparatus and procedure, reproducibility of resulta, affects of thermal history, ate, Tha directions above are Inadequate except aa a working outline. The bath temperature la controlled by adding dry lee to acetone for pour points below 0*C. FAB:am - 1-JO-48 Copied by rs - 4/87/48 HONS 057998 Monsanto Chenlonl Company Alulaton Method Xo. 14-48-48 JUBJfcCTt Tbs Testier of Aro'olors for Inorganic Chlorides MKIHOD:__________ Rcflulrsd standard ChiorIda solution! Dissolve 0.660 (Tarns of jura aodiun ehiorIds In aufflolant ester to nan aura exactly 900 nl.; l ml. than sontains 800 nloroerana Cl. Plpatta 29 al. of this oolutlon to a 900 *1. flaale and make to tha nark to give a 0.00119 X IfaCl solution, 1 al. of whloh oontalna 40 alorocTsme of 01. Preserve la a Pyrex hottla. Caution: Tha aatar uaad la prapartition must ha ohlorIda freo by tha Tyndall Bean tost; tha 0,00119 a solution should not bs kept over 1 month. Stiver Kltrata solution lOg: Dissolve 9 rrans of silver nltrata oryatala In 40 nl. of aatar and add 10 ml. of oonosntratad nitric acid. Ohlorlda ft*sa dlatlllad *ster. Apparatus Rsanlrad laVatts 10 nl. oolor tuhsa (13 an. X 100 m). Taat tuba mok with a black surface at tha baaa for unlfom conparlscn (Kota: so ara using black gasket rubber over tha entire board that sup ports the base of tost tubas during comparison.) Sox. About 7" long and 4" vide, nils box contains holes In top and notches In tha bottom to hold Lanotta color tubas. It la just hl<* enough to silos 1/4" of toot tabs to extend through the holot In the top. Tbs bon should bs painted a flat blaok on tha lnalda and on top and ahould oontoln enough holes to aoeamodate at lsaet seven tubes. Method Clean all flaaka, tubes, and plpettee to be used. Then rinse with dilute nltrlo said than with chloride free distilled eater. Add 90 nl. chloride trm eater to a 290 nl. Erlesnejrer flask, heat to boiling, add 800 gran of tbs Aroolor to bo tested, >*loh has bssn hasted to 100*0, shake rigorously for 1 minute, eool la cooling pan. Carefully dsoant sons of the eater extract to a separatory funnel. Test with pare ethyl ether (ohlorlda free). Transfer 10 al. of the other unshod extract to a 10 nl. lalbtte color tube after rinsing tube with portion of extract. Prepare standards by diluting exactly 9 ml. of the 0.00199 H NSC1 solution to 100 nl. la a XONS 057993 Tbs Tasting of Aroolora for Inorganic Chlorides - 2 - voluastrls flask. Qas nl. than oontalns 2 mlorogrens of Cl. Transfer 1, S, and 9 al. portions to 10 il. tubes, bki to the 10 ul. anrk with Cl free H,0. Plsoe standards sad sample la light fras boor from whleh only the top at tubas ara exposed add O.S nl. of tbe sllrar nitrate to sooh tuba oompere la a specially prepared test tuba raok. The eoaparlsoa Is to be neds quickly end from a eoaatant source of light, preferably day llfjit from a window away fro* the sunlight. Comparison la easier when other aouroes of light ara shielded froa the eoaparlsoa rack, look dlrootly Into tha top of the tubas and eoapara. Rota tbe known solution which most nearly fetches tbs star eztraet aatlMtlng to the nearest whoIs slotof^en. The extract blank end the distilled -tatar Should show no turbidity. Celeulet Ion DIt Ids tbs Ohioride oontoat in oleororrams of tha known solution whleh aetohas tbs extreot by tha weight of the Aroelor represented by the extraot to obtain tha chloride oontent of the Aroolor la p.ps. . In tha prooadure doscribed, tha 10 nl. extraot represents 40 'Tens of Aroalor (1/8 of 900 g. taken). Tha three known* contain 2, 4, aid S alerograaa of 01, thus represent lag 0.08, 0.10, and 0.18 p.pj, reapaatItaly. Taluaa should be reported to the nearest 0.028 ppa. Praeautlona Baeauaa of tha sensitivity of this teat, serious errors nay result through wary all(t eontaalaatlaa .or Inattention to details. All equlpaaat auat ha scrupulously cleansod, tha distilled water absolutely ohlorlde free and tooting dona away froa funsa of RBI or chlorine fuaaa. re 4/87/48 HONS 05TS74 Uonsanto Chamloal Coapany Anniston Method Ho. 14-03-48 amHTJWTi Utw Cont> of Liquid Aroolore MHIHCP: Titration with Karl Flasher Reagent Outline The Aroalor Is dlasolTed la a alxture of benoeno and aathaaol whlah baa baan titrated with Fleoher reagent to tha eharaetarlstle and point. Flsoher reagent la a aolutlen of lodlna, aulfur dloride, and pyridine, lodlna la eonauaad aa loon aa any watar la treaeot. Tha aolntlon la again tltratad to Obtain tha watar oontant lntroduood by tha Aroclor. Solutions and Apparatus Carl Flasher Reagent: Walgi Into a flaak 264 grans of pyridine, Barrott M or Bastnan Q44, and add 61 graaa of liquid or gaeeoua aulfur dioxide. Add tha liquid aulfur dlozlda dlreetly from tha inserted sylInter by attaching to tho outlat Taira a glass tuba extending Into tha pyridine. Sulfur dloslda gaa aan ba bubblad Into tha pyridine until proper aaotmt la addad. Store In a glaaa atopparad bottle. Trunafar 65.6 graaa of tha pyrldlne-SO* alzturo and 134 nl of abaoluto ethanol to a 1 liter Florenoe flaak. Oool thoroughly in an lea watar both. Add 16.9 grans at lodlna, stopper, oool again before shaking. Altarnataly tool and ewlrl until the lodlna la in aolutlen. TCakea 200 nl of reagent. Store la glaaa atopparad bottle, lot etand 84 houra before ualaf. Then fraah, one >1 of reagent la equivalent to about 0.0003 gaa. of water. Aroolar Solvent: Hlx 2 parta dry benzol with 1 part anhydreua aathaaol. The dry beniol la prepared by shaking the aoanarolal grade with anbydrowo oalelua ahlerlde, decanting Into a flaak and distilling, rejaetlag the flvat 10k< to eooe over. Coop In glaaa stoppered bottlea with nlnlwaa exposure to air. Hloro Burst: 10 m. x 0.06 ill. Cooh autonatlo with glass atopparad