Document zQRKOXZEVZN9Ya93nOGkXYxam

REFORT NO. 2215 FINAL REPORT 017 AROCLOnjJAT; BOOK Job No. 171-451 Fll No. Hl-27.1 April 37, 1948 R. R. KMrht RESEARCH DEPARTMENT Pfiotphcta Division __ hTTOOlT' ST22- I REPOST NO. 2210 FINAL REPORT OH AHOCLOR DATA BOOK Job No. 171-451 File No. 141-27.1 RESEARCH DEPARTMENT - PH03I&AHS DIVISION Anniston. Alabama a**************** comply. Report Submitted - April 27, 1948 Chemists: A.U, Ellenburg R.R. ltoldht Prepared by: R.R. Knl&t I sere mede of this report and distributed as follows: No. 1. Reaearoh File No. 2. R.L. Jenkins - C.B. Durgin No. 3. R.R. Cole - R.3. Weatherly No. 4. W.T. Durrett - F.P. LaBelle No. 0. H.F. Hearer No. 6. C.A. Hoebwalt No. 7. I.P. Rucker No. 8. Edgar B. Hardy No. 9. J.F. Reeres No. ID. J.F. Reeres No. 11. A.11. Ellenburg No. 12. RJt. Knl(d>t No. 13. Paul Logos No. 14. P.O. Benlgnus . No. 13. ' No. 16. No. 17. No. 18. This la oopy No. 7 HONS 058853 RESEARCH DEPARTMENT - HtOTPH.TT; DIVISION MONSANTO CHEMICAL COTiPAlJT Anniston, Alabama AROCLOR DATA BOOK Oensral I Information on properties of Aroolors, Aroolor process lata, uiea of Aroolors, and physiological effects of Aroolors. | TORBJOHD As a means of presenting the aveliable data on Aroolors to the in terested personnel within the Monsanto organization, this looseleaf notebook la being compiled. Most of the date has resulted from work carried out within our orm organization. Literature references, however, will be cited In all cases throughout the compilation In. order to allow more detailed Infor mation to be obtained by the user. The following detailed outline Is for facilitating the location of data In ths'book and to assist In properly Inserting new data sheets. Each Arooloir Is to be given a series number for location under ths general headings. This scherae at present Is as follow*] Aroolor 1221 - ! Aroolor 1232 | Aroolor 12*2 aroolor 12*8 Aroolor 1234 Aroolor 1260 Aroelor 1262' s Aroolor 1268 Aroolor 1870 Aroolor 1271 Othor Diphenyl Aroolors 100 series 200 sorles 500 series 400 series 300 series 600 series 700 series 800 series 900 series 1000 series 1100 series Aroolor 4465 - 1300 series 1 Otlher High Boiler Aroolors 2100 series 1 Aroelor 3442 - 2400 series Aroelor 5460 2500 series 1 Aroelor 5465 2600 series Aroelor 5468 * 2700 series Aroelor 2863 3000 series Related Compounds - 4000 serie a HONS 058854 THIS REPORT AND THE INFORMATION CONTAINED HEREIN IS THE PROPERTY OF THE MONSANTO CHEMICAL COMPANY. Tbs page pertaining to tho solubility of Aroelor 4465 In various solvents would be of this type "IAJ - 1500". In cases where the Infor mation for ell Aroalors oen be compiled on one sheet, such as refrac tive lndloea, the pare will be Inserted under the general heading and will beer orily the number for the first Aroelor, for example, lAh - 100. I. oeneUl woraiTisi of ;jiooi.or3 A. Phyaloal Properties (a) General Physical Constants i 1, Formula and molecular weight , | 2. Specifications for Manufacture b) Density and Specific Gravity e) Cubical Coefficients of Expansion (d) Vapor Pressure and Hate of Evaporation . a) Specific Koat and Heat Capaolty If) Thermal Conductivity is) Viscosity ihi Refraotlvs Index lio Roots of Vaporization - Other Thermodynamic Properties (3) Solubilities (k) Flash and Flame Points (l) Miscellaneous B. fcleotrloel Properties (a) Dielectric Constants (b) Power Faotors (o) Dleleotrle Strength (d) Volume Resistivity (e) Dipole Portents (f) Miscellaneous MCNS 058855 -3 II.METHODS OF HUTOFACTORK A. Monsanto Process 1. Dan Materials 2. Chlorination 3. Distillation 4. StoroRo and Chipping B. Carman Process C. Cthsr Procasses III. D3K3 OF AR00LCR3 - A. lleotrleel Field 1. Transformers ' Capacitors I, Coating for '71re Other usss B. Varnishes C. Plasticizers D. fydraullo Fluid 3. 1'lre Retardants F. Heating medium 0. Miscellaneous R. JuRgestlons for new Uses IV. PITTS [OLOOIC.U, Ery-CT3 1. 3kIn Tests 8. Systematic Tests PiT2ST:3 UlINO /JJ0CL0R3 HONS 058856 iniv ncrvn i flrtu I HE INFORMATION CONTAINED HEREIN IS THE PROPERTY Of THE MONSANTO CHEMICAL COMPANY. 4 Tbs book Is subjeot to revision and chances as various data ara located. Graphs end diagrams will be inserted when possible and new graphs drown as information is oomplled. No Indices of sections Is planned at this time, but later re visions may Include such pages If the volume of lnformutlon warrants It. I ' '. Contributions of new and sunplementary data era earnestly so licited. Any discrepancies In the existing data or advloe as to a .better means of present Inc the information will be grestfully acknow ledged, Address all correspondence to the group loader In ohargs of the resoaroh on Aroclors at Phosphate Division - Research Department, Anniston, Alabama. ' ! : R. R. Knight - i a,vi, I A. H. Ellsnburg r 12/8/4T l HONS 058857 i Pi... STANDARD SPECIFICATION OF Monsanto Chemical Company PH05PHATE DIVISION ANNISTON. ALABAMA Pag* No. PRODUCT! __ GRADE: _ ArooiQT1 iag.1 Haculur CODE NO.! 1040-CaarWTtifl. amt^oiFt *>1946 PROD. DEPT. NO.! .1 t!.K) J.T.U.I APPROVED BY (Initial.) lg-l?-46 13-1^5 r,A,9. Control Conaumar II Specification Specification Crufl* Aroolor 11311 ')p. 0!',. at 68*0, AelSJ.ty, nr,. NaO!l/rcn. Aroalor 12811 | Oolor _ Anidlty, m<;. Noai/pm. Tp, Or. ot 6B/l5,B0. Chlorine eintent Vlaaoolty tit 100F, 1.150-1.160 4L0.0- 40 aPTU max. 0.01 mix. 1,146-1.156 20.5^1.0,; 30-41 tOO NOTES: I Ooplat by ra i 4/8/46 | I HONS 058058 STANDARD SPECIFICATION OF Monsanto Chemical Company ' PHOSPHATE DIVISION ANNISTON, ALABAMA Page No. PRODUCT: __ GRADE: _ DATE Deeentar 4, 1448 AUTHORIZED: PROD. DEPT. APPROVED By (Initial*) .lg-17-46 1S-1B-4G 12-10-40 ia-19-48 Control Specification Consumer Specification 1.840-1.848 <-0.5 50 /LRU nail .01 an. 1,255-1.840 NOTES: Oopta 1? ra i a4//8b//4j0b . I M0NS 058859 STANDARD 3PE0iriCATI0W or M0N3AKT0 CHEMICAL COMPANY Produoti Qhloxjlaated Diphenyl. distilled Code No. 1040-840-73-09 Oiadei AroOlor 1848 Dot# Author1sad Juno 81. 19*0 Suparaedaa Specification Dated July 3, 1984 ' i' Tolerable Unite Typloal Value Sp. Or. at ^5/15.5*0. Color, N.P.A. Aoldlty, IM NaOH/sit. Vleooelty at 54.4*C. 1.338 to 1.348 0.8 Maximum .01 Maximum 47 to SO Seoonde Saybolt Universal Approved by Approved by A. B, Oerter Chief Chemist Bdw. A. O'Neal. Jr. Works Manager Approved by Robert 3, Weatherly SiTeeHan gar Authorised by T. N, Oarothe re__ ' Chenloal blreetor Oopled by re 4/8/48 . HONS 058860 i STANDARD SPECIFICATION OP 1IOH3ANTO CHEMICAL COtiPANT Produot i Chlorinated Diphenyl. distilled code No. io*o-aeo-7&-o Onto i Aroojor 1848 __________________ Date Authorised Tune 81. 1940 Superaedos SpeoIfloatlon Dated July 3, 193* Tolerable Limits Typical Value 3p. Or. at 60/X9.9*C. Color, N.PjL ' Aoldlty, Mgis HaOVst Vlsooslty ai 94.4*0. 1.404 to 1.414 0.5 Maximum .01 Maximum 69 to 76 Seoonda Daybolt UnlTeraal Aroolor 1262 Dp. Or. at iO/lB.5*C. Color, N.P.A. Aoldlty, Mg i NaOH/pn. Tleooslty ai 96.9*0. 1.972-1.90S 1.0 Maximum .01 Maximum 88-100 90S Code Ho. 1040-810-76-09 Approved by Robert 3. Weatherly ........... toies Banegar Authorised by J. N, Carothers Ohemloal Director HONS 058861 i ! Produoti Aroolor 1254 Qrodo; Dlejl^otrlo STANDARD SPECIFIC T10H or MPNaANTO CHEMICAL OOKPAWT Oode No. 1040-880-76-09 Date Authorized 10/3/41 Superaedea! 6/81/40 Color, AFHA 30il0 Condition 3poolflo Qravlty at 68/18.6*0 Acidity, Ugr>. NaOH/ot. Inorganic Chloride*, ppn. 3aybolt Viaooalty ot 98.9*0, mo. Oleleotrio Constant at 100*C Realatlvlty at 100*0, ohm-cm. at 600 volta Refraotlve Index at 26*0 Dlatllllns Ranee, Obaerved, 10* . ! Obaerved, 80* | Obaerved, 90* Pour Point 1 ' Water, ppa. | Bra. at 100*0 {evaporation, ( Corroalon Tealh-Change la iwlgbt Acidity 1 after teat' Inarcnnlo Onl<irldea after teat Condition F_after Coat . Color i[?ter teat 100 utx. Clear 1.493-1.608 .01 0.10 Max. 44.6-47.8 4.16-4.38 Above 800 X 10* 1.6370-1.6390 380-383*0 358-368*0 368-373*0 B to 18 35 Max. . *0.4* 00 0.01 0.10 Max. Clear 160 Ihx. 6/11/48 | i HONS 058862 sifthoard mnso memos or MONSANTO CHEMICAL COMPAKT Produot: Aroclor 1260 Orade: Dleltotrlo Coda Ho. 1040-290-75-09 Date Authorized 11/16/41 Superaedaa: 1/30/56 Oolor, APHA Soila Condition Specific Gravity at 90/13.8*0 Acidity, ligp. HaOH/pn. Inoreanlo Chlofldea, ppm. Sayto It Vlaooelty at 98.9*C, aeo. Dle.leotrlo Oonatent at 100*0 - . Reaietivlty at, 100*C, ohm-om. at 600 volte Refraotlve Indiut at 26*0 Distilling Ranee, Ohearred, 10$ Observed, 60$ | Obaerred, 90$ Pour Point ; Water, ppm. Evaporation, $ Hr*, at 100*C Oorroaion Teet-Ohange la weight Aoldity after teat Xnorganlo Chlorides after teat Oondltion I after teat Oolor ' a?ter teat 100 Max. Clear 1.550-1.660 .01 0.10 Max. 78-80 3.6-8.8 Above 600 X 10* 1.6455-1.6465 370-377*C 377-388*0 385-400*C 26-34 35 Hex. . $0.2 $ 00 0.01 0.10 Mix. Clear 180 Hex. ra 6/11/48 HONS 058863 1260 1289 1270 1271 aracracanoHs kb scop nigenup ahoclobs appearh*cs a ccam HOLD FOOT ACID DO. HgJtaaH/g* COLOR 5i T0HJEHS HELTHK} romr TOTAL CHIORIU TThlto to polio* oryctalllno powder '.Thite to crop or 11git polio* cryotalllno pondor TJhito cryotalllno ponder Practically obit* 11git tlnHy pondor 135-160*0. 0.05 Max. 225-255*0. 285-300*0 - 80 araa Uai. 80 AEHA HU. .- 304*C# Mia* - 69.5 70.5 Copied bp re 4/8/48 HONS 058864 rn < STANDARD SPECIFICATION OF Monsanto Chemical Company PHOSPHATE DIVISION ANNISTON, ALABAMA Page No. PRODUCT! _ Araclor 4460 (rtemlar) GRADE! _ CODE NO.: 10'KM30-TO-09 DATE AUTHORIZED! Ootober 4. 164 PROD. DEPT. NO.: APPROVED #Y (Initiali) ____ SUPERSEDES! *o 3, 1944 Il.V.'.t P.L.1 ll.3.'7.| P.A.B. 10-gwt 10-2-14 10-4--14________ Control Specification Coiuumar Specification Aprcareno* i ] ! Color, It,!' i, m >/ loftobln*. point {*!- 1,T,14,) | ,inl(! ihinbet (ffettaOI^fT!,) Crynt-aUlnlty closr, llr.'ht yallon, brittle resin 2,0 rx. 60 - 66*0. 0 - .WS Ho. spec. * Halnlntt palor limit to 2,0 maximum Is W'oomnenaed beoauso Inotwotlpn reoorflo ebon that all lota praluooC In 1944 have- bad a oalor of 1J>^, I i NOTES: i l Oopioe by rs! 4/6/40 : MONS 058865 STANDARD SPECIFICATICjj COT MONSANTO CHEMICAL COMPACT Pyaflugtt Chl,o|rlnated Hltth BoilerCode No. 10*0^460-78-09... _ flraa.t Aroo^lor 5460 i . Date Authorized Hay 10, 1940 Supersedes Specification Dated Deoeiriber 25, 1938 ! Tolerable .Liraits Typical Value Appearsnoe Color, N.P Crystalling ty Toat Softening Point, ASttM Acid Number Kgt NeO] Chlorln* Clear, light yellow, brittle resin 2.0 maximum To pass test 100 - 105.5*0. 0 - .05 53.0-80.6# Approved by A. B. Oerber Chief Chemist Approved by Bdw. A. O'Neel, Jr. Vlorks Manager Approved by Robert 3. Weatherly, 5/6/40 Seles Manager Authorized by J. N. Carothera, 5A0/4Q Chemleai Dlreetor Copied by re, 4/6/48 ; HONS 058866 Monsanto Chemical Company Anniston; Alabama Aroolor Test Methods and Designations 3peeiflo'Oravlty of Aroolors Total Chlorine in Aroolors Softening Point of Solid Aroolors Determination of Iron In Aroolor Flash and Flame Points Viscosity of Liquid Aroolors Distillation Bangs of Aroolors Rvoporstlon Toot of Liquid Aroolors Refraotlve Index of Liquid Aroolors . Resistivity of Liquid Aroolors Disleoti^io Constant of Liquid Aroolors Aold Humber of Liquid Aroolor Color of Aroolor - HPA soale Color of Aroolor - AISA Seale Aold Humber of Solid Aroolors Pour Point of Liquid Aroolors Xnorgnnie Chlorides in Aroolors Water Content of Liquid Aroolors 14-10-48 14-13-48 14-17-48 14-81-48 14-24-48 14-29-48 14-31-48 14-32-48 14-34-48 14-33-48 14-36-48 14-42-48 14-43-48 14-44-48 14-46-48 14-47-48 14-48-48 14-63-48 i l HONS 058867 ttouoanto Chemical Company Anniston Method No, 14-10-46 Specific Oraylty of Aroolors Tbs temperature at which the Gravities of liquid Aroolors are taken varies Kith the viscosity of the liquid. Note the temperature at which the' cravlty is to be taken for the Aroolor under test and heat the sample to 10*0. above that temperature. Pour the hot sample Into the steam or.hot water jacketed hydrometer jar provided for this test. Stir well: with an aoeurate thermometer and adjust the temperature to the desired point by ooatrolllnr the steam or hot water feed to the jacket, jcontlnue stirring until the temperature remains oonstant for half a minute. Allow the hydrometer to sink Into the liquid, then read the hydrometer scale at the point of tho lower meniscus and record with the temperature. . Report tl speolflo gravity to the nearest 0.001 unit. HONS 058868 i Monsanto Chemical Company Anniston Method Mo. 14-15-40 iPBJSCT; Total Chlorine In Aroclara }IT.lSiODt Volhgrd Titration following Peroxide Fusion Chlorine In Aroolors nay ha determined by fusion of the sample vilth sodium peroxide In a Burgess-Parr fusion eup, extracting the fusion with notor, ocidlfylng tho eater extract with nltrie acid, and pre cipitating the ohlorlne by addition of an exosss of silver nitrate. After filtration, the exeess of silver nitrate Is determined by ti tration aicpinst potassium thlooyanate, usin': ferric ammonium sulfate as Indicator. Apparatus The fusion eup used Is the Burgess-Parr Sulfur Bomb No. 3 for flame ignltlonJ A lead gasket la used. For Ignition, the bomb Is suspanded ttpough a 1-3/16" round bola In a 1/8" translte plats. This allows the fusion eup to extend through tbs elate for about 9/8 lnoh. Ignition Is sffaoted by strongly heating the bottom of the fualon oup with the full flame of o Maker burner for two minutes. The bomb, gaskets, and the aodlum peroxide era obtained from the Parr Instrumert Company, Moline, Illinois. Charge for Fualon Tbs fusion mixture la made up of about 15 grams (one natal aooop) of sodium peroxide and 0.3 grans of finely powdered cane sugar. The reagents[should be free from oblorlns, or a blank run and eorraoted accordingly. The fualon mixture is wsll mixed by placing the Ingre dients In a small glass stoppered bottle and shaking vigorously. A measuring spoon for the sugar la oonvenlent. '.50LID AlluCLiOm: The non-oryatolllne type are wolghod in the form of small pellets. These are prepared by beating the Aroclor until a eonsletenoyjls reached as will permit dropping It from a glass stirring rod onto a tinned surface (a can top), eeoh drop forming a pellet. ./hen oool these pellets can be removed from the surface by Inserting a spatulu under them. .4 grume are uaad. The pellets are brushed Into th?^bottom of the fualon oup and tbe fusion mixture placed on top of t^iem. After tightening the lid, the Charge le ready for fusion. The orystolllne type Aroelore ere weighed In tbe powdered form. ,4 grams being used. They are charged In the same manner as the nonorystalllne type. MONS 058669 t Total Chlorine In Aroelors 8- LIQUID ARCCLQR3: .20 to .30 grama ere weiehed by drorlng fron e stirring rod onto a piece of thin heralspherically shaped glass, or 1/2 gelatin oapsul (Oelatln Capsules No. 00, United Drug Company, Boston - t|t. Louis), which hes boon Just nrevloualy tered, and nhleh remains on the balanoe. It Is necessary to heat the more viscous Aroelors to "dropping" consistency. The piece of glass then easily slides off the bolonoe pan Into the fusion cup. Cover with the fusion mixture. . The following quantities of a..mple, sugar, and AgN0s are used for the respective chlorine contents; 01 CanteM OJC - 90^| SOJl - 45,1; 48it - BE#; 98/ - 60)1; 6j! - 70/^ Prooeduxaj .'eight of 3ampla 0.3 grams 0.3 grama 6.3 grams 0.3 grama 0.3 grams Amount sugar 0.3 g. 0.3 g. 0.3 g. 0.3 g. 0.3 g. AgNOp SO ml. 50 ml, 50 ml. 75 ml, 100 ml. Place the fusion cup, which oontalns the prepared sample and fusion mixture, in the transits lenltlon plate and apply the full flame of the Maker burner to the bottom of the fusion oun for 2 minutes. (CAUTION: Do not stand too near the fusion during Ignition. The use of a safety shield Is recommended.) Then remove the flame and cool under the tap. '.'.'hen cool remove screw cop. Thoroughly rinse the cup oover with water, collecting the rinsings in a dean 400 nl. beaker. Then place the fusion cup on Its aide In the beaker and cover with a watch glees. 90 - 70 ml. will ha in the beaker from rinsing the sap, and this [Is aufflolent to decompose the charge. Remove the eup and rinse wall, .lien decomposition la complete, rinse off cover-glass and add purejHNOg, with stirring, until sold Is present in excess to the extent of about 10 ml. (About SO nl. of add are required.) Add exactly 80, 75, or 100 ml. of standard silver nitrate solution from . a plpet (depending upon Chlorine present) and stir to effect coagulation of silver nitrate precipitate. Filter with suotlon through an asbestos pad on aj 1-1/2" perforated poreelaln plate and wash beaker and filter 4 times with nail portions of eold water. Allow the filter to drain com pletely Mtween washings. Transfer the filtrate baek Into the 400 ml. beaker aid rinse the flask twiee, adding the ringings to the banker. Add S mil of ferrlo Iron lndleator to tbe solution and titrate with standard.XDN3 solution until a distinct pink tint Is just obtained. HONS 058870 Total Cl .orlns in Aroolors -3- Subtract the volume of KCN3 required from the volume of KCN3 required to titrate the amount of etanderd AgtJ03 solution used. This will five ohlorlne In the sample. Multiply the volume so obtained by the ohlorlne value of eaoh ml. of K0N3 and divide by the weight of sample taken. For example: If 50 ml. of silver nltrote solution Is equivalent to 61.4 ml.[of X0N3 solution and the volue of 1 ml. of KCN3 solution Is .005770 pram 01; then If it la found that 0.3 rram of sample Shows a KCB3 titration of 10.4 ml. the peroent of ohlorlne let (61.4 - 10.4) I .003770 X 100 ,, 64 09< Cl .3 ' In ease the fusion mixture or other reagents oontaln ohlorlne, the amount suet be determined and deduoted from the ohlorlne found. Solutions Required Standard AgNO, solution: Dissolve 22 grams of silver nitrate In sash liter or water. Proteet the solution from light. Standard KCN3 Solution: Dissolve 10 'rams of KCTI3 In 1 liter of water. Forrle jron Indicator: Use a saturated solution of ferric ammonium alum, a^out 50 e. per 100 ml. of water. Aire Nlirlo Acid: stock add suffices provided It Is oolorless. It oan be boiled in a beaker until eolorlees If neoessar;' using 600 ml. IIHO, end 300 ml. of Ha0. Standardization of Solutions ielgll 0.3 and 0.15 gram portions of pure dry NaCl Into separate 600 ml. beakers. Add 250 ml. of distilled water to eaeh and 10 ml. of pure 5011 nltrlo aold. .Then eolutlon le complete, add 50 ml. of standard AgI03 ablution from plpet. Stir well end filter through an aobaetoa mat on k perforated porcelain plate, using suotlon. iVash filter and transfer the filtrate back to the beaker In the same manner as when working"with a sarnie. Titrate the filtrates with etanderd KCN3 eolu tlon, ualng ferrlo Iron indicator. . '. The value of 50 ml.'of ApjaOj solution In terms of KCNO eolutlon le found tjy subtracting the ml. of 1CCH3 solution In titrating the 0.3 gram Of BaOl from twice the number of ml. of KCm solution used In titrating the 0.15 gram of Had. MQNS 058871 Total Chlorine In Aroelors 4- Thla talua Is oheoked by titrating SO ml. of AgfIOa solution added to 400 ml. of mater and 10 ml. of pure 30/ HtTOs with KCtts solution. This titration should agree Tory olosely (1 0.1 ml.) with the yalue found from the titration of NaCl. The titration must be made slowly to aeold drainage jerrar. Sines purs NaOl oontalns 60.66/. Cl by theory, the value of the KCHS In terms of chlorine may he found by dividing the welcht of ohlorlns in the MS'Cl taken by the ml. of KCH3 equlvulent to the silver nitrate required. trample:j Two 0.3 gram portions of NaCl show K0N3 titrations of 13,11 and 13.13 ml. Two 0.16 gram portions of NsOl show HCNS titrations of 37.88 and 37.24 ml. Tbs KCN3 equivalent to 30 ml. of AtfiOg Is thsn (37.88 37.24) - 13.13 or 61.4 ml. By titration of 50 ml. of ArWCj against KCfn solution. It Is found that 61.56 ml. era required. This agrees within .04 ml. of tha value obtained from the NaCl titrations. The chlorine value of the KCN3 Is thsn, .6066 X .3 divided by 61.4 13.18 or .003770 grams 01 per ml. of K0N3. Tha ehlcrlne value may also ha calculated from the titration of 0.15 gram of NaCl. 0.6066 X .13 divided by 61.4 - 37.86 gives .003770 grama Cl, per ml. of KCR3. Precautions 1. Thejfuslon materials have explosive properties If handled lapropofly; consequently ears muot be taken to use safe proportions; to secure e good mixture free of large lumps, end to orooerly seat the oovar of the fusion sup. The fusion mixture muot be kept sway from rater or moist sir, either of wl leh may lgalte the eharge. The fusion mixture should not be ground to reduoe lumps. 8, The method as described la not applicable to volatile organlo com pounds unless precautions are taken to avoid loss of sample during weighing. Bffcot lot Variables 1. On aeoount of the high ohlarlne oontent of many of tha Aroelcra and the nail amount of sample taken, great eceuraoy' la required in weighing, transfer, end mixing of the sample. The plpet and buret for measuring the standard solutions must ha vary elean to avoid drainage errors. MONS 058872 Total Chlorine In Aroolors 2. melons which show black carbon deoosltos on the oover and side of thi fusion cup nay or nay not five the full chlorine content. If a iorbon deposit is found, a second fusion should be made using a smaller sample or reducing the amount of sugar in the charge or both.' 3, The temperature at ivhloh the standard solutions are standardized should be noted. In case room temperatures Tory from this tem perature, appropriate volume corrections should be made. 4. The fusion mixture materials should be ossentlally free of chlorine. T s ohlorlne content may be determined by making a blank fusion, that la, without addition of sample, and titrating In the usual way. rive hi. of AgNOj may bs added Instead of 50 ml. portions of AgHOs solution In like volumes of solution end nitric acid. Heferenoes Beamish! Determination of Organic Halogens, Ind. Xng, Chern Anal, td., 302 (1934). T.tfJtcm 1-89-45 Copied by! ra 4/80/46 i 1 I HONS 058873 j Monsanto Chemical Company . Annlnton I'ethod No. 14-17-40 : `graJTSCTi softenin'' Point of Tolld Aroclora I ITt.TlIOD: Ball end Ring This method la a modification of the A.3.T.I'. standard method of teat for softening point of bituminous motorla la, serla? designation: E 28-397 i The method differs from the standard method in that the rings are larger than specified. A two ring support Is also used Is order that two tests nay be made simultaneously. Apparatus The apparutus oonslats of the following: (a) Two tapered brass rice, 3/8* inside die. at bottom. 11/16" inside dloneter at top and l/4" deep: thickness of well 3/32". (b) Two steel balls, 3/8" diameter 'sighing 3.49 to 3.55 grans each, (e) A 800 ml. drlffln lov: form beaker. (d) A ring support for the two rings haying a brass plate exactly one lnoh be low the elate supporting the ring, (e) A 300*0. A.3.T.K. low distilla tion thermometer graduated 1*C. i Preparation of the lemple The sample shell be melted end stirred thoroughly, avoiding overheating or incorporating air bubbles In the mss and then noured into the ring so as to: leave a slight excess on eoollng. 31noe the Aroelors shrink considerably on eoollng, the ring should be well filled, nearly to over flowing.' A little of the excess should be drawn over the top of the ring at several points so as to prevent the eooled Aroolar from dropping out of the ring, in the serao way, the second ring is filled with a standard Aroolor of known softening point. The standard Aroolor should have e softening within et least 10 to 15*of the Aroolor being tested. The rings while being filled should rest on e clean can lid or on a brass plate whloh has been amalgamated to prevent the Aroalar from ad hering t!o it. The Aroolor In the rings should be fully oooled and hardened^ before proeedlng with the test. Prooedurja Add oool solution (employ water for softening point between 0-80*0, glycerin for between 80-200*0., mineral oil for above 200*0.) to the beaker until the surfuce of the solution Is 2" above the plate holding the rinse when the ring support is suspended In the beaker. Place the rings containing tbe Aroolar to be tested end the standard Aroelor on the rlnj sujport. Ploee e ball on the oenter of the upper surfeee of the Aroilor In eaoh ring. 3uspend the thermometer ao that the bottom of tbe ijulb la level with tbe bottom of the rings and . just midway be tween t(io two rings. MONS 058874 Softening Point of solid Areolar* - 2 - Pleoe beaker end apparatus on a 6 lneh round hot oluto and heat at auoh a rcjte that the temperature la ralaed 5*0. each.minute. Tlte temperature reoorded by the thermometer at the Instant the Aroolor touches the bottom piste Is reported as the softening point. The heat ing Is continued until both Aroelora have dropned to tie bottom 'late. No corrections are made for emergent stem. Notes j I 1. The itandord Aroolor is run along with the sample under teat In order to compensate for variations In rete of hosting, dilution of glycerin, and thermometer variations. 2. The softening point of the standard sample in determined by making several determinations using frssh glyeerln and oarefully cheeking the rise In temperature of the glycerin so that It Is as near as possLble to 5*C. per minute. 3. The glyoerla may ba used repeatedly for the testa after moral of the Aroolor. 4. Benzol is used for oleanIn.g, the rings and balls. 5. '.atejr can be uocd Instead of glyoarln for softening points up to 90*0. 