raaartolr. Xsk and nraba #8460. Equip reservoir with a no1stura guard tube oontalnlng Drlorlto or a alallar dehydrating agent. Proaaduro ' Beat a alean BOO nl. narrow south Erlenneyer flaak la an oven or on hot Plato until thoroughly dry. Sweep out for 10 alnutaa or until oool with air whlsh baa bean thoroughly dried by passing thru tubas eoatalalag 6 ap DrierIts. Disengage the flask fron the aaplratlag train and me diately aloes with a paper sap hold by a rubber band. HONS 057995 :/etor Content of Liquid Aroolora - 2 - lltbout delay, trenefsr 100 ml. of tba hansena-methanol solvent to tto flnok ton toall halo punctured into tto paper asp. Cover again with paper. Titrate at ones with Karl Flasher reagent to dietinet red-broen ana pout vhleh aoaa not fado after swirling aeveral tinea. The Flaohsr reagent la dispensed Tram the mlaroburet the tip of whleb projects Into the flaak thru the punoturs la tbs paper cap. At the end point any eater ocatant of the solvent baa bean roaoted. DuperImpose a fresh paper ean immediately. a Obtain weight of the solvent and nail-covered flaak on a T<rslon balenee ar equlvalmit. (JHokly lntroduoa with a dry pipette about 100 areas of the slightly earned Aroolor to bo teated. Cover at ones and weigh agrta to obtain tba ealebt of Aroolor to nearest gran. Shake until tbs Arcelor Is dissolved. If the mixture Is aloudy, earn slightly. If cloudiness persists another mixture should be prepared. Punoturs a snail hols In the paper oap for ths Insertion of the hurst tip ant titrate with Tlaohar reagent to the 1lrst definite brown eolor, agitating with a gentle swirling motion. The and point should persist through several swirls. The and point nay elowly fade thxou slow aoeesa of staoaphsrle moisture la whloh ease It Is rasterad by a drop or too of reagent. If not so restored, the end point may have been e false one or tbs oloaure Is faulty. A definite and point la impossible If bunld air la not nail sxdndsd. Fran tba amount of reagent required and the wslgit of Aroolor used, cal culate the water content In p.p.a. Calibration of yieoher Reagent and standard -fater Solution Standard water solution In methanol: Tranafar exaetly 0.40 ml. of water from a nloro buret or a 1 ml. measuring pipat to a 100 ml. volumetrla flask, rill to ths mixk at onoe with anhydrous methanol and nix. One nl. of solution than contains 4000 mlero-rams of rater in addition to a^ eater ahloh may to present in ths msthanol. Transfer exactly S ml. of ths above standard eater solution (equivalent to O.GB (pans of motor) to a 200 ml. Crlanneyer flaak which has bass dried and swept with dry air. Close with paper oap end titrate with Tlsoher reagent In the sene manner as the smipla. The sod point la sharp. A methanol blank, found by titrating 9 al. of the methanol used In wkliq; up the standard water eolation to a like and point, meat alraye be aubtraeted from this titration. Divide the amount of wator taken by the net Fischer reagent required to obtain the titer of tho Flaohar reagent la tarns of water. Dxaaple: A B ml. aliquot of standard solution, equivalent to 20,000 alororxams of water, required 6.S1 al. of Fleehar rea'-ent while 9 ml. HONS 057996 'later Content of Liquid Aroolon - 3 of the methanol required 0.99 of Fleeter reagent. 80,000/(6.61 - 0.95) - 60,000/6.06 " 3900 aleronrana enter/ml. Reoallbratlona: Baaansa the Flaohar reaent deterloretea rapidly, lta tltar met be determined for eeeh daya uaa. If tba aaae atandard eater aolntlon la uaad la reoallbratlon ae In the initial oallbratlon, the titer of the Flaohar reagent mat ba calculated from lta total eater content (lneludlnc that Introduced by the methanol). The total eater la the produot of the Initial rroaa titration and lta titer, Thle In the example above the total eater contact of a 9 tel. aliquot la 6.61 X 3300 - 31813 mlorograiu. If on reoallbratlon 7.37 nl. of Fleeter roecent la 81813/7.37 3960 niorogrema of eater per nl. Too or more oallbratioae ahould be made with agreement within 0.089 ml, Caleulatlon of B0 cample Standardization of Standard 8,0 aol. Titrate 9 ml. mixture ^0 aol. Titrate 9 nl. of methanol Tit of 3 nl. mixture * A Tit of 5 al. methanol S A - B nl. reagent for HgO added 3/100 of .4 Divide 8/100 x .4 by A - 8 faetor grama of HaO/nl. Multiply faetor X B giving maa. of H,0 in 9 ml. of methanol. Add thle et. of H,0 to .08 already addad giving H,0 in 9 ml. (Total) . 5---------- . *. 11,0 St'd Titration * Tj_ X aample Titration T, Tt X 1,000,000 ppm HpO et. aample TABson 1-87-49 Copied by re 4/87/48 HONS 057997 MiVTi.SIAL susara * Trow PBOPSHTICS or BASIC HH/Km* PBCBQCTS Letter to S.C.I'.yj.T.Bol^r (!hloaax Prodnot* Dit. .Union Carbide and Carbon Carp., SO I. Tarty-Second 3t., H.T. 17, B.T.). Letter datad Tab. 87, 1M8. Mo. 1000 . Bo. 1001 Bo. 1013 SO. 1014 Colors White to Palo Straw 'Tbits to Pala Telloa Pale Tallow Pels Tallow Pice Point Clod. AST!! Softening Point) dar. f. Liquid 194-801 ' 847-258 m~28S , S .eolf lc (iTSTity at 77 dap.. 7. 1.19 - 1.89 1.93-1.99 1.65-1.71 Prostration ("od. ASK) 200-e. load at 77 dee. 7. 10-19 5-8 8-8 7` jcoelty (Saybolt Unitareal Saeonda) 0iatIllation Ranga (ASTI) dan. 7. 33-37 at 77 da*. 7. 33-37 at 866 der,, 7. 31-35 at 866 deg.T. 33-87 at 80-590 600-660 &5-&6 308 dwe.f.' nsw--fs8 1 ish Point (AST!! Clavaland Opan Cup) dar. 7, 800 .884 356 398 P: rs Point (AST?.' Cl etaland Onan Cup) dae. 7. Fnter Factor at 1,000 oyolaa at 10* ayalaa i electric Constant at 1,000 eyclas at 10 cycles 0 C, Reeletltity (wee. ew.) at 30 den. C. 338 -- -- _ --. Rena to bolllne Less than 0,2f 0 43!! 3-6 5-6 Otar 107 - 10* Bona to bolllnn Laaa than 0.8/ 0.70? 4-5 4-5 Otar 107 - 10 Bona to TSsoUSui 001 0.70? 