6. For jaoftenlng points above 100*0, well boiled glyoarln should be used. The usual glycorln la not satisfactory above 125 to 130*C, It colls with loss of water while the temperature remains prooti osity constant. It Is well to have a supoly of hlgh-bolling glyoarln on l^and to he used only for softening points above 100*C. 7. Air[bubbles on the rings and balls during the teat should ba avoided as far as possible. B. The'tats of rise of temperature of the glycerin ehall be uniform for eaoh minute, after the flrat 3 minutes of heating and not averaged over the period of the test. . FAB:en 1 1-31-43, Copied by ra 4/20/48 HONS 058875 Monsanto Chemical Company ( Anniston Method No. 14-21-45 3PBJTCT; Determination of Iron in Aroclora Iron In Aroolore may ba determined by extracting a bonzol solution of the Aroolor tilth diluto hydrochloric add until further extractions shorn no appreciable iron content. The iron in the combined extracts Is then determined by dlohromate titration. Procedure! Transfer 5-10 grams of sample to a olean separatory funnel of about ISO ml. capacity. Add about SO ml. of benzol and shake until the sample is in solution. Shan solution is ooaplete, add 10 ml. of 1:1 lron-froe BC1 and shake for about' 8 minutes, let stand until separation of the two layers . Is oomplkte, ttsn drew off and preserre the aeld extract. Add another 10 ml. of 1:1 HC1 and shake again. Dram off the sold layer and combine with the Iflrot extract. Continue until HOI layer Is clear. Determine the iron (by aaual dichroOata titration nethod* ( TAB: cm 1-31-48 Copied by re 4/81/48 I i i I ( I moms 058876 J Monsanto Chemical Company Anniston Method 116. 14-24-48 3IBJECT: flash and Fla.-no Points r.3'.TilDD! Cleveland Open Cup ^ Ihs flash and flams points' of Aroolor shall ha determined In the Cleveland Open Cup Tester, following the prooedure described In A3TU D 92-33. Apperotu i The sap ihall be supported by a metal plate 1/4" (.635 cm) In thick ness and 6 lnohes (15.24 om) In width. The plate shall be of brass, oast Iron, (Trought Iron, or steel. In the center of the plate there shall be a plane depression 1/32" (.079 cm) In depth, and of lust sufficient diameter to fit cup. There shall be a circular opening 8 3/16" (3.00 cm) In diameter, out thru the plate, centering with the - center of the aboTe mentioned depression. The plate shall be covered with a sheet of herd asbestos board 1/4" In tbloknesa, and of the same shape as the metal plate. There shall be cut In the center of the as bestos b'osrd a olroular bole lust flttlnc the cup. nest may be supplied from any convenient souroa. The use of a pas burner, electric heeter, or alcohol llamp is permitted, but under no circumstances are products of com bustion or free flame allowed to oome up around the cup. The source of heat shell be centered under the opening In the plate and shell be of a type that will not produoe looal superheating. If a flame heater Is used. It may be protected from drafts or excessive radiation by any suitable typo of shield, that doe a not project above the level of the upper surface of the asbestos board. Tha thermometer obeli conform to the requirements of thermometer Ho. 8. (nee A3IH table of thermometers). Proeedu; The the ammeter shall ha suspended or held In a vertical position by any sultabli davice, tha bottom of tha bulb aball ba 1/4 In. (.635 am) from the bottom of the oup, end above a point half nay between the eenter and baek of tha eup. The cup shall be filled with oil to be tested In mieh a manner that the top of the meniscus la ezeotly at the filling line at room temperature. The aurfaee of tha oil shall ha free from bubbles. Tlmre shall be no oil above the filling line or outside of apparatus. The test flame shall be approximately 5/32" (.397 cm) In diameter. The test flams shall be applied as the temperature read on the thermo meter xfeeohes eaoh suaoesslve 5*f mark. Tha flame shall pees la a straight line, (or on the olreumferenee of e olrcle having a radius of at least 6 Inches|) aoross the oenter of the eup and at right angles to the diameter passing thru the thermometer. The test flame shell, while paeelng eorose the eurfaoe of the oil, be in the plane of the upper edge of the oup. The time for the passage of the test flame aoroes the oup shall ba approxl- motelyl second. . HONS 058877 71aah and iFlame Points -2 - The oil stjall be heated at a rate not exceeding 30*7 oar minute tem perature rise till a point Is reached approximately 100 *F below the probuble iflaah point of the oil. Thereafter the rate of heating shall be deoreased and for at least the last 50*7 before the flash point Is reaohod the rote shell be not less then 9*7. or more than 11*7 per minute. I ' The flash point shall be taken as the temperature read on the themo- .netor whon u flash appears at any point on the surface of the oil. The true flash must not be confused Tilth a bluish halo which sometimes surrounds the tost flame. . After detbrmlninc the flash point, the heatlnr shall be oontlnued at the speolried rate of 9*7 to 11*7 per minute, and application of the teat fit shall be made at the specified Intervals until ths oil lrpiitea and con tinues to burn for a period of at least five seoonds. The method of application of the flame shall be the aame as for flash point. The tem perature read at the time of the flame application, which oauees burning for e period of five eeoonds or more, shall be reeorded as the flame . point. ' The flash point end flame point tests shall be made In a room or com partment free from elr drafts. The operator shall avoid breathing over the eurfaoe of the oil. It Is desirable that the room or compart ment may be darkened sufficiently so that the flush nay be readily dis cernible, ' Wots Aroolors 1248, 1294, 1260, and higher ehlorlneted Aroolora do not have a distinct flash or flame point below tbeir boiling temperatures. FAB:on 1-26-49 | Oopled bir re 4/21/48 ! HONS 058878 I ; Monsanto Chemtoal Company | Anniston Method No, 14-29-48 '1 SUBJECTi Vloooelty of liquid Aroolara i ULTIIOD: 3aybolt Universal, A3TH D 88-44 Vlsooslty Is a moasuro of resistance to flow. It Is measured by the time necessary for a oboaen volume to be foroed thru a tuba of chosen length and internal diameter. By theory the viscosity of a fluid is related to the average distance between its molecules snd to their average speed and their sire. Apparatus Vleooslmeter assembly with oil tube, bath, receiver, thermometers, strainer, timer, and plpet to mast all requirements of A3TM D 68-36. The vleooslmeter now in use is made by Krebs Klee, and LXr. Co., New York, purchased from Emil drainer Co,, their 2-tube capacity #862. One tube! - on left hand - has been certified by the Bureau of Standards. Prooedufe The vleooslmeter is set up in aoeordanoe with manufacturers directions using No. 20 motor oil for the bath. The procedure end method of reporting results are those deaerlbed under A3TM D 88-44. Care of Apparatus Bath: At conclusion of test, open the eontaet points until 1 or 2 laohea apart so as not to rut undue strain on thermoetatlo eontrol when bath cools. Put a fen drops of oil in motor cups occasionally. Keep outside of bath wiped free of oil or Aroelor. Cover nltb hoot when noy in use. Maintain proper level of oil by occasional additions thru hole in front.T'.'hen oil blaekens. Cl auntie, clean heaters, tubes, and orlfloep, then refill nlth fresh oil. Oil Tubs: While still hot, remove all possible Aroelor from gallery with plpet. When oooled to 70-60, fill tube and gallery nlth benzene, drop thfcu orlfloe into beaker, drain rsllery nlth plpet, repeat with aeetoae, and wipe dry with absorbent paper in such a "ay that fibers oannot jfall into tube. Repeat until elean. Oooaslonnlly oover the leather plunder with sized thin paper ("copy" HONS 058279 Viscosity lof Liquid Aroolars - Z - shoots) sijd sweb walls of tube before Doin'-; denning fluid . This keeps nails polished. Cover oil tubes with lids when not In use. Orifice: orifloe. foroops, dean. Do not pass wires, strings, pipe cloaners, etc. thru the If a hair falls across orifice, renave with long handle If the orifice booo.nes clogged, dismantle apparatus to Calibration Oheofc thejtlner occasionally for 60 second periods. Oheok bath ther mometer from time to time. Cheek performance of vlsooslmeter periodi cally by running a reference sample of Aroolor on whloh eareful deter minations^have bean made. Available for calibration Is also an oil standard, called "Alpha 48", of the American Petroleum Institute. The oil Is obtained from the Atlantis Refining Company, Philadelphia, Pennsylvania. Because sueh oil standards are subjeet to obanpe they are eheeked annually. TAB) on 1-31-48 Copied by rs 4/21/48 |I I MOMS 056**0 Konsanto Chomloal Company Anniston Mothod Ho. 14-31-48 3UBJSCTi Distillation ltanre of Liquid Aroolors METHOD! A.3.T.M. D-20 with Kodlfloatlong The apparatus, consisting of flask, oondenser tube, shield, and ther mometer, Is exactly the same as described under A.3.T.1.1. test D-80 "Distillation of Bituminous Materials suitable for Hoad Treatment". Attaob a 6 inch auxiliary thermometer (0 - 1S0*C.) to distillation thermometer. Plooe bulb half say botneen top of cork and probable evoruge of distillation rands. Cover both thermometers pith a 3/4" diameter nines tubs to Insure e uniform temperature correction for the exposed stem, barometrlo pressure and thermometer error. The procedure Is dunged only to the extent that thermometer readings are taken1 when specified peroentariee (usually 10, 30, and 90?) of Aroolor nuvo been distilled Instead of following the A.3.T.K. proce dure of weighing the distillate between specified thermometer readings. In testlJg liquid Aroolors, 100 ftis. of sample arc welched Into the distilling flask and distillate received In a tared flask or beaker resting on pan of a Torsion balance with 100 gram scale. Procedure Velgh out 100 grams of sample Into the distilling flask. Assemble apparatui ae described under A.c.T.H, D-EO. Insert thermometer (A.3.T.K high distilling 0 - 400*0.) thru oork In the neok of the flask soithat the top of the bulb Is level with the lowest point of Juncture.!of the tubulature and neok of the flask. Apply heat to the flask supported on two sheets of 20 mesh wire gauze s0 that the first drop comes over In from S to IS minutes. ' Conduct distillation at rate of BO to 70 drops per minute. Collect distillate In a 890 ml. beaker tared on a balance. Take temperature readings, ot 1?, 351, 8?, 10?, 20?, 30?, 40?, 80?, 60?, 70?. 80?, 90?, 93?, 98?^ 96?, 97?, and dry. Corrections for emergent stem end pressure ere spoiled to tbe thermo meter readings If required. Teke correction readings at first drop, 10?, 80?, 90?, and dry. Report the temperatures to the nearest 1*C. Example: (rxposed stem In degrees) X (temperature difference In degrees) X 0.000168 > degrees stem correction - T],. The exposed stem la read from the top pf the cork. The temperature difference Is the reading of the thermometer minus- the temperature of the auxiliary thormometor. ' HONS 058681 Distillation Ranro of Liquid Aroclora - 2 0.00012 tJ A k barometric oorreotlon " T2 T*, - normal boiling point In degrees absolute; A jp ohanre in ureeaire from 780 mm. Hg. Tba oorrettlon la addad if baromoter la below normal and aubtraotad If the bolometer la above normal. (MacDounall - "Thermodynamics and Chemistry? pp. 112). Corrected Temperature Observed tampsratura * Tx 1 Tfc. VABt cm 1-29-88 I Copied byj ra 4/22/88 ! HONS 058882 Monsanto Chemical Company Annljston Method No. 14-32-40 CiUBTrETi Evaporation Test of Liquid Aroolors ICTlioD; 6 Hours Heating ot 1Q0C. AST?' D6-39T - Modified Procedure './lgh on 4 rough bolanoe about 50 grama {" .5 gm.) of tho wall mixed Aroolor Into an soourately tared tin box, 55 m. die. X 33 nm. daap (3 on. Qill-etyle ointment box, daap pattern), Flaher (fl-BBO. Let tand until box and oample era -t room temperature, than weigh accu rately. | Plooe the-box in a ventilated oonveotlon oven maintained at 100*C. * 1* for 6 houre. Remove, oool in desloeator to room temperature and accurately rowelgh. From the loan in weight calculate the evaporation in per oept. Report to eeeond dooimal plaoe only. Hoten 1. Be sufl * box is at room temperature whenever exact weleht ia taken. ( The oven ahould not oontain other cample a which might Interfere with Evaporation. 3.' Because the evaporation loss la eenaltive to temperature, the air bath ftust be olooely maintained at 100*C. FAB: cm ! 1-29*49 | Oopled by re 4/23/48 ! i ( HONS 058883 Monsanto Chonioal Company Anniston Method No. 14-34-48 SUBJECT; Refractive Index of Liquid Aroclora METHOD; Abbs Rofraotometcr________ RafraotlTc Indox The refractive Index or any medium Is defined as the ratio of the ve locity of light In sir to the velocity of light In that medium. It Is measured by the ratio of the sine of the incident angle to the sine of the angle of refreotlon. The denser the medium, the ''raster is the refruotlon toward the normal (higher refractive index). Because the refractive Index is characteristic of each substance, It Is useful la Identifying liquids and verifying their purity, in determining the mo lecular structure of organic compounds, end In some quantitative analy ses of mixtures. As applied to Aroelor testing refractive Index proIdes a verification of composition and purity. Abbe Rafrcctcaeter with aooessorles, Bauseh and Lomb, Cat. #2350, Serial No. 377. Calibrated to reed directly In terms of refraotlve Index of the D line (sodium) at a temperature of 20*C. should be familiar with the Bausoh and Lomb "Directions for Use" ana prsatlce the manipulation as there described before attempting determinations on Aroclar. The abridged directions below provide a working outline but at the expense of omission of essential explanatory details which are eontained in the B. and L. directions. 3crew thermometer into Its socket In water jacket of. upper prims. Open prisms and oheok their condition. Clean If they are soiled, streaked, or spotted. With lower fixed prim horizontal, place on It 2 or 3 drops of the Aroelor from a stirring rod - sufficient to fill the spaces be tween prisms when damped together. Close prisms and lock with lock nut. Adjust Jhe Instrument and mirror to refleot white light Into the refrso- tometerJ No spots on air pookets should be visible. Connect water jaeket to source of oonstant temperature water, usually the tap, and pass water until the thermometer has been oonstant to 0.2*C. for st least 3 minutes at 23*0. The Aroolors flow more easily at 25*C., henoe tbs oholoe of this temperature. With prisms Illuminated, rotate the prisms by means of the Index arms until the border of the light and dark fields passes exactly thru tbs Intersection of the cross hairs. It the border line 1s fringed with oolor, rotate the oompensator until the oolor disappears. If the bous- MOMS 058884 t tRefract lv Index of Liquid Aroclors - 2 - dary 1* nit sharp, adjust mirror until a dlstlnot half shadow la ob tained. If the line or the erosa hairs are blurred, adjust eyepiece until a good foous la obtained. 3eoure final fine adjustment by means of tho slpw motion aorew. Read the pefrsotlve index, estimating to the fourth dealmal niece. If the temperature or the water jacket is other than 23*0., correot to 35* by use of the eorreetlon faetor, * 0.00044 per *0. Phis foetor is applicable only to Aroolors 1340, 1254, 1260, and 1262. It nas found by careful measurement on eaoh Aroelar thru the ranse 10* to 50*0. The correction la subtraoted when tho working temperature is below 25*C. and added; when above 25*0. ' Example! If the refroctlve index is found to be 1.6422 at 15*0., the index corrected to 25*0. is 1.6422 - (10 X .00014) - 1.6370. . Pare and Calibration of Instrument Immediately after use, clean the prisms with swabs of pure cotton dipped in' benzol, finally wiping dry with a soft oloth. The prisms, eapeolalljf the upper one, tarnish end scratch easily. Consequently greet oarp must be taken in eleanlng. Before use the prisms should always be inspected and recleaned if necessary. 'Then not in use, the refraetometcr should be kept in its closed case. For practice or for oheeklng erformanoe, distilled water is useful. Water has a refraotlve index of 1.3330 at 20*0., with temperature co efficient; of 0.0001. A test piece of special glass of known refractive index is supplied with the instrument for calibration and adjustment if necessary of the position of the index arm. Refract Its Index of Aroclors - Typical Careful njeasuromants at 5*0. have given the following typloal values for Aroelers. ' Aroelor 1248 Aroolor 1254 Aroelor 1260 Aroelor 1262 1.6295 1.6376 1.6460 1.6482 Substantial departures (over 0.0010) from these values should be in vestigated immediately as they - if correct - indicate substantial error lnlthe composition of the Aroelor or. contamination with other materials. TABion I 1-27-45 I .I Oopled by ra 4/23/48 ] ' `. HONS 058225 Ijonsanto Chemical Company Ann laton Method No. 14-33-48 tUBJEGT: Resistivity of Liquid Aroolcrs METHOD: '.icalstance Measurements between Conductor a Apparatus Megohm Bridge: Oeneral Radio Company Type 5148, AC operated - 300 volts, serial ftp. 171. This la a dlreot-eurrent Jheatetone bridge for measuring high resistances, bridge balance being obtained thru use of a vacuum tube voltmeter. Range: 0.1 megohm to 10,000 megohms, covered by a dial and 5-position multiplier switch. A resistance of 1,000,000 megohms oen be doteoted. Teat Electrodes: Two oonoentrlc nickel cylinders (or braes, nickel plated) |wlth feet. Obtained from General Electric Company. The Inner alaotroda has outside diameter of 2.0" end height of 3.89", Tilth area Of 184 aq. on. The outer electrode hoa Inside diameter of 3" and Ilka height of 3.89", with area of 198 eq, cm. The dlatance between electrodaa la therefore 0.1 Inch or 0.894 cm. By'theory the electrode constant, area/ length, |ls 191/0.894 or 798 where 191 la the average area. In praotloe the oell, constant supplied by Oeneral Electric Company la used. Tor the electrodes now in use, the cell constant was given as 819. Class Plata: Pyrez, about 3-1/8" diameter with eonoantrlo oxooves to asalat In apaolng the electrodes. Obtained from Oeneral Electric Company. Oven: cjenoo-DeKhotensky drying oven with two holes In back wall for por celain tubes for lend wires. Holes must avoid oven heating elemnte which oooupy 8" paths vertically and horizontally Intersecting at the oenter pf the olroular wall. Lead '.'Ires: Provide 300 ohm Amphenol twin conductor oable to oonneot tile electrodes In oven to the posts of the bridge. The nortlons sznosed to oven'tompsroture are bared end then oovered with noroelaln beads. Provide!also e flexible lead to ground the bridge to a water pips. Clean the leuas, beude, end porcelain tubas Periodically. Aasemblj of Teat Cell The grooved glees plate Is placed In an 800 so. beaker. The clean eleotrodes are plooed in the grooves of the glees olate with tbs connector posts dlreotly opposite in order to give the widest possible spacing to reduoe Isurfaoe conductivity. The cylinders Aould be very elone to equidistant. The apparatus should be dried for 2 hours at 100"C. before UBS. | Hast the sample to be tested to about 110"C. on a hot plate end pour Into the eleotrode assembly until the level of the liquid Is 1/4 to 1/6" above the eleetrodes. Care must be used to moke sure that the MONS 058886 SOiTSCT: Resistivity of Liquid Aroclors -_Po513_S.__ ( Resistance fessurements between Conductors lip of tho oonteiner, from which the liquid la poured, la clean. Tilt the beaker!In such manner that all sir bubbles in the Aroelor will rite to the surface. Air oool to 10S-104*C. then without removing thermometer, transfer to the oven which la maintained at 100*C. and oonnect the electrodes to tho two flexible wlreo wiiloli lead to the me(juhi'i bridge. Hion tho Aroolor oomee to temperature (100*0.), remove thermometer, check cen tering of (electrodes, ond procede to meeeurerr.anta. Measurement vilth Megohm Bridge Connect the two leed wires to the megohm bridge with the lead from the outer electrode to the 10"J unknown post of the bridge; the inner elec trode to tho unknown poet. Connect the PHOUND post on the left side to water pipe. owing tho spring connector, pivoted on the "G" poet, to tjhe LO'.f post, Connect the attachment cord to the 110 V power ripply- (1th the Aroolor ot 10C*C., turn the control knob (CIIECIC-OFEIi'.TE-CTiRGE) ( to tho CHUCK position. Throw all 3 ewltohes at the rear of the Penal to ON. After 2 minutes bring the galvanometer pointer to zero by moons cf the ZERO ADJUST knob. Then turn tho control knoh to CHAROE for one minute. Turn the knob tc OPERATE end return the f.aTvenomster pointer to zero by adjustment of the WJLTXH-Y BT switch and the raoeobm dial. Read after one minute, fe- poot theCHARQE and OPERATE positions for verification. The reeiaijplvlty of the Aroolor is tho product of the "multiply by" reading tii.rase the dial reading times the electrode constant. Report in units of to ohm em, rounded off to two significant figures. Example: : "Multiply by" reeding: L'ogohm dial reading Electrode Constant 100 5.4 meg. ohms 615 cm Itcsletlvity - 100 X 5.4 X 815 . - 4.4 X 10s meg. ohm cm - 440 X 109 ohm cm Values fpT resistivity are qinlified by designation of temperature and voltage, These are 100*0. and 500 volts for the test above. Like con- ( dItIon a ire used at Plant B HOMS 0588a? SJSrpr; Resistivity of Liquid Aroolora - Porp a___ irariODi Roslstonco I'easuremonts bstmeon Conductors Caro of Apparatus The "Operatin'' Inotruotiono", General Radio Perm 4D8-B, which accompany the megohm bridge, recite details of Installation, measurements, uses, and conatrucjtlon, illustrated by figures and circuit and wiring dlagrome No attempt Is mads to reproduce such Information hore. The operator should acquaint himself with the contents of tho G.R. manual and refer to it for ma'lntenunce of tubes and parte, 'hen not In use the megohm used and stored In cabinet. After tho measurements are made the eleotrodes ere removed from the toatod liquid, and allowed to drain until the liquid stops runnlnr from tha oleotrodsa. V.'hlle still hot they are Placed In a beaker flllod with benzene under a wall runlit ted hood and allowed to cool. Then cool, the eleetrodes era removed from the benzene and scrubbed with powdered trlsodlum phosphate end a benzene earbontetraohlorlde mixture (50-50 by volume). TtyIs scrubbing can be done with cither a brush or the hands. The elootrotyeo ero then rinsed with acetone, followed by tap water and than distilled water. 'The eleotrodes should not be touohed by the hands after the acetone wash. After final rinsing the alactrodes are placed In an oven lit 120*0. for one hour or until they are used again. The glass sbaoer plates are cleaned and handled In the same manner as tlie electrodes except that they ore wrapped in lenno paper before being placed In t![ie oven. Calibration! - . For a rough1 chock on the condition of tho bridge, one or more cortrldge- type resistances of known approximate value should be kept on hand for periodlo orremergenoy verification of the meter Itself. 8/3/48 MOMS 058888 Monsanto Chemical Company < Anniston Method No. 14-36-48 : SUBJECT: Dleleotrlo Constant of Llauld Aroolor i ----------------; METHOD: Measured at 100*0. and 1000 oyolss i 3QOPS I This method appllas to mineral oils and oil substitute used for lnaulatlng purposes. Apparatm i Oapaoltanas Bridge Oathoda Hay Null Datestar Oscillator Constant Temperature Oven Variable Air Condenser 1500 eo.'Pyrex Beaker Proeedai sji General Radio Co., Type 716-AM General Radio Co., Type 707-A Oeneral Radio Co., Type 606-A Ceneo-DeKhotlnsky #99050 Oeneral Radio Co., Type 334-F Ileetroi and beaker must be oleened as dlreeted under "Cleaning Apperatus fi Dleleotrle Constant", and be at 100*C. Heat Aroolor In the ean to 105*0. Pour over eleotrode until pletea and oeramle Insulation are oovered. Connect leads. Stir with thermometer outside {oven until temperature reaches 101*; place In oven which has been carefully adjusted to 100*C. At the time sample Is plaoed In oven Its temperature rikould not have fallen below 90*C. Connect |leads to eapeeltenoe bridge, observing that the lead from Insu lated side of oondenser goes to Insulated terminal on bridge, Balanoe bridge carefully aeoordlng to dlreotlon under "Balancing Capaoltanee Bridge"] Until Aroolor and oven temperatures have beoome Identical the bridge balanoe mill constantly shift. After oven temperature reaohee 100*0.,laalntaln bridge balanoe until no pronounoed Shift Is evident. Reoord reading of oepaoltanee soale multiplied by multiplier setting. Dleleotrlo Constant Oapaoltanoa In Aroolor at 100C. Capaoltanee In air at 100*C. Balancing Capacitance Bridge Condensed prooedure. Operator should read operating Instruction for Null Detector for eomplete details. 1. Conkeot to power supply leeds to osolllator and null detector. Ground the oscillator. S. Turn on osolllator by pushing 5000 ohm, 10 multiplier, 100 cycle frettieney buttons. Adjust harmonlo control until oscillation begins as shown by eloslng of aeotor In cathode ray tube. HONS 058889 Pago #S Dielaojtrlo Constant of Mould Aroclor - Toot ld--3P-40 3, On null datootor turn brilliance knob to extrema left, the foous knob to extrens right, gain ecntrol to extreme left, sweep amplitude et mld-soala joaltlon, the sweep frequency ewltoh on line side.1 j. Turn on power switch, lighting pilot light. 