4-3 4-8 Otar 107-108 -- Copiad by arb 4/8/48 MOMS 0S7996 E I-A-B-4000 Prom ~ Hhlooax Product* DItlaIon Union Caxblda and Carbon Corporation SO last 42nd 3traat Now Tork 17, Raw Tork Latter - Vf.C Jl./P.If. Cola, Teeh. Rap. 2/16/48 Zyrox 300* (11-313) (gHEHAL IHPOBlt'.TIOR Color 3p. OraTlty Softenlnc Pt. Storaar Vlaeoaitp 3apbolt Parol Tlncoalty Panatration at 30*c. Panatratlon at 2S*C. Tlaafc Pt. Plra Pt. Caabuatlbllltp Praotura Acid Raalatanea Alkali Saalatanoa Volatility P.P. at 29*0. (1000 eyslaa) Dial. Oonatant at 25*0. (1000 oyolaa) DO RealatlTltP at 2S*C. - Brow - 1.40-1.45 at 25*C. - 79-85*0. - 59-89 at 130*C. - 79-180 at 130*0. - Approx. 15 (200 gm. load) - Laas than 3 (200 at. load) - Approx. 590*?. - Kona to 600*?. - 1111 not aupnort aonbuatloa - Oonoholdal - Kxoallant - Uxoallant - Araraga for 24 houra at 130*0. Laaa than 0.10 ag./aq.ca./hr. - Approx. .001 - Approx. 2.96 - Orar 108 mag. ema. Coplad bp ra 6/8/48 HONS 0579*9 Pron - Halonex Products Dlvlalon Union Carbide and Carbon Corporation 30 East 48nd Street Haw Tork 17, Raw Terk Letter - 7J.C.1l./J.E. Cols, Taeb. Rep. SAd/48 Zproz 3007 (11-308) ancRAL nmiahTiCB Color sp. Orsvlty Softening Pt. . Stornsr Viscosity aaybolt Purol Tlsocslty PanstratIon at 90 dog. C. Penetration at 29 doff- C. Plash Pt. Plro Pt. Combustibility Praeture Add Resistance Alkali Resistance . Volatility P.P. at 89 dag. 0. (1000 cycles) Dial. Constant at 89 dag. 0. (1000 oyolea) DC Resistivity at 89 dag. C. - Broun - 1.89 - 1.32 at 39 dag. C. - 69 - 70 deg. C. - 80-87 at 130 deg. C. - 20-30 at 130 deg. C. - Approx. 79 (90 g. load) - Less than 3 (800 g. load) - Approx. 930 dag. P. - Hons to 600 dag. P. - 7111 not support oambustion - Concholdal - Excellent - Exoallant - Average for 84 bra. at 130 deg. C. O.Sttng./aa.em./hr. - Approx. ,004 - Approx. 3.0 - Over 10 nag. ons. Copied by rs 4/8/48 HONS OS8000 00*-p-V-I Tia >vun ooo-p-v-i Iron: B.1.0.8. Final Rapt. B). 8(3 APPEHUU H. PHT3ICAL AID CHE3CAL raOPOlTICt OF CLDFHni OILS Pages 108 - 109 as quoted In I. Ge Furbsn* a salsa sheets) Proparty Ulophan A30 Clophen A40 Clophen ABO Clophen A60 Clophen A70 Clophen A80 Form .. ................................... Colour............................. ... ., 3Pacific Gravity at 20*0 .. Solidifying Point ................... Flash Point* ................... stirlaka.oo: ICC* - 30*0 .. 50* - 20*C .. 7i3C0slty at 100*0 .. 3cilinl'* Point Limit at 12mm. of liercury..................... .. Less during, ^.Taporation {after 6 hours at 100*C) Liquid Liquid nearly Nearly colourIsas colourless 1.35 1.48 -10*0 -5*0 166* 193* (Penalty - Hortons) 6* 3> 1.1*E 1.2*E 165 - 195* 180 - 215* o.oo>i 0.03" (Ijim. of Hercury for 100 hours) Ue4t Conductivity at 40*0 (In Calories par metre per per *C), Saponification Ho....................... <0.0092 0.093 0.0 -cjo.oos,: 0.091 0.0 Liquid Liquid nearly Hearly colourless colourless 1.53 1.68 12*c; 30*0 222* 236* In as open crueIbis 6-; 32 l.S*E 62 1.9*E Firm Firm, nearly crystalline Thlto colourless 1.7 1.72 - 1.77 50*C >160*C 240* 290* or -osar . (Pensky - Itartena) 5 - 6f, _ 3)5 - * 190 - 330* 193 - 25C* 200 - 235* 210 - 260* ' 0.082 <0.012 -to.0092 <0.0092 0.012 <0.0092 0.0 (2 hrs. at 125*) <0.0092 0.087 0.0 0.086 0.0 0.0 0.0 M Aeb . ......................................... .. Permittivity at 20*0 .. .. Ixaulatlon Resistance In 0hm.cn. 7. nail 6.0 <0.001 200k?/on. 1 X 1013 7. snail 5.4 <0.001 200CT/ora. 1 X ID13 7 roll 5.0 <0.001 > SOOCT/ojs. 1 X 1014 7. samll 7. small 4 - 4.5 3.0 <0.001 <0.001 > 200k7/era. _ >11 1014 >1 X 1014 7. small 3.0 - > 1 X 1014 L J* MOMS 058004 Clophors ere not combustible and do not aupnort uanbustlon of materials Into which thv are Impregnated. TABLE I Fron - United "States Patent 2,070,268 Patented February 9, 1937 Pa'-e 2 1-------2-------3-------4-------5 --6-------- Hydrocarbon compositions . Dlphenyl Dlstilled hlfji bolline CO-T.V- pounds Percent 0 0 80 eo 50 50 Percent L00 10C 20 20 50 50 Properties of dielectric Ohiorine content Percent 23*9 40.3 41.2 52.2 42.0 36.4 Viscosity sec. lay- bolt at 210* F. 3-i.Cifl* BTSTlty at 65*/65* C. 63 290 35.7 47.5 48.8 40.8 1.351 1.405 1.352 1.490 1.383 . 1.324 Dielectric constant 1C at 100* C. (1,000 cycles) 4.35 4.98 4.87 4.56 4.84 4.89 Properties of chlorinated diphenyl 7-------8-------- 100 100 0 54.0 0 42,0 46f0 34.0 1.523 1.380 4,30 4.80 i to Copied by re oOmo 2/2/48 emo t tx w C0 I 01 8 IW I-A (j) - 500 Stability of Orado P Hycnr and TafIon In Aroelor 1254 at 130*C and 45*C Short Form Depart Mo. 2179 File Mo. 141-27.1 . December 29, 1947 Notebook references: Smith 45137 Grade P Hyoar and Teflon Immersed In Aroelor 1254 Material Temp. Hours % Oaln in '.'t. % Gain In Thickness Orado P Hycnr Crude P Hyoar Teflon Teflon 130*0 45 *C 130*C 45*C 285 285 285 285 68.6 26.3 Negllftrib lo Negligible 26 6 tteffllfjtlble Negligible rs 1/14/48 MOMS 058006 I-A-l - 500 From - Memo P.C.B./R.L..T. 3/22/43 Aerovox Corporation Nan Bedford, Massachusetts Determining Fluoroscence In Aroclar "The ultraviolet light we uoe for determining fluoroscence In Aroclor is manufactured by Geor"o Oates and Company, Franklin Square, Loup. Xoland, New York. It Is a CB 4, 100 Jatt, C. E. Mazda Lump with filter. "Our procedure Is to pour a small amount of Aroclor Into a 5" watoh glass or a 5" Pyrex evaporating dish end observe for the degree of fluorescence under the CH 4 lamp, preferably Is a dark room. If the sample has been oontamlnated with Mineral Oil it will show up as a streaky or milky fluorescence as oompnred to pure Aroclor. The fluorescence around the menlacus of pure Aroclor Is not to be confusod with the fluorescence resulting from contamination. "This tost Is qualitative and, 09 such, is based on the experi ence of the person performing It. 