5. visit fifteen seconds, turn brilliance knob to extrema right. k. Adjust foeua and brilliance knobs until sharp fine line. y, Gonneot external terminals on detector to output terminals on oscillator. Snltoh tweep froquonoy to external side. B. Connoot detector terminals of bridge to Input terminals of detector, taking oars that tha black wire (ground wire) of the lend goes [to grounded terminal on both ends of lead. 9. Set gain oontrol at mid-scale and selectivity to extreme left. Turn sweep amplitude to extreme left, obtaining vert loci line. '71th 10, with turning control knob obtain the maximum length of thle line,' keeping It .always under 1/4 lnoh with sain knob. 11. Set aweep amplitude to extreme left. 12. set gain oontrol to rive vertical straight line of about 3/8 lnoh, 13. Balance bridge by adjusting power factor end oapaoltanoe dials until only a dot ramcine on the acreen vhen the gain oontrol la at extreme right, - id. Set aweep amplitude beyond mld-polnt, end slightly displace the power-factor dial to obtain a tilted ellpse. IS. Adjust phase control until this allIpsa closes Into a straight llnelnollned to the horizontal. |l6. Bring power-factor dial back to balance position, whloh should restore the horizontal stralfpit line. Dlapleoe this aontrcl the same amount in the opposite direction. This ehould again tilt tha straight linebut In tha opposite direction. Adjust phase control until there Is no tendency for this line to open up when It Is swung 30 degrees from horizontal In both directions. |17. Throughout these adjustments the other bridge oontrol (the MOMS 058890 i Paw #3 Dielectric Constant of Llouid Aroclor - Test l/t-26-48 papaoitanee Dial) must be In halanee position. If the ellipse grad ually opens when the line is horizontal it may be brought back to the }iae again by making alight clanges in this oontrol. If oonfaslon results, balanos both controls again as in (13) and repeat the eueoeodlng adjustments. This is the position of bridge balance: An alteiCtlcn of the pone:ip-faotor oontrol Dili tilt the line which does rot open eppreeiable phru an angle of 30* to the horizontal both <ye; sn alteration of th oapaeltanee dial opens the ellipse but does not change the inoll;nation of the major axis. The apparatus may be left In this balanced condition, turned off by switching off first the brilliance knob of the detector, then the powef switch, then turning off the osoillator. For suoocsslTa measurements the controls are not ohanged, the apparatus left in adjustment. Then tha following, steps define the procedure: 1, Conneot all lends as previously directed including that from null detector to bridge. 2. Turn on oscillator by pushing 100 eycle frenuenoy button. 3. Turn on null detector, wait 15 seconds then turn on oathode ray |tube. Turn sweep amplitude to oxtreme left end adjust brilliance to obtain a fine vertical line on aoraan. 4. Briiy this line to a dot by adjusting the two bridge controls. Initial adjustment is facilitated by having "Gain" control to left. Whep final adjustment le obtained this knob must be at extreme right. 5. This dot remitting unchanged shews condition of brld-e beltnos. Cleaning Apparatus for Dielectric Constant The oondeneor la removed from the tasted dielectric and allowed to drain while still in the oven at 100*0. The oondensar la then pleoed, while etlll hot, in a beaker cf benzene under a well ventilated hood andTallowed to pool. It is then thoroughly washed with powdered trleodlum phosphate and a 50-50 mixture of benzene and eerbon tetreohlorlde followed by an aoetone rinse. The operator should be very careful not to touch the metal plates of the oondeneer .after this paint. The oondenser is then rinsed thoroughly with tap water followed by distilled water and dried on e oleen paper in an oven at 180*0 for at least one hour or until it is again used. Wb 3/1/48 HONS 058891 Monsanto Choralcol Conpany Anniston llethod Mo. 14-12-48 SUBJECTi Aoia Humber of liquid Aroolora ______ KT-TKOD: Titration with Alkali using Phenol Red Coops j The Aold:Number Is the wolght In milligrams of sodium hydroxide re quired to neutralize ono gram of Aroolor to pH 7.6. It thus lneludea any hydnohlorlo acid, ferric chloride, and other Inorganic or organic oonstltutnts haying sold characteristics. It corresponds to the Neu tralize! Lon Number of ASTI.! Designation D1C8 except that the latter la expressed In texms of KOH Instead of NaOH and has a somewhat higher (phenolphthaleln) end point. Procedure To 100 ml. of adjusted (pH 7.6) solvent containing Indicator slowly add 0.1 N NaOH dropwlse until the color corresponds approximately to pD 7.6 when compared against a suitable reference eolutlon. Readjust If neoesaary to maintain pH 7.6. Add SO grams (tig.) of Liquid Aroolor land mix well. Titrate from micro buret with 0.01 N NaOH until the original red oolor of the solvent Is restored. A portion of solvent In a similar oontalner Is. a useful reference In determinin'- the end point. The mctoh Is governed by estimation of the Intensity of red because the hue la pot exaotly reproduced on aooount of the yellow oolor lntroduoed by the Aroolor. 1 ml. of 0.01 N NaOH * 0.4 llgn. NaCE. Calculate In terms of Mfjn. NaOH per gm, of sample.** Report to 4 decimal places. ml. of 0.01 N NaOH X g.i g. of sample Upm. NaOII/fp. Example If titration la 0.08 ml. for 50 g. of Aroolor, the Aeld Number Is 0.08 X 0.4/50 0.00064 tl#. NaOH/gm. Report as 0.0006. solutions Required 3olvontl Nix 600 ml. of benzol, 200 ml. of S-A alcohol and 200 ml. of acetone! Add 5 ml. of 0.2j phenol red solution. Phenol Red Solution, 0.2#: To 0.1 an. of dry lndlootor In a small beaker kdd exaotly 2.0 ml. of 0.1409 N NaOH. Stir to dissolve and dilute with 3-A aloohol to SO ml. ** Reference Buffer pn 7.6: Dissolve 0.41 e. Nan8P04 and 0.59 n. NaaHPO (both qnhydroua) In 100 ml. of water. Add 0.5 ml. of 0.2,. phenol red. Solution Is used for reference In adjusting the solvent If LaMotte pH 7.6 oolor standard Is not available. HONS 058892 Add Numbep of Liquid Aroolora - 2 - Standard 0.01 N NaOKt S ml. of .5 N NaOH to 250 ml. vol. of 3-A eloobol. PrjoteoT at all tlmaa from atraosoherlo C0c. Note i By using 350 ml. aeetons In solvent Instead of 200 ml. a 100 #n. sample of [1234 may be taken for analysis. FABtom 1-30-46 ; Copied by |rs 4/23/48 : HONS 058893 1 Monsanto Choraloal Company Anniston Method No. 14-43-48 | SPBJEOTi Color of Aroolor on N.P.A. Teals I.?;TnODi Helllro Pooket Comparator 300PS The method Is applicable to Aroelors 4465, 5460, or others hoeing N.P.A. colors In' the ranee 1 to 5. Procedure V.'axm the lAroolor is necessary to obtain pouring consistency, rill the test cup [of the Helllga Fooket Comparator, Model 60S, tilth Aroolor, lnaert cup in the comparator, and compare against the oolor disc (No. 620e40, Lubrlooting Oils and Petrolatum) whloh has N.P.A. oolors from 1 to 8 In ona-half]etopa. Report color to nearest 1/4. Clean the test eup with a mlxtur^ of OCI4 and benzol, with final rinse of benzol. ACTS! color numbers coincide with Notional Petroleum Association color number (1918). The relation of the N.P.A. oolor numbers to other color seules iff tabulated below! NPA Color NOS. 1 J(-19.1..8) |j 1/4 i/s 8/4 ! l; 1-1/8 | 2; 8-1/2 3 8-1/18, 41 4-1/8 81 6 7 e, NPA Names m m Illy whits Cream white Extra pale Extra lemon pale Lemon pale Extra orange Orange pale Pale Light lied Dark Ked Claret Red - Union Petroleum Co. m .- 0. H I J K L M N 0 P B A1TH Color Nos. Lovlbond Analysis Bed Yellow Blue 800 510 neo ' 1 0.12 1.5 0.60 8 2.5 8.5 4.6 3 6.9 3.5 9.4 4 14.0 4.5 21.0 5 35.0 6 60.0 7 60.0 B 166.0 0.6 1.1 1.7 2.4 8.0 26.0 37*0 32.0 45.0 50.0 56.0 93.0 60.0 106.0 64.0 - - - - .55 .55 .55 1.80 * FiiBtoa | 1-86-48 1 Copied by TB 4/27/48 MONS 058894 Monsanto Chemical Company | Anniston Method No. 14-44-48 j 3UBJECT! Color of "v;ater yhlte" Aroclora i METHOD; Comparison against A.P.H.A, Ceala 3QOP> i ' The method Is appllouble to Aroolors 1054, 1360, or others haring color less than N.P.A. #1 ("..'ator V.'bite"). A.P.H.A. standards ' Those eolpr standards are sold solutions of potassium ohloropletlnate and coballoue ohlorlde. The unit of color la thot produced by 1 mg. of platinum per liter. The ratio of oobelt to platinum nay be varied if neoeasaryto mateh the hue. Beenuse the hue of Aroelor 1254 end 1260 seems best matched without cobalt, this has been emitted In the prepara tion described. Dissolve 1.245 g. of potassium ehloroplutlnete (KgPtClg) containing 0.5 g. of platinum In weter with 100 ml. of oonoentrated hydrochloric acid, and dilute to 1 liter with distilled water. l%ls solution has a color of 500. Prepare standards from 10 to 100 In steps of 10 by diluting 1, 2, 8 ml. ete of the above solution with distilled water to 50 ml. In standard hlgi form Kessler tubes. Protect the tubes from evaporation. Refer to page 13 of "standard Methods for the Examination of ,'ater and Sewage" eighth edition (1936) for details of standards containing cobalt. Published by American Public Health Association, 1790 Broadway, New Turk. Prooedur^ Till a matching Nesslpr tube with Aroelor to a height equal to that la tbs standard!tubea. Compare with standards by looking vertically downward through the tubes upon a white or mirrored surface pieced at eueh an angle that light la refleoted upward through the column of liquid. A color tuba support (Fisher #7-065, 30 ml.) Is oonveniant. Inaanuoh as the proportions of the standard color solution In the compari son tubeji are such os to represent an aliquot part of a liter, the readings are dtrept aa parts per million. Colors up to 100 arc recorded to tbs nearest 5. Direct eomperlcons are aaticfaotory up to 100. Above till* tbe cample ehould be diluted with Oarbon tetraohlorlde (maximum A.P.H.A. color, 5), and ttw odor obtained to nearest 10 by multiplying by the dilution ratio. | ' . FABtom I 1-30-45 ' , Copied by ra 4/27/48 | mens 058895 Konssrito Chomloal Company s Anniston Method No. 14-46-48 TOBUM T; Acid Number of Solid Aroclars and Heavy Llnuld Arodors USTHOIIi Titration tilth Alkali using Phenolphthslsln l'rocsdurs! Dissolve grams of the i.roolor In 50 ml. benzene In e 400 ml. beaker, warming t< haeten solution. Add 50 ml. 3A alcohol, 200 ml. dlatllled water, hei t to boiling, add 1/8 ml. 1$ phenolphthaleln solution, and titrate, n the eaee of the dlatllled Aroolcra with 0.01 N sodium hy- droxlde lutlon, to a faint pink oolor which is permanent for at least two mlnuti s after rigorous stirring. A reagent blank should be ran oon- ourrently The acidity of the sample Is ealouluted as milligrams of odium hyi iroxlde required per grem sample. Calculations ' Using O.Ol 19 RaOH, -Add No. - ml, titration X 0.4/sample weight Tor 50 gmj, ~ Add No. (ml. tit. ml. blank) X 0.008 Using O.ljR NOOtl, Add No. ml. titration X 4.0/sample weight Tor 50 Acid No. (ml. tit. - ml. blank) X 0.08 Apparatus 10 ml. burette In .05 divisions. Conversion1 * 3 4 1. To obtain Neutralization Number In terms of KOH, multiply the Acid Number In terms of NaQH by 1.408. Inverse factor la 0.713. 8. Multiply the Add Number by 1000 to obtain the parts of NaOH re quired to neutralize one million parts of Aroolor. Thus Add Hunker of 0.|0006 Is equivalent to 0.6 parts of NaOH per million parts of Aroeljor. 3. The large amount of water used causes Sharper separation of the aqueous layer from the non-aqueoua layer, thereby making the endpoint moreIcasily distinguishable. If the titration Is oarrled out against a very light background or In a fluoresoent light, the end point le easily seen. 4. Aside from froo add as a oause for NaOH consumption, ferrlo ohlorlde which la usually present In ana11 amounts, also consumes KaOt! In neu tralization to phenolphthaleln. It therefore follows that an Aroolor of vfry low add number must be also extremely low In ferrlo chloride. FABtm 1-86-45 Copied by rs - 4/87/48 HONS 058896 Monsanto Chemical Company Anniston Method Ho. 14-47-48 SUBJECTi -Pour Point of Liquid Aroelors METHODi A.3.T.M. P-97-39______________ The pour point of an Aroolor la the loviest temperature at which the material will flow When It Is chilled under eertaln prescribed condi tions listed In AOTM D 97-39. ApparotJs oonslsts of test Jar, thermometor, oork, Jacket, disk, gasket, and bath as described under A.3.T.U. method 097-39. The thermometer te the A.O.T.hJ Cloud and Four Test, ranee -38 to 30*C. Present aoneratus Is the mill Orelaer Co. #0R 2234 single unit with 0r2242 test jar. Procedure for Aroolor Follow 097-39 In all respeots except that the centigrade scale la sub stitute^. Only on outline follows: Add 40 ml. of Aroolor to test Jar. Adjust thermometer to center of Jar with beginning of capillary l/B Inch below surfaee of the Aroolor. '..'arm the Aroolor without stlrrlnr to 46*0. In a bath at 46-48*0. Cool to 32*C. In air or water bath at 23*C. Trans fer the | Jar to the Jaeket of the coolin'; bath which Is maintained at 0 to 3*C. Beginnlilg ut a temperature 8 to 10 degrees above the pour point, at eaeh interval, of 2*C., remove the test Jar from the Jacket and tilt just enough to date:mine If there la movement of the Aroolor. This Inspection should not retire more than 3 eeoonda. '.Then movement Is not promptly apparent, the tesi Jar should be held In a horiaontal position for exactly 9 seconds as noted by a stop watoh. If movement occurs, Immediately return the teat Jar to the Jaeket. Repent Met for flow ot the next temperature 2*C. loner.. Continue the test infsteps of even degree's oentigrade (14,12,10, ate.) until the Aroelcr shows nj> movement when the test Jar Is held horizontally for exactly 9 secondsL This is the solid point. The pour point la the previous temperature, 2*C. above the solid point. The pour point Is thus the lowest temperature at which the liquid will flow or pour under the test conditions. Technicians must familiarize thamaelvea with 097-39 which gives complete details1 of apporetus and procedure, reproducibility of results, effects of thermal history, etc. The directions above are Inadequate except es a working outline. - The bath temperature Is