'It keep a standard sample for comparison. If there arc any further Questions pleaae feel free to oonteot us". Copied by ra 4/2/48 HONS 058007 :n - 100 December 2, 1947 ELSCffilCAL DATA OW -ROCLORq Introduction Time haa not permitted ua to carry out electrical aeasuremente on all of the Aroelor samples sent by your laboratory and aa Hated In your letter to Dr. C. K. Bump of June 27, 1947, It wee believed that dielectric constant, Ions factor, and direct current resistivity measurement a over a temperature ranee for a Ion chlorinated and highly chlorinated biphenyl; also one sample each of the terphanyl and the mixed biphenyl and terphenyl serlea mould represent the electrical be havior of Aroolors. The trend of the electrical properties of the samples not measured oan be estimated; l.e, aa the viscosity of the Aroclors of a particu lar series Increases, the loss faotor will decrease and the loss faotor maximum (If within the temperature range measured) will be shifted to higher temperatures. An Increase In viscosity will Increase the resis tivity of the Aroelor. The dielectric constant of a material Is a mao sure of Its polarizability. Therefore, any change In the structure of the molecule which will Increase Its polarizability will cause an lacrosse In dielectric constant. Accuracy >f Data The accuracy of the alternating current data Is dependent on the dissipation factor of the dielectric at a particular frequency and a particular temperature. The dielectric constant values are acourate within .2# provided the dissipation factor Is lass than 10?,. The error Is greater with Increasing dissipation factor. Idle accuracy of loss factor (dielectric constant X dissipation factor) la also dependent on dissipation faotor. Aroelor 3442 was the only sample which had a dis sipation faotor greater than 10% and that occurred at the following conditions: 41*C, 300 cycles 41*0, 750 eyales 3S*C, 500 cycles It will be noted that the dielectric constants extrapolated to 100*C. ohoclc satisfactorily with the values listed In your letter to Dr. Bump. The direct current resistivity values have e 30)1 error for the greatest resistance reedInga on our instrument. Tor lower resistance values the error decreases. Aroclors 1221, 1254 showed an lnorease In resistance with time whioh la indicative of polarization effoots. Tor these matsrials then, resistance was read after the voltage was applied and then at the end of one minute - an emplrloal method used for taking e reudable value. Aroclors 4465 and 5442 did not show noticeable pola- MONS 058008 13 - 100 ' December 2, 1947 rlzation effects, even at the high temperatures. Data The dielectric constant of Aroclor 1221 and 1254 Is Independent of frequency. The dielectric constant of Aroclor 4465 and 5442 la alao Independent of frequency at the high temperatures. The 11quid-like properties of 4465 and 5442 disappear at the lower temperatures where a dispersion region becomes trident. It will be noticed that the dielectric constant curses (at the lower tempera tures) hare the seme order as those of the corresponding loss factor curves and the Inflection regions occur at the loss factor maxima tem peratures. The loss factor curves of 5442 at the higher temperatures show a sharp up-swlng, indicative of a large conductance component in the loss faotor. Similarly, the loss factor curves of 1221 and 1254 aeem to be In the conductance region. Aroclor 1221 showed an unusual sensitivity In changing loss factor values and as great an Insensitivity to change In dielectric constant. It was found that a sample measured initially at room temperature and measured at successively Increasing temperatures gave different loan faotor values when compared to measurements made with the initial tem perature high and than successively lowered. Results showed that raising the temperature of the liquid or allowing the material to stand in the open for long periods always lowered the loss factor, probably volatilizing the more conducting or the higi lose substances In ths Aroelor. Below SOOC oyclee this effect was vary noticeable, the diffe rences increasing with decreasing frequency. It may be mentioned here that loaa faotor measurements at low frequencies might possibly be used as an analytical tool or as a oontrol method of Indicating volatile sub stances contained In tha Aroelor 1200 series. The log, resistivity versus l/T graph Is useful as an Indication of the change that oooura In resistivity with temperature - or what la related, tha change In vlacoalty with temperature. Tha actual slopes of 4465 and 5442 cannot be assured sines there Should have been more measurements made at high temperatures. Hovjever these two Aroclora have a much larger viscosity-temperature coefficient than the other two plots. It la hoped that the enclosed raphs will summarize the dielectrlo properties of the Aroelors measured. Bore complete information or aoy queations concerning the data will be sent on request. eon/ Copied by rs 1/15/48 R. Levreault Monsanto Chemical Company Plastics Division Springfield, Massachusetts HONS 05*00* -i,, tivHrm'l'U*l'mww', oer*-. MONS 05*011 MONS 058012 II-B From - B.1.0.3. Final Report "o. 903 Item Noa. 1, 7, 22, and 31 Panoa 12, 13, 14. 15, 16, 4 17 XXI. CnLORXNiiTED DIPHENYL. 1. general. Chlorinated diphenyl la manufactured by I.B. Ferben under tne trade name of Clophan. 