controlled by adding dry loe to acetone for pour points [below 0*0. FABiom - 1-30-49 Coplod by rs - 4/27/48 HONS 05889 7 Monsanto Chonlcal Company ( Annljjton Method No. 14-48-48 3JPJECT: The Testing of Aroolore for Inorganic C'ulorldea IKTHpD: Solution* Required Standard ChiorIda Solution: Dlssolvo 0.660 grume of pure eodlum ohlorlde In sufficient rater to meueure eroetly 500 ml.; 1 ml. then contains 800 mlcrogrums Cl. Pipette 85 ml. of this solution to a 500 ml. flask and make to the mark to give a 0.00113 li NaCl solution, 1 ml. of which con tains 40 iqicrogrems of Cl. Preserve In a Pyrex bottle. Caution: The water used In prepsrutlon must be ehlorlde free by the Tyndall beam toot; the 0.0011j3 M solution should not be kept over 1 month. Silver Nltjrate solution 10t Dissolve 5 grams of silver nitrate orystals In 40 ml. of water and add 10 ml. of ooncentroted nltrlo aeld. Chloride free distilled '-star. Apparatus Required J Lalbtte 10 ml. oolor tubes (13 mm. X 100 mm). Test tubs rock with a blaok surface at the barn for uniform comparison (Note: wi ere using bleok gasket rubber over the entire board that supports the base of test tubes during comparison.) Box. About 7" long and 4" wide. This box contains holss In top and . notches In the bottom to hold Lamotte oolor tubes. It Is Just hlfji enough to allow 1/4" of teat tube to extend through the holes In the tap. The box should be painted a flat blaok on the Inside and on top and should oontaln enough holss to aooomodote at least seven tubes. Method Clean all flasks, tubes, and pipettes to be used. Then rinse with dilute nltrlo sold then with ehlorlde free distilled water. Add 60 mil ehlorlde free water to a 250 ml. Erlenmeyer flask, heat to boiling, add 00 gram of the Amoelor to be tosted, '*lch hos been heated to 100*0,[shake vigorously for 1 minute, eool In cooling pan. Carefully deoant eolto of the water extract to a separatory funnel. '.Joeh with pure ethyl ether (ohlorlde free). Transfer 10 ml. of the ether washed extract to a 10 ml. Lalbtte oolor tube after rinsing tuba with portion of extraot. Prepare standards by diluting exaotly 5 ml. of tha 0.00133 11 NaCl aolution to 100 ml. in a HONS 058898 The Tostliig of Aroolora for InorRaalo Chlorides - 2 - volumetric flesk. One ml. then oontalns 2 mloro^rama of Cl. Transfer 1, 8, and 3 ml. portions to 10 ml. tubes, rake to the 10 ml. mark with Cl free nLo. Place standards and sample In light free box from which only the top of tubes are exposed add 0.5 ml. of tha silver nltrote to eaoh tube oompare In a specially prepared test tube rack. The comparison Is to be made Quickly and from a oonstant source of light preferably day llfjit from a window away from the sunlight. Comparison is easier when other sources of light are shielded from the comparison raek. lopk directly into the top of the tubes and compare. Rote the known solution which most nearly matches the -mter extraet estlmtlng to tbs nearest whole mlorogxara. The extruct blank and the distilled -later should shpw no turbidity. Calculation Divide the chloride oontent In micro,"Tans of the known solution whleh mutohes ti)e extraet by the welcht of the Aroclor represented by tha extract to obtain the chloride oontent of the Aroclor In p.p.m. In the procedure described, the 10 ml. extraet represents 40 reams of Aroolor (1/5 of 200 c* taken). The three knows oontaln 2, 4, and S mlorograms of Cl, thus representing 0.05, 0.10, end 0.15 p.p.m. respec tively. Values should be reported to the nearest 0.028 ppm. Frecaution Beoause df the sensitivity of this test, serious errors may result through very slleht contamination or Inattention to details. All ship ment must be scrupulously cleansed, the distilled water absolutely ehlcrlde free end Itestlng done away from fumes of HC1 or Chlorine fumes. 4/27/48 I II HONS 058899 Monsanto Chemloal Company Anniston Method No. 14-53-48 StJBJXCT; '.'star Content of Liquid Aroolors METHOD! Titration with Karl Flaohar Reagent Outllns The Aroolor is dissolved in a mixture of benzene and methanol whleh baa bean titrated with Flsoher reagent to the eharaotarletle end point. Fischer reagent is a solution of iodine, sulfur dioxide, and pjrrldlae, Iodine la consumed as long as any water is oresent. The solution is stain titrated to Obtain the water content introduced by the Aroolor. Solutions and Apparatus Karl Fisehar Reagent: Welgi into a flask 264 grams of pyridine, Barrett 2-A or Kastman 214-11, and add 61 grans of liquid or gaseous sulfur dioxide. Add th liquid sulfur dioxide directly from the inserted cylinder by attaching to the outlet valve a glass tuba extending into the pyridine. Sulfur dioxide eas can be bubbled into the pyridine until proper amount Is added. Store in e glass stoppered bottle. Transfer 65.6 grams of the pprldlne-SO* mixture and 134 ml of absolute methanol to a 1 lltar Floranea flask. Cool thoroughly In an lea mater bath. Add 16.9 grans of iodine, stopper, oool again before shaking. Alternately oool and awlrl until the iodine is in solution. Makes 200 al of reagent. Store in class stoppered bottle. let stand 84 hours before using. When fresh, on# ml of reagent la equivalent to about 0.0033 91a. of water. Aroolor Solvent: Mix 8 parts dry benzol with 1 part anhydrous usthsnol. The diy benzol is prepared by shaking the oommeroiai grade with anhydrous salaium! ohlorlda, deoantlng into a flask and distilling, rejecting the first l6>: to cone over. ' Keep in glass stoppered bottles with Minima exposure to air. ' Jiloro Btaret: 10 ml. x 0.05 ml. Koch automatio with glass stopparsd reservoir. Kok and Krebs #8460. Equip reservoir with a moisture guard tuba oontainlng Orlerlte or a similar dehydrating agent. . Prooedu Heat a clean 500 ml. narrow mouth Erlenmeyer flask in an oven or on hot plate until thoroughly dxy. Sweep out for 10 minutes or until cool with air which has bean thoroughly dried by peasing thru tubes oontalnlag 8 math Orlerlte. Disengag* the flask from the aspirating train and ` dieted olosa dlth a paper oap held by a rubber band. MOMS 056900 ;atr Content of Liquid Aroclors - 2 - '.'llthout delay, transfer 100 ml. of the benzene-methanol solvent to the finale thru a mall hole punctured Into the paper cap. Dover again with paper. Titrate at once with Karl Plaoher reagent to dlstlnot red-brown end point which doee not fade after swirling several times. The Plaoher reagent la dispensed from the microburet the tip of which projects Into the flask thru tha punoture In the paper cap. At the end point any water ooatent of the solvent has bean reaoted. Superimpose a fraeh paper eae Immediately, Obtain wllght of tha aolvant and well-covered flask on a T<rslon balanoe or equivalent. Qplokly lntroduoa with a dry pipette about 100 frame of tha slightly wunne% Aroelor to be tested. Cover at once and weigh again to obtalii the weleht of Aroolor to naaraat cram. Shake until the Aroelor la dissolved. If tha Jlxture la cloudy, norm sllfjrtly. If cloudlneaa persists another mixture hould be prepared. Puncture1 a small hols la the paper cap for tha Insertion of the buret tip and {titrate with Plaoher reagent to the first definite brown eolor, agitating with a gentle swirling motion. The end point should persist through {several swlrla. The end point may slowly fade throudi alar aooese of atmospheric moisture In whleh ease It Is restared by s drop or two of reagent. If not so restored, the end point may have bean a falsa one or the oloaure Is faulty. A definite end point la lmposalbls If humid air la not wall excluded. Prom the amount of reagent required and the vmlght of Aroolor used, cal culate the water content In p.p.m. Onllbrotlon of Plaoher Reagent and Standard rater solution Standard water aolutlon in msthnnol: Transfer exactly 0.40 ml. of water from a micro buret or a 1 ml. measuring plpet to 100 ml. volumetric flask. |p111 to tha mark at onoa with anhydrous methanol and mix. One Ml. of solution than contains 4000 micro'rams of rater in addition to cny water which may be present In tbs methanol. Transfer exactly 5 ml. of the above standard water solution (equlvslmt to O.Cejgrama of water) to a 260 ml. Erlenneyer flask which has bean dried aid awapt with dry air. Close with paper esp and titrate with Flaohsrfreagent In the seme manner us the sample. Tbs end point la sharp. A methanol blank, found by tltrntlng 9 ml. of the methanol seed In mklK up the standard water aolutlon to a Ilka end point, mast always be subtracted from this titration. Divide the amount of water taken by the net Fischer reagent required to obtain the titer of the Fischer reagent in terms of water. Examplei A 0 ml. aliquot of standard solution, equivalent to 20,000 mioroiirema of water, retired 6.61 ml. of Fleoher rea-ent while 5 ml. HONS 068901 later Content of Liquid Aroolora 3- Of the mpthanol retired 0.33 of Fischer reagent. 20,000/(6.61 - 0.55) - 20,000/6.06 3300 mlororrems tvater/ml. Beoallhrletlone: Because the Fischer recent doterloratee rapidly, lta titer nupt he determined for eaoh daye use. If the same standard eater solution Is used In reoallhratlon as In the Initial oallbretlon, the titer of1 the Flsoher reagent must he calculated from Its total eater content (Including that Introduced hy the methanol). The total eater ie the produot of the Initial gross titration and Its titer. This In the example above the total water oontent of a 5 ml. aliquot Is 6.61 X 3300 21813 mlorograms. If on reoallhratlon 7.37 ml. of Fischer reagent, la 21813/7.37 2960 miorograms of eater per ml. Two or more calibrations should be made with agreement within 0.025 ml. Calculation of H0 sample Standardization of Standard HgO sol. Titrate 5 ml. mixture HgO sol. Titrate 5 ml. of methanbl Tit of 5 ml. mixture - A Tit of 5 ml. methanol B A 4 B ml. reagent for HgO added - 5/100 of .4 Divide 3/100 X .4 by A - B - faotor erams of HgO/ml. Multiply faotor X B glvlnc (pcs. of H,0 In 5 ml. of methanol. Add this wt. of BgO to .02 already added giving B^O In 5 ml. (Total) ` 2ftetor He6 St'd Titration -*1 X sample Titration Tg X 1,000,000 - ppm HsO ft. aampla FAB:om 1-27-45 Ooplod by re 4/27/48 ONS 058902 M '.TC^IAL OTJB8R _ERoeHiiss oit_a&sic_' Ho. 1000 grow Products Dir, .Union Cartids and Carbon Coro.,, 30 E, Forty-Second St,, N,T< V) N,T.), ' --- -- ------ ' Ho. 1001 w1013 ! rt * C^lOTS Hhlte to me Straw Thlto to Pale Tellon Pale Tellow Pale Tellow Few Point (Fed. AST!! Softening Point) dog. T. Liquid 194-201 247-252 277-283 S icif ic Gravity et 77 deg. F. 1.19 - 1.25 1.53-1,59 1.65-1.71 1.75--1.PI P:ietratlon (Pod. AST!!) 200-g. load at 77 deg. F. 10-15 5-8 ' 5-8 V :cosity (Seybolt Universal Seconds) 3 3tIllation Range (AST!) deg. F. . 33-37 at 77 dew- F. 33-37 at 2S6 depjt 7. 31-35 at 266 deg.?. 33-37 art \ 302 deecF,' 480-590 600--550 &15-655 S%-730 ' ^t^.sh Point (AST?* Cleveland open Cup) der. F. 203 284 358 392 *|-~e Point (AST!! Cleveland Onen Cup) deg. F, F-var Factor at 1,000 cyclea . at 10s cyclea 338 None to boiling Hone to boiling None to boiling -- Less then 0,2/ Less than 0.2f Less than 0.24 -- 0 43? 0,70c! 0-70? r electric Constant at 1,000 cycles st 10 cycles 3 0, Raaiatirity (nag. cm.) at 30 dag. C. 5-6 4-5 4-5 -- 5-6 4-5 4-5 - Oyer 107 - 10? Over 107 - 10 Over 107-109 Copied by i 4/2/48 MOMS 058903 I-A-B-4000 From - IteXovjax Products Division Union Carbide and Carbon Corporation SO East 42nd Street New York 17, New York Latter - r/.c.H./J'.n. Cole, Tech. Rep, 8/16/48 Zyrox 3009 (11*513) GENERAL INFORMATION Color | 3p, Oravltyj 3oftenlng Pt. Storner Viscosity 3aybolt Fur01 Viscosity Penetration at 80*0. Panetratlon at 28*C. Flash Pt. Firs Pt. Combustibility Fraotura Acid Resistance Alkali Resistance Volatility P.F. at 25*C. (1000 eyelss) Dlel. Constant at 8S*C. (1000 eyelee) DO Resistivity at 80*0. - Brown - 1.40-1.45 at 25 *C. - 79-03*0 - 59-89 at 130*C. - 79-180 at 130*0. - Approx. 15 (200 gm. load) - Less than 3 (800 gm. load) - Approx. 590*F. - None to 600* F,, - ".'Ill not support oombustlon - Concholdal - Excellent - Excellent - Average for 84 hours at 130*C. Less than 0.10 mg./s<i.om./br. - Approx. .001 - Approx. 2.96 - Over 10B nag. oms. Copied by ri 4/8/48 [ HONS 058904 From - Hal07:ax Produota Division Union Carbide and Carbon Corporation 30 'Cast 42nd Street New York 17, New York Letter - /.C.U./J.M. Cole, Tech. Rep. 2/16/48 Zyrox 3007 (11-308) GENERAL raTOHM'.TION Color ; 3p. Gravity 3oftoning Pt. Stomer Vinooslty Saybolt Furol Viscosity Penetration at 50 deg, C. Penotrotlon at 25 deg. C. Pieah Pt. Fire Pt. Combustibility Fracture Add Reels ianoe Alkali Res Lstance Yolot111ty P.P. at 25 deg. C. (1000 oyoles) Dial. Constant at 25 deg. 0. (1000 oyeles) DO Resistivity at 25 deg. C. - Brown - 1.29 - 1.32 at 25 deg. C. - 65 - 70 dee. C. - 20-37 at 130 deg. C. - 20-30 at 130 deg. C. - Approx. 75 (50 g. load) - Less than 3 (200 g. load) - Approx. 530 deg. P. - None to 600 deg. P. - '.'Ill not support combustion - Conoholdal - Excellent - - Excellent - Average for 24 hra. at 130 deg, 0. 0,20 mg./a^.cm./hr. - Approx. .004 - Approx. 3.0 - Over 10^ meg. cma. Copied by fa 4/2/48 1 MOWS 058905 I-A -d-400 HONS 0 5 8 9 0 6 003-P-V-I Tran: B.I.O.s. Final Rapt, *>. 893 . AFPEHDEL ZX . PHYSICAL AR3 CBEKICAL PH0PUffIE3 OV CLOmf* OILS Ban Nos. 1, 7, 22. A 31 Fegss 108 - 109 (aa quoted in I. 0. Farted' a sales sheets) Property Clophen AS0 Clophen A40 Clophen A50 Clophen A60 Clophen A70 Clophen ABO Form .. ,, ,, Liquid Liquid Colour ....................... .. .. Spec ifio Oravity at 20*C .. .. Solidifying Point.......................... Flash Point* .. .. .................. Shrinkage: 100* - 20*C ' 50* - 20*C .. .. Viscosity at 100*C .. .. .. .. Roiling Point Unit st 12m. of ISsrcury ................................. Lose during Evaporation (after 6 hours at 100*C) nearly eolourless Hearly eolourless 1.35 1.48 -18*0 -5*C 166* 193* (Pensky - ttartens) 3# 1.1*3 e# ss: 1.2*E 165 - 195* 180 - 215* 0.05# 0.03# Volatility at 20*C.................. ...... (la, of Bsreury for 100 hairs) Beat Conductivity at 40*C (in Calories per aetre per hour per *C), Saponification Ho............................. ^0.009^ 0.095 0.0 <0.009* 0.091 0.0 Liquid Nearly colourless Liquid . Vim Nearly Nearly colourless colourless crystal!Ids - Thlts - 1.55 1.68 1.7 1.72 - 1.77 +12*C +30*0 +50*C >160*C 822* 236* In an open erueihle Or 6# si 3# 1.5*2 1.9*3 240* 890* or over (Pensky - Itertens) 5-6# . 9# * - 4*2 ` 190 - 230* 195 - 250* 200 - 255* 210 - 260* 0.02# <0.009# <0.01# <0.009# 0.01# <0.009# 0.0 (2 hrs. at 125 <0.009# 0.087 0.0 0.086 0.0 * 0.0 0.0 Ash . .. .. .. .. . Permittivity at 20*C .. .. .. Poser factor .................. .. .. Breakdown 3trngth ................ .. .. Insulation Reslstanoa in Ohn.oni. V. Mall 6.0 <0.001 200kT/on. 1 X 1015 V. Mali 5.4 <0.001 200kV/ea. 1 X ID13 V. snail 3.0 <0.001 7200kV/an. 1 X IO14 V. anil V. email 4 - 4.5 3.0 <0.001 <0.001 > 200kV/om. - yll 1014 >1 X 1014 V. email 3.0 - >1 X IO14 MQNS 058908 O H 'M ' Clopkau an not goahiatnia end do not support ocnbustlon of enterlale Into riilek thqr lapraflntad. 11/19/47 TABLE- I F*on - United Ttntee Patent 8,070,268 Patented February 9, 1937 Bags 2 -I-A {b) (e) B (a) 300, 2100 O tU li^U N H 1 --* 2-------3-- 4-- 5-- 6-------- 7-------8-------- compositions Di phenyl Dis tilled blfih boiling com pounds Percent 0 0 80 80 50 50 Percent 100 IOC 20 20 50 50 Properties of dielectric Chlo rine content . Viscosity see. leybolt at 210* F. Percent 23.9 40.3 41.2 52.2 42.0 36.4 - 63 290 35.7 47.5 48.8 40.8 SoecIf1. axerlty at 65*/65* C. 1.251 1.405 1.352 1.490 1.385 1.324 Dielectric constant K at 100 C. (1,000 cycles) 4.35 4.98 4.87 4.56 4.84 4.89 . Properties of chlorinated diphenyl 100 0 54.0 46.0 1.523 4.30 . 100 0 43.0 34.0 1.380 4.80 'd Copied by rs 2/2/48 HONS 058909 I-A ( }) -500 ( Stability of Orade P Hyoor and Taflon In Aroclor 1254 at 130*0 and 45*0 Short Form Report No. 2179 File No. 141-27.1 December 29, 1947 Notebook references: Smith 45137 i Oracle P Hyoar and Teflon Immersed In Aroolor 1294 Material! Temp. Hours ft (Jain in ".t % Gain In Thlokness Qrede P Hyear Orede P Hjnoar Teflon Teflon 130*0 45*0 130*0 45*C 285 28$ 265 285 68.6 26.8 Negligible Negligible 26 6 Negligible Negligible rs 1/14/48 II HONS 058910 I-A-l - 800 c From - '.'smo P.O.B./R,L.J, S/&2/48 Aerovox Corporation Hen Bedford, Massachusetts Determining Fluorescenoe In Aroelor t"The ttlt| avlolet light no use for determining fluorescenoe In Aroelor s manufactured by Oeorre Outoe and Company, Franklin 3quare, [Lone Island, Hew York. It Is a CH 4, 100 V/att, 0. E. Menda UWJip with filter. "Our procedure Is to pour a small amount of Aroolor Into a S" watoh glass or a S" Pyrex evaporating dlah end Observe for tha dagrea o|f fluorescence under tha CH 4 lamp, prefersbly In a dark room. If the aampla has boon contaminated with Mineral Oil It will sbojw up as a streaky or milky fluoresoence as oompired to pure Aroelor. The fluorescenoe around the meniscus of pure Aroelor Is not to be confused with the fluorescence resulting from contamination. ' ( "This ta st Is qualitative and, as suoh, is based on the experlenoe of the parson performing It. He keep a standard sample for oomparlson. If there are any further questions please feel free to eonta ct us". Copied by rs 4/8/48 ( HONS 058911 13 - 100 December 2, 194? ELECTRICAL DATA ON AR0CL0R9 Introduction Time has not permitted ua to carry out eleetrioal meaauremente on ell of the Aroolor samples sent by your laboratory and as listed la your litter to Dr. C. K. Bump of Tune 27, 1947, It mas believed that dleleetrlo oonstent, loos factor, and direct eurrent resistivity measurements over a temperature range for a low chlorinated and highly chlorinated biphenyl; also one sample each of the terphenyl and the mixed biphenyl and terphenyl series would represent the electrical be havior of Arodors. The '.rend of the eleotrlcel properties of the samples not measured can be estimated; l.e. as the viscosity of the Aroolars of e particu lar aerie.i Increases, the loss factor will decrease and the loss factor maximum (:.f within the temperature range meucured) will be shifted to higher telleratures. An lnorease In viscosity will Increase the resis tivity of the Aroolor. The dleleotrlo constant of a material Is a measure o:' Its polarizability. Therefore, any change In the structure of the no ieoule which will Increase Its polarizability will oauee an Increase in dleleetrlo constant. Aoouracy if Data The aoouracy of the alternating ourrent data is dependant on the dissipation factor of the dielectric at a particular frequency and a particular temperature. The dleleetrlo constant values era aoourata within .2$ provided the dissipation factor is less than 10$. The error la greater with Increasing dissipation faotor. The acouraey of less factor (dleleotrlo constant X dissipation faotor) is also dependent on dissipation faotor. Aroolor 5442 was the only sample which bad a de al pation faotor greater than 10$ and that oeourred at the following condition! 41*0, 500 cycles 41*C, 750 cyoles 35*C, 500 eyoles It Jill be noted that the dielectric constants extrapolated to 100*C. oNack satisfactorily with the values listed In your letter to Dr. uumpj . The direct ourrent resistivity values have a 30$ error for the fleetest resistance readings on our instrument. Tor'lower reslstanoe values the error decreases. Aroclora 1221, 1254 showed an lnorease In resistance with time whloh la Indicative of polarization effeots. for these meterleIs then, realetance waa read after the voltage wee applied and then let the end of one minute - an emplrloal method used for taking a readable value. Aroolore 4465 end 5442 did not show noticeable pole- MONS 056912 i IB - 100 c; "8 - December 2, 1947 rlentIon effects, even at the hl$i temperatures. Data j The dieiectrlo conatact of Aroclor 1221 and 1254 is Independent of frequenoyL The dlelectrle constant of Aroclor 4465 and 5442 la also Independent of frequency at the high temperatures. The llquld-llke properties of 4465 and 5448 disappear at the lower temperatures where a dispersion region becomes evident. It will be noticed that the dleleotrle constant curves (at the lower tempera tures) have ihe same order as those of the corresponding loss factor curves end the inflection regions ooour at the loea footer maxima tem peraturee. The loai factor curves of 5442 at the higher temperatures show a sharp up-swikg, Indicative of a large oonduotanoe component In the lose faotor. Similarly, the loss faotor curves of 1221 and 1254 seem to be la the conductance region. Aroclor 1221 showed an unusual sensitivity In changing loss factor values and a|s greet an Insensitivity to change In dielectric oonstant. It was found, that a sample measured Initially at room temperature and measured at successively Increasing temperatures gave different loes faotor values when compared to measurements made with the Initial tem perature high and then successively lowered. Results showed that raising ths (temperature of the liquid or allowing the materiel to stand in the open for long periods always lowered the loss factor, probably volatilizing the more conducting or the hlgi loss subetanees In the Aroelor. Below 5000 oycles this offset was very notloeeble, the diffe rences Inrreasing-with deereeslng frequenoy. It may be mentioned hare that lose 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 the Aroelor 1200 series. The log resistivity versus l/T graph Is useful as an indleatlon of the obange that ooeura In resistivity with temperature - or what le related, ths change In vleooslty with temperature. The actual slopes of 4465 and 5442 oannot be assured slnoe there ahould have been more measurements made at high temperatures. However these two Aroelors have a much larger viscosity-temperature coefficient than ths other two plots. It Is hoped that the enclosed renha will summarize the dleleotrle properties qf ths Aroolors measured. More complete Information or any questions concerning the data will be sent on request. i W I Copied ty vs 1/15/40 ; R. Levrsault ' lion santo Chemical Company e- flaatloa Division 3prlngf laid, liaisaohusetts MONS 058913 /fesishi/ity mtvbt**tm.- E>TJ1`P| 5 O I-S -I j MONS 058916 II-B From - B.I.O.S, Final Report Mo. 893 Item Nos. 1,7, 22, and 31 Pages 12, 13. 14, 15. 18, & 17 III. CHLCRINATgD DTHIENYL 1. Qefaeral. | Chlorinated diphenyl Is manufactured by I.O. Farben under the trade name of Clophen, Some types are liquid and others solid at normal temperatures. They are used as lmpregnants as alternatives to hydrocarbon oils and nazes. Clophen shares with other ohlorlnated materials a high permittivity and has tl>|e same dancers In handling, due to noxious properties. In addition to tas grades suited to eapaeltor Impregnation, a grade known os T64 Is mads by I.O. Farben, suitable for trans former ooollng. Tho total output of Clophen A50 and A60 far th|e years 1938 and 1943 trass | 1938 Type ABO 21 tons 99 . A60 182 94 i 1943 49 A50 170 99 49 A60 506 91 I Tho cost of ths material In domany le:- Type A50 111, S0pfg.to 111, 60pfg. per Klloirram " T64 HI. 20pfg. per Kilogram. The following is a list of the principal prewar consumers of Clophen:- I Siemens-"5chuckert, Berlin. | A.B.O. (Bydrawerk), Berlin. [ Kloefll (Brown Boverl), Zurloh, Switzerland. j Alethom, Paris. j Ouaatl, Milan, Italy. '' j It was stated that no daman eapaeltor manufacturer uses Clophen for the manufacture of small cupaeltors for radio and telephone purposes and where these have bean used by the Car man fighting services they were supplied by the Italian fine, Duoatl. 2. nufaotura. The ayntheala of diphenyl from benzene. Biphenyl Is synthesised from benzene es shown In the figure, following:- HONS 058918 ! 200*C Two-stage Heat Exohanger 1 The synthesis oooura In the vapour phase, at 600*0. and | atmospheric pressure. In an electrically heated reaetlen | coll of coppor-manganese alloy. Ho catalyst Is required. The apporatus, apart from tbo reaction ooll, Is of Iron, end operates at the temperuturae shovn above. About 10,? of the benzene vapour Is eonverted Into diphenyl In one ; passage through the reaction coll. : The purity of the benzene Is of Importance for the eleetrleal quality of the ultimate chlorinated produets and a specification Is attached overleaf. The benzene used i was believed to contain 0,2 to 0.3* of paraffins but | little definite Information oould be obtained regarding | any undesirable Impurities or the mechanism by which they j oeuee poor electrical performance. Thiophene was stated to be definitely harmful, and vague reference sea made to "nltro-oompounds", to 'aliphatic hydrooarbons" and to j "substanoas whloh oould not be chlorinated". The precise , nature of thoee materials mas not known, but their abeenee | mas ensured by obtaining benzene always from suppliers | whose product vies known to be satisfactory. Analytical Specification for Pure Benzene Appearancei Clear end eolourless. ! Penalty at 20*c.; 0.876 | Distilling range: First Sf. within 0.2S*C. 5Jt - 95* " 0.38*C, 95,'. - end 0.25*0. i S Solidification points Hot lose than S*G. ! Bromine consumption: Hot more than 0.5 gm. i ~~1 bromine per 100 o.o. j Sulphuric eeld test: Not more than 0.15 gm. *eCr807 I Carbon disulphide: Shall ha frea from C%. HONS 058919 ! Dlffleult7 la the ayutheala nao still being experienced, due to rapid corrosion of the copper-manganese reaotlon ; eoll, operating at 80O*C. A small scale experimental | apparatus using a fused silica coll had been made, but had not been developed for production use, * j In addition to diphenyl, about 5$ eaoh of 1-3 and 1-4 l terphenyla are produced by the process, These are ee- parated, chlorinated and used In sealing varnishes; I presont produotlon la about 4 tons per month. No use j Is made of ehlorterphenyls as paper lmpragnants, since I the materials are resinous and tend to crack; moreover ; the permittivities are lover than thoae of the ohlordiphenyls. | The erude diphenyl Is next purified by distillation. | During this process the terphenyls remain In the residue. | They are extracted