3one types are liquid and othera aolld at normal temperaturea. They are ueed aa tmpregnants aa alternatives to hydrocarbon olla end nexea. Clophan aharea with other chlorinated nnterlala a high permittivity end has the same dangers In handling, due to noxloua propertlea. In addition to the grades aulted to capacitor Impregnation, a grade known ns T64 la made by I.G. Ferben, suitable for tranaformor cooling. The total output of Clophan /V50 and A60 for the yeara 193Q and 1943 nas:- 1933Type A50 21 tana . " A60 132 " 1943 " A50 170 " " A60 506 " The coat of the material In Germany is:- Type A50 IK. 50pfg. to IK. 60pfg. per Kilogram * T64 1U. 20pfg. per Kilogram. The following la a list of the principal prewar oonaumera of Clophm:- Gionens-Gchuekert, Berlin. A.E.O. (Hydrewerk), Berlin. T.'loafll (Broun Boverl), Zurloh, Switzerland. Alathom, Porla. Duoatl, Milan, Italy. It wea stated that no German capacitor manufacturer uaea Clophen for the manufacture of smell capacitors far radio and telephone purposes and where these have been used by the Ger man fighting services they were supplied by the Italian firm, Ducatl. - 2, Manufacture. (1) The synthesis of diphenyl from benzene. Diphenyl la synthesised from benzene as shown In the figure, following:- ' HOMS 0$S0l3 i. -vwv-- Condenser Distilling Column 500-650*C 200*C Two-stage Heat Exchanger Reaction Coil> soo*c> 3ynthet;la of Diphenyl from Benzene The synthesis occurs In the vapour phase, at 800*0. and atmospheric pressure, in an electrically heated reaction coil of copper-manganese alloy. Ho catalyst la required. The apparatus, apart from the reaetlon coll, la of iron, uud operates at the temperutures shorn above, About 10,! of the benzene vapour is converted into diphenyl In one passage through the reaction coll. The purity of the benzene is of Importance for the elec trical quality of the ultimate chlorinated products and a specif lest Ion is attached overleaf. The benzene used was believed to oonteln 0,2 to 0.3 of paraffins but little definite Information could be obtained regarding any undesirable Impurities or the mechanism by whlah they cause poor electrical performance. Thiophene was stated to be definitely harmful, end vogue reference vs mode to "nltro-oampounds", to "aliphatic hydrocarbons" and to "substances which could not be chlorinated". The pre Isa nature of these materials was not known, but their absence wee ensured by obtaining bsnzsne always from suppliers whose product vies known to be satisfactory. Analytical Specification for Pure Benzene Appearonce; Clear end colourless. Density at 20*0.: 0.876 Distilling range: First 35! within 0.23*c. 5ft - 95,: " 0.25*0. 95-;: - end " 0.25*0. Solidification point: Dot less then 5*0. Bromine consumption: Tulphurlc acid test: Hot more than 0.5 gn. bromine per 100 c.c. Hot more than 0.15 0a, haCrgOT Carbon disulphide; Shall be free from C3g. HONS 05801A Difficulty In the synthesis was still belnr experienced, due to rapid corrosion of the copper-manganese reaction eoll, operatin': at 800*C. A smell scale experimental apparatus using a fusel silica coll had been made, but hod not been developed for production use. In addition to diphenyl, about 3% each of 1-3 and 1-4 terphenyls are produced by the process, These are se parated, chlorinated and used In sealing varnishes; present production Is about 4 tons per month.. Ho use Is made of ehlorterphenyls as paper lmpregnants, since the materials ere resinous and tend to crack; moreover the permittivities are loser than those of the ohlordlphenyls. The crude diphenyl Is next purified by distillation. During this process the terphenyls remain In the residue. They are extracted In the following msnner:- The residue is dissolved In hot benzene, filtered, and the 1-4 Isomer obtained by fractional crystallization. The crude product la distilled in vacua, yielding 1-4 terphanyl with melting point of 208*C. The 1-3 Isomer, remaining In solution In benzene. Is more difficult to Isolate. The solution Is clarified with activated char coal, filtered, und the benzene evaporated. The residue Is distilled to yield 1-3 terpbsnyl with imltlng point 80-84*C. (2) Chlorination of diphenyl. For the chlorination of diphenyl a lead lined vessel of 10,000 litres capacity Is used. It Is charged with 6000 kg. of diphenyl and 15 kg. of ferric chloride. The mix ture is heated to 110*0., agitated and chlorine passe:: in. The addition of chlorine Is continued for 100 hours at a rate of 130-135 kg/hour during which tin the tem perature Is raised gradually from 110*C. to 130*0. The and point of the chlorination la determined by measuring the density of the product. To remove hydrogen chloride formed in the process, dry air la blown through the liquid for 2 hours end this hy drogen chloride is recovered. The product is transferred to another vessel and treated with 1/251 of solid sodium hydroxide, heeted and agitated. The sodium hydroxide la allowed to settle out and the Clophen drown off from the top. transferred to another vessel to which Fuller's earth and soda are addad and the liquid redistilled. The stills for this process ere gee heated. HONS 058015 3. Properties. ' . (1) Capacitor lmprernatlag grades. A suiimury of the physical and chamlcal irooartlas of tha capacitor Impregnating grades of Clophsn la given In Appendix XI. Thors are six grades of capacitor lwpregnont, A33, A40, ate. up to A0O, the 3, 4, 5, aAc. Indi cating the number of chlorine radicals combined with the dlp'ienjl. Cash grade contains a proportion of the adja cent homologues not exceeding 20. Grade A30 has the highest value of permittivity. Theoretically the highest value obtainable with a chlorinated diphenyl is 9.0, and a grade having a permittivity of 7.0 has been prepared, but la chemically unstable, and very sensitive to moisture and Impurities. The most commonly used grades ere A30 end A60; A30 la tha most stable grads and has the lowest dielec tric loss. Grade A60 Is considered by 1.0. to ponsess the optimum oooblnatlon of non-lnflammablllty, stability and lsoosity. As with Nlbren, It Is considered that no addi tives are required since the substances are stable in use, provided that the capacitors are efficiently eealed against tho air. Klcufll of Zurich are the only users of A30 and A40. The following table shows tho variation In capacitance and power factor with temperature for a Clophsn Impregna ted paper capacitor. The lmprecnant Is ASO, tha dielectric Is Cchoeller and Hoeseh "A" flnlah rag tissue (density 1.2 - 1.29) with a thlokaese of 10 u; froquoney of measurement Is 000 e/e. Power faetor shows a maximum value of 0.0S2 at about 4*C, while eapaoltanoe falls off by soma 20# at temparotures below thle critical value. Variation In ct-pacltanca and powcr-factcr with temperature for a Clophsn-Impregnated capacitor. Temperature CC.) Relative Capacitance Porter factor -60 0.07 0.036 -40 0.91 0,024 -20 0.94 0.013 0 1.02 0.040 4 1.06 0.052 (max.) 20 1.10 0.006 40 1.10 0.005 60 1.10 0.004 00 1.11 0.005 No evidence was obtained from I.G. on the use of any type of additive tilth a view to depressing the temperature at which the ohongc of state occurs. HONS 052016 Tbs method adopted for evnluatln" the -.rater content In oils such as Clophen la described In Appendix III. It Is also applicable to such solids as Nlhren. Ettgelhardt stated that no source of failure had bean ex perienced during the nhsle period of production of Clo phen, whioh Is about 17 years. Consequently no improve ments or modifications had been made or found necessary during this period. (2) Transformer-cooling grade (Clophen T6d). No detailed Information *,tss sought on this material, since It Is unsuitable as a capacitor impregnent and is only used as a coolant for tranuformers and phase shifters. A sunaary of Its physical and chemical properties is given In Appendix 17. It has a lam viscosity, la moderately stable under electrical stresses and has the distinct ad vantage over mineral oil* of being non-inflammable. The principal users of this product are A.E.G. and llemans, but It la understood that, aa with other ehlorlnat-d eonpounds , eonservatlsm nnd prejudice among customers have prevented Its wider use. No stabilisers are added to the material aa their function of absorbing hydroehlcrte aeld would ha defeated by the formation of "ehlorldo salts", which In turn become elec trolysed. It was said to be vary Important to avoid con tamination of Clophen T64 which may occur In transit and for thla reason the use of leather for gaskets mist be avoided. 4. Methods of use, precautions, etc. No details were obtained on the method of Impregnation uaad by I.O. for the construction of tast-speolmena of Clophen-lmpregnuted capacitor. This mi partly eouaed by the nonappoarenee, after the first day, of Engelhardt, but It Is not oonslderad likely that any novel processes are Involved. Tot Information on the precautions neeassary In the usa of Clophen, see lection II, S, above. re 11/19/47 HONS OSdOU IH-A-b - 500 "'rora - B.I.0.9. Final Beport Wo, 893 Item Nos. 1, 7, 22 anil 31 Page xIt Clophen Is mala In seTeral grudea, which oorreopond closely with their 0.9. counterparts, A.50 being the grade most eonnonly used for capacitora. _ Except for very rare use by lemons and Ilolske for special orders, Clophan hea not bean used In Germany for small capacitors of the teleoonminloatlon typs, but It hca been usod extensively by 31enens-'chucksrt for power oapaeltors. It Is Interesting to note that the Carman forces used Clophen Impregnated and filled tubular capacitors made by Oueatl, of Ullan, who obtained the lityregnant from I.C. The prejudice against Clo phen mas, however, being gradually overcome and several manufacturers were contemplating an extended use of this material. Gome of them con sidered it to be equal to or possibly batter than mineral oil for opera tion at power frequencies. rs 11/24/47 HONS 058018 III-A-b-50 Prom - B.I.0,3. Pinal Report !fo, 893 Item Noe. 1, 7, 23, end 31 PaRea. 98, 99 (2) Clophen The only chlorinated lmpregaant used by "HemensSehnokert la Clophen, supplied by 1*0. In potter factor correction and high voltage applications It la consider ed practically Ideal, The only type of Clophen used In bulk is A.50, pentachlordiphenyl, (corresponding to Aroclor 1234). A.30 and A.40 have been tried and found unstable. A.60, A.70 end A.80 ure too viscous to allow for good Impregnation and have lower permittivities. Although the viscosity of A.50 at room temperature Is much greater than that of oil, the viscosity at impregnation temperature la sufficiently low to give no trouble in attaining thorough Impregnation. A routine cheek on conductivity la mode on each drum of Clophen, and formerly If the conductivity were too high, the Clophen was treated with powdered chalk to neutralise the free acid. As the result of continual pressure on I.G. over a period of years, the acid content had gra dually diminished, and It is now possible without chalk treatment to mcrk to the same rejection limit of resletlvlty as for oil, viz. 101 ohm.cm. at 20*C. Drums of Clophen felling to pass the conductivity test are returned to I.G., unless urgently needed. A certain elasticity la permissible in view of the hlgi standard act. Apart from conductivity, further acceptance checks are specific {parity (1.54-1,55) and permittivity (5.0 5.2). Permittivity Is measured at 800 cyclic and 20*C, on a Sobering bridge at low voltage. The acceptance standards for Clophen A.50 are shown graphically in Appendix XXXI7. Clophen costs about 1 E. 60 pfg./kg., and is therefore much dearer than oil (30 pfg./kg.). This extra expense Is offset, however, by the use of a special design whleh reduces the amount of Clophen required. An ad vantage