In the following msnner;- i 'As residue Is dissolved In hot benzene, filtered, and the 1-4 Isomer obtained by fractional crystallization. The crude product Is distilled In vacua, yielding 1-4 terphsnyl 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 charcool, filtered, and the benzene evaporated. The reeidue I le distilled to yield 1-3 terphsnyl with melting point | 80-84*C. (2) Chlorination of diphenyl. j Tor the ohlorlnatIon of diphenyl a lead lined veeael of | 10,000 litres capacity la usod. It la charged with 6000 ! kg. of diphenyl and 13 kg. of ferric chloride. The mlx- ture la heated to 110*0., agltatad and ahlorlna passed I in. The addition of chlorine la continued far 100 hours ! st s rats of 130-135 kg/h"r during which tins the ten- i perature Is raised gradually from 110*0. to 130*0. Ths j and point of ths chlorination Is determined by measuring 1 ths density of the produet. j To remove hydrogen chloride formed in the procaee, dry j air le blown through the liquid for 2 hours and this hy| drogen Chloride la recovered. The product Is transferred to another vessel and treated with 1/2# of solid sodium hydroxide, heated and agitated. The sodium hydroxide Is allowed to settle out and the Clophen drawn off from the top, transferred to another i vessel to which Teller's earth and soda are added and ths | liquid redistilled. The stills for this proeass are gas | heated. MONS 058920 3 (1) Capacitor lmpreroctla; grades. A euramury of the physical and ohamical properties of the capacitor Impregnating grades of Clophen Is given In 1 Appendix n. There are six grades of oapecltor lnpregnant, A30, A40, etc. up to A80, the 3, 4, S, etc. lndleating the number of chlorine radicals combined with the < diphenyl. Each grade contains a proportion of the adjaj cent homologues not exceeding 20$. Grade A30 has the ! highest value of permittivity. Theoretically the highest i value obtainable with a chlorinated diphenyl Is 9.0, and I a fyade having e permittivity of 7.0 has been prepared, | but Is chemloally unstable, and very sensitive to moisture I end Impurities, The most commonly used grades are ABO and ! AfiO; ABO Is the most stable grads and has tbs lowest dielec tric loss. Grads A60 Is considered by 1.0. to poosess the optimum oonblnatlon of non-lnflammablllty, stability and viscosity. As with Hlbren, It Is considered thst no addi tives arc required slneo the substances are stable In uee, j provided that the capacitors are efficiently foiled against i the air. 1'J.cufll of Zurich arc the only users of ASO and | A40. j The fbHoeing table shows the variation In oapaeltonea ! and power factor with temperature for a Clophen lmpregna- t | ted paper capacitor. I The ImpreGnant Is A50, the dielectric Is Schocller and i Hoosch "A" finish rag tissue (density 1.2 - 1.2S) with I a thickness aT 10 u; fre<fionoy of measurement la 800 a/a. ! Power factor shows a maximum value of 0,082 at about *4*0, ' while eapaeltanoe falls off by some 20$ at temparetuxas | below thle oritleal value. I Variation In capaeltanee and powor-faetcr with temperature for a Clophen-lraprernatod eapeoltar, Temperature CC.) Relative Capaeltanoe Foxier Factor -60 0,87 0.03B -40 0.91 0.024 -20 0.94 0.019 0 1.02 0.048 4 1.06 0.052 (max.) 20 1.10 0.006 40 1.10 0.005 60 1.10 0.004 80 1.11 0.006 So evldenee wee obtained from 1.0. on the use of any type of additive with a view to depressing the temperature at Chleh the ohnnea of state oeeurs. HONS 058921 The msthod adopted for ovaiuatlnp the water contest In oils suoh es Clophon Is described In Appendix III. It Is also applicable to such solids as Nibren. Engelhardt stated that no source of failure had been ex perienced durine the uiiolo period of production of Clo- phan, which Is about 17 years. Consequently no lmprove- j meats or modifications had been made or found necessary during this period. I (!) Transformer-cooling grade (Clophen T64). No detailed Information was sought on this material, since It Is unsuitable as a capacitor impregnant and Is only used as a coolant for tranuformers and phase shifters. ; A summary of Its physical and ehemieal properties Is given In Appondlx IT. It has a low viscosity, la moderately stable under eleotrloal stroesea end has the distinct ad vantage over mineral oils of being non-inflammable. j The principal users of this produot ara A.E.G. and llsmsna, ! but It Is understood that, as with other chlorinated om- | pounds, eonservotlsm and prejudice among customers have 1 prevented Its wider use. No stabilisers are added to the materiel as their function | of absorbing hydrochloric acid would be defeated by the | formation of "ehlorldo salts", which In turn became eleoi trolysed. It nee said to be very Important to avoid con tamination of Clophen T64 whleh may ooour la transit and ' for this reason the use of leather for gaskets must be avoided. 4. Methods of use, precautions, ets. No details were obtained on the method of Impregnation uied by 1.0. for the construction of test-speelinens of Clopisn-Impregnated capacitor. This nes partly coused by the non appearance, after the first day, of Engelharat, but It is not considered likely that any novel processes are involved. ' J Tor Information on the precautions neees9ary In the use of Clophen, see lection II, B, above. re 11/19/47 i HONS 058922 III-A-b - 500 "rom - B.I.0.3. Final Heport No. 893 Item Nos. 1. 7, 22 and 31 Page xlv Clophen la made In several grades, nhleb correspond olosely with their 0.3.' counterparts, A.50 being the grade most oonnonly used for oapocltora. Exoep; for very rare use by siemens and Dolake for speolal orders. Clophen bn i not been used In Qemany for small eapaoitors of the teleoommunlootLon type, but It has been used extensively by slenena-lehuekert for povr capacitors. It la Interesting to note that the Sermon forces used Clophen lmpreenoted and filled tubular eapacltors made by Dueatl, of Milan, who'obtained the imprecnaat from I.O. The prejudice against Clophen ms, kowovor, being gradually overooae end several manufacturers wore contemplating an extended use of this material, aorae of them con sidered It to bo equal to or possibly better tban mineral oil for opera tion at pojter frequencies. re : 11/24/47 I MONS 058923 III-A-b-30 From - B.I.0.3. Final Report No, 893 Item Nos. 1, 7, 22, and 31 PaRes 96, 99 ; (2) Clophsn . i The only chlorinated lmpregnent used by lieraens sehuokert la Clophen, supplied by 1,0. In power faetor eorreetlon and high voltage applications It la oonslder- | ed practically Ideal. [ Hie only type of Clophen used In bulk Is A.30, pentachlordlphenyl,'(corresponding to Aroelor 1254). A.30 and A.40 ha-re bean tried and found unstable. A.60, A.70 and A,80 ure too viscous to allow for Rood Impregnation : and have lo-.ver permittivities. Although the viscosity of A.50 at room temperature is much creator than that i of oil, the vlseoslty at Impregnation temperature is | sufficiently low to give no trouble in attaining thorough Imprecation. ; A routine cheek on conductivity is made on eaeh drum of i Clophen, and formerly If the conductivity were too high, i the Clophen was treated with powdered ahalk to nautrallaa 1 the free acid. Aa the result of oontlnual pressure on i ' 1.0. over a parlod of yaara, the acid content bed graj dually diminished, and it la now possible without chalk i treatment to work to the same rejection limit of resls| tlvlty aa for oil, viz. 1013 ohm.cm. at 20*C. Drums ! of Clophsn foiling to paaa the conductivity test are : returned to 1.0., unless urgently needed, A certain !. elasticity is permissible In view of the big! standard ; sat. Apert from conductivity, further acceptance cheeks ! are specific gravity (1.54-1,55) and permittivity (5.0I 3.2). Permittivity la measured at 600 cycles and 80*0. i on a 9cherlng bridge at low voltage. The acceptance standards for Clophen A.50 are show graphically In ! Appendix XXXIV. ! Clophen costs about 1 K. 60 pfg./kg., and 1b therefore { muoh dearer than oil (30 pfg./kg.). This extra expense is offset, however, by tbs use of a special design which reduces the amount of Clophen required. An ad . vantage claimed for this lmpregnant Is that is has a similar permittivity to paper (viz. 5). , Other lmprewtanta studied. i As Clophen la considered nearly ideal, no serious [ attempts have bean made to find superior materials or addi tives to improve its performance. This attitude is sup per ted by service experience. In which no failures have been reported. It la realised, however, that on freezing discharges may ooeur In the.contraction voids, whloh ray result In decomposition of the Clophsn and failure of the HONS 058924 i dielectric. Teats wore performed (see Section XT, B, (3)) | to check whether this degradation does In feet ooour, end ! no failure mis noted. i Nevertheless, I.O. supplied snail samples resembling Clophen A .SO but' having a lower melting point so that this possible source of failure could be Investigated, bej preeslon of the temperature at willoh the dipoles become i lnmobllo should raise the maximum usable frequeney and ; benoe broaden the range of applications bp Introducing those for audlo-frequenoy furnaces. Two of these 1.0, eannles, Tilth references A.162K and A.162N, are, like Clophen, made from benzene, but have a lower Chlorine content beoause of the presence of an i additional alkyl group (CjiHen*l), and hence a lower density. I Their advantage over Clophen A.30 is that the setting point i (l.e. temperature of maximum dispersion and of eepaeltanee ' I diminution) Is lowered from -0*C. to -17*C. The pormlt- j tlvlty, viscosity and non-lnflomnablllty resemble those ! of Clophen A.60. The vleeoslty/temperoture curves of | these two samples, K.7 mineral oil and Clophen A.BO., are { oonrpared In Appendix XXX7. ' re ii/n/*? HONS 058925 III-B-2300 December 28, 1947 TO: H!0 aFUJYTE DIVISION 'ALK3I,I!N SUBJ: Aroclor 5460 as Used In Ethylcelluloco Lacquer RE: Federation of Paint end Vomlsh Production Clubs Official Dlgestj (Ootober, 1947). to ettyleollulose. Ethyloelluliee is used in lacquers of varlouo types, the ethyloelluloae actins os a lone chain polymer to Import toughness and flexi bility and jto increase the speed of drying. Some of the| principal uses for ethylcelluloee laoquers are for the eoatlng of nigh tension ignition eeble; heat sealing laoquers for foil and puper where the alight discoloration nhloh may develop in nitrocellulose laoquers on heat sealing is not permissible; linoleum laoquers whero alkali resistance is essential; textile printing; printing inks, particularly in multloolor designs where hydrocarbon solvent does not soften or bleed into previously printed designs; alroraft lacquer for resistance to both heat and cold and to cuiek temperature! ehanges; record lacquers, especially for home recorders; and in wood sealers where good sanding and flexibility ere essential. A good plfpncnted ethyloellulose lsoquer baa been made, based on the following fornuls: Ingredients 6.4 6.4 4.2 0.06 67.0 16.0 100.06 rh \ Copied by its 2/2/48 Benlgnus MONS 058926 II1-0-300 From - Memo 0.7. Frankla/P.O. Bonlgnua Mareh 11. 1948 Soil-Poison Conoentrete Aa described below, thane materials are formulated Into a mater emul- slfinbiejaoll-polson ooncentrate carrying almost 80 per cent bp weight of ootlvq Ingredients. . Aroolor 1848 Trlohlorobenzene (Mixed isomers) Pents ohlorophenol Isopropyl alcohol Toluene or Xylene Sterox 38* Santomerse 3 Pasta 33. 33.5 10.0 3.3 16.7 1.5 -ML 100.09C f Other non-lonlo type emulsifying agents sueh as Triton HS or Span and Tween can be used to replaee I the 3terox 33. Copied by ra 4/2/48 HONS 05892? Chemical Abstracts F033IBLF. U3E OP /iROCLORl Vol. 41 Pag# 6067 III-H-10 TT|,3.P. ,425,978 to Anderson and Coalahan, (Hercules Ppwder Company). Foundry eores sprayed with 15 solution of chlorinated naphthalene in hydrooerbon solvent show greater scratch reslotanoe {than untreatod oores. Cla content remains from 40 - 80/ 01*. I Particularly rood for use with VI castings. I 12/E/47 I HONS 058928 IT-10 From - B.I,0,3. Final neport TJo. 89S Item Nos. 1, 7, 22 and 31 Pages - 10 and 11 Mubh leas trouble hea been experienced with ohiordlnhenyl than with ohlornophtbalene, probably beoauae the former, beIn?, liquid, in volves {Less physical dontuot In disposal. (2) Preventton. Tery thorough washing of all areas of the akin likely to be contaminated with solid, liquid, or fumes has always been the basis prlnolple In prevention of akin troubles, and Is still looked upon as fundamental. "fhpn fatty soaps ceased .to be available, because of the di version! of fats to food, it became essential to Insist upon the use of barrier creams, of wliloh the best vies one named "QPIKBO", made at Trommersdorf. This has non been replaced, for lack of supplies, by an alternative made by 1,0., named "KITI'M.", which Is considered Inferior to eutmbo but satisfactory. The Tlssan firm put up a Bpeolal powder named "sCTI'TJFELHJLVTR"j to act aa a barrier, but thla was found to be Inefficient exoopt to