claimed for this lmpregnant Is that Is has a similar permittivity to paper (vis. 5). Other lmpreppiants studied. As Clophen la considered nearly Ideal, no serious attempts have been made to find superior moterlals or addi tives, to Improve Its performance. This attitude is sup ported by service experience, In which no failures have been reported. It is realised, however, that on freezing discharges may occur In the contraction voids, whleh may result In decomposition of the Clophen and failure of the *0NS 058019 dielectric. Test3 were performed (see lection 17, 2, (3)) to check whether this depredation does In fact oecur, end no failure 3 noted. Nevertheless, I.G. supplied stall samples resembling Clophen A.50 but having a lower melting point so thut this possible source of failure e >uld be investigated. De pression of the temperature at which the dipoles beecme lntnoblle should raise the maxima usable frequency and hence broaden the range of applications by introducing tbose tor audio-frequency furnaces. Two of these I.O,. oatwleo, with references A.1621? and A.162N, are, like Clophen, made from benzene, but have a lower chlorine content because of the presence of an additional alkyl group (CQHgn+l), and hence a later density. Their advantage over Clophen A.50 Is that the setting point (i.e. tonpernture of maximum dispersion and of capacitance diminution) la lowered from -8*C. to -17*C. The permit tivity, viscosity and non-inflammnbllity resemble those of Clophen A.SO. The vlscoslty/temperoture curves of these two samples, R.7 mineral oil and Clophen A.50., are compared In Appendix XXX7. rs 11/19/47 HONS 056020 III-B-2500 December 22, 1947 TO: FHOOT.TE DIVISION ~AL1.-3ITOI UBJ; Arcelor S460 oe Used In Lthylcellulooe Lacquer RE: Federation of Paint and Varnish Production Clubs Official Digest (October, 1947). Aroelor# uaad aa plostlclzers and reaina Impart excellent qualities to atbylcellulose. Ethylcellulose la uaed in lacquers of yarlouo types, the ethylcallulose aotlng as a long chain polymer to Impart toughness and flexi bility and to Increase the speed of drying. .Soma of the principal uses for ethylcellulose lacquers are for the coating of high tension Ignition cable; heat seeling lacquers for foil and paper where the alight discoloration sdilch may develop in nitrocellulose lacquers on heat sealing Is not permissible; linoleum laoquere sbers alkali resistance la essential; textile printing; printing inks, particularly In multioolor designs where hydrocarbon aolvent does not soften or bleed Into previously printed designs; alroroft lacquer for resistance to both heat and cold and to ouick tempereturo ohangea; record lacquers, especially for home recorders; and In wood sealers where good sanding and flexibility are essential. A good plfjnented ethylcellulose leequer bus been mode, based oa the following fomuls: Ingredients Kthylcellulose H-22 Aroolor 9460 TiOg Menthylphenol Toluene Ethanol Rirta (by weight) 6,4 6.4 4.2 0.06 67.0 16.0 100.06 rh Copied by re 2/2/40 Benignus HONS 056021 II1-0-300 From - Memo c.T. Frankle/P.O. Ranimua torch 11, 1940 ' Soll-Polaan Concentrate Aa described below, the-.a materials are formulated Into a mater emulalflable aoll-polaon ooneantrata carrying almost 30 per cant by weight of uotlra Inuredlenta. Aroolor 1242 Trlohlorobenzene (llxed Isomera) Fenta eblorophenol Isopropyl alcohol Toluene or Xylene Oterox 3E* Santomerse 3 Paata 33.31,! 33.5 10.0 3.3 16.7 1.3 1.5 100. Of. * Other non-lonlo type emulalfyln.i amenta such as Triton NIC or 3pea and Tween oen be used to replace the 3terox 3E. Copied b;> ra 4/2/4S HONS 058022 Chemical Abstracts P031IBLR U'JE OF AHOCICRI Vol. 41 Page 6867 ni-H-io O.S.P. 2,425,973 to Anderson end Coalahan, (Hercules Fonder Company). Foundry eores sprayed with 1%' solution of ehlorlnat.ed naphthalene In hydrooarbon solvent sho-7 greater scratch resis *.tance than untreated cores. Cl2 content remains from 40 - 80/ 01 Particularly rood for use olth 1 castlnrs. rs 12/2/47 MONS 058023 17-10 Tram - B.I.fKS. Final lieport Ho. 893 Item Nos. 1, 7, 22 and 31 Pagos - 10 and 11 Mioli loaa trouble has naan experienced with efclordlohenyl than with ohlomaphtholena, probably because the former, balm?; liquid, In volves lass physical Contact In disposal. (2) Prevention. Very thorough washing of all areas of the skin likely to be ' contaminated with solid, liquid, or fumes has always been the basic prlnolple In prevention of skin troubles, and Is still looked uptn as-fundamental. Then fatty soaps ceaaed to be available, because of the di version of fats to food, It became essential to Insist upon the uae of barrier erearis, of which the best was one named "qjJIT.TBO", made at Tronmersdorf. 'Oils has now been repleoed, for lack of supplies, by an alternative made by I.O., named "JIITICAL*, which Is considered Inferior to 'ulmbo but satisfactory. The Flaaan firs, put up a special powder named "-'CHTFELKJLV'SH" to act as a barrier, but this was found to be Inefficient except to allay Irritation on skin areas exposed to fumes only. For this purpose It still finds use at Leverkusen and at the Hydravterke factory at 3erlln. A special point la .mode of fume extraction, and the minimum air speed away from the operator is 1 metro per second. TO cheek the efficiency of the preeeutIona, a thorough exami nation Is made every 4 weeks of every worker coming Into contact with chlorinated hydrocarbons, and sines ths enforcement of the precautions, no deaths or symptoms of internal Injury have occurred. lines superfatted soaps have cessed to be available, e cleansing composition containing llehlor-nethane has been devised. This Is so powerful a detergent for chlorinated materials that harrier craaras ara considered unnecessary, but It la uncomfortably Irritant to many skins. (3) Cure. .hen severe attaoka of ehloracne end Internal sickness were encountered, In ths early years, when the properties of chlorinated materials were not well understood, extensive rest periods had to be prescribed, together with a generous diet, entire absanea of further contamination, and long periods in the open. Tines precautions have been taken to minimise the effects, only a few mild cases of ehloresne hove been met. These have been traated with s solution of acetic end salicylic ectds in methylated spirits. MQNS 058024 -2 - (4) Conclusions and Recommendations. I.G. oonaldor that neither toxicity nor skin affection need now be eny deterrent to the uae of chlorinated naphthalene, and that ehlordlphenyl la If anything less troublesome. Certain people, notably those -1th fulr skins, show distinct ollorgy, end ore beet diverted to other work not lnvolvlnr contact. cerupulous cleanliness of the skin (Including the face, neck, and arms) and of the clothing (especially undergarmenta) Is essen tial and needs strict enforcement, '.'ashing with hot vjeter and good soap Is sufficient, so long as the soap Is superfatted,, since the skin bsoomes aenoltlvo to Irritation by alkali. Barrier cream should bs used on thoss parts of the skin wklsb ooat Into contact tilth solid or liquid material, and the arse of contoct should be minimised by the uaa of protective clothing and gloves where possible. Areas of the skin which ere contacted by fuaeo only, and particularly those ehafed by clothing (e.g. the nock adjuoent to the adga of the clothing) need protection by a suitable soothing powder. ",'hera fumes are generated, they should be drawn away from the operator at an air spaed of at loast 1 metre per seoond. It may ba found aasentlal to have two ducts, one at floor level end one overhead, with exhaust In two directions simultaneously. In ease the procautions are being, evaded, or last there should be soma ldlosysorasy, monthly medical Inspection la desirable. 11/24/47 HONS 058025 X7-B-100 From - The Journal of Industrial Hygiene and Toxicology Volume 20, number 2 February, 1938 I./0RPII0LOGICAL CH.1NGE3 IN TIE I.ITCliG OF ri.-Tl REVOLTING raOK EXTO3EHF TO CERTAIN CHLORmtTL'D HYDROOil)BOPT8 * Chlorinated hydrocarbons, particularly chlorinated neohthnlenes and ohlorlnuted diphenyl, have been used extenelTely In certain In dustries. Their use In the manufacture and preparation of many types of aleetrlcal equipment Is constantly Increasing. Although it Is known that some of these compounds cause acne, only recently has the possibility of more serlouo systemic effects been reoognlzed. The present paper describes the pathological changes observed in rote that had been exposed to furious chlorinated naphthalene com pounds and to chlorinated diphenyl. Compound 0 (chlorlnotod diphenyl) --as administered to two "roues of animals In low concentrations. An eforoee concentration of 0.37 rams, per cu. m. was employed 16 hours daily for 134 days In the first experiment. In the second experiment (employing an oferore air con centration of 0.93 mens, per cu. n.) the enlmale -ere exposed 8 hours dally for 143 days. The present experiments demonstrate that chlorinated noohthalene compounds and chlorinated diphenyl ara capablo of producing marked lifer damage In the Hhlte rut without demonstrable mlorosccolc shonpes appearing In the other orp,.na. Furthermore, the characteristics of the lifer lealons reaultlnr from comparable amounts of any "Ifen com pound are the same, regardless of the method of administration (Inha lation, feed Ins, or suboutaneoua Injection). Of the furious chlorinated hydrocarbons tested, oblorln ted di phenyl ftare erldenco of bolnq the most toxic, /hen administered by Inhalation In fery low concentrations (oforope 0.57 to 0.93 mrms. per cu. a.) lifer coll chunros '.vers fery pronounced uftor the first exposure period. The most striking change was tbs hyallnlzatlon of t the oell eytoplssm (seo f1r. 6, plate III). 3uch cellular alterations were essentially unchanged after a 2 month recovery period. In these animals small sublathal doses of surbon tetrachloride and alcohol uni formly produced extenelfe lifer necrosis and waa hie My fatal to them (fire. 1 and 2, plate VII). Chlorinated diphenyl fed In snail doses produced similar but more marked lifer Injury (see fir. 3, plate III). In large doses this compound was highly fetal. The lifer changes In animals dying after short exposures were lneonsoleuoua and consisted mainly of swelllnp. of cells and active regeneration (see fie. 4, plate XII) . llowerer, animals removed from exposure before being fatally HONS 058026 .. 2 polaoned, subsequently developed hyaline degeneration of liver celle elnller to that produced by prolonged u Aminlstrotion of snail doses of thle oonpound. - Thus the results of the present study, as ".'ell as certain field studies that hose been nude (1) surest that the solution of the in dustrial hazard Involved Is dependent lurpoly on a reduction of the sir concentration of these compounds to u level that villi not produce liver danope. The present experiments Indicate that loner air con centrations must be obtained In the esse of the more highly chlori nated naphthalene oomoounda and chlorinated dlohenyl than for trlehlor-. naphthnlenee If u aafa environment for workmen is to be assured. Be- cuuee of the pronounced toxlo effect of snail doses of carbon tetra chloride on the llvere of anlmuls already Injured by cxnosure to ' chlorinated naphthalenes and chlorinated diphenyl. Its use as s sol vent for these compounds would appear to be very hazardous. ra 2/3/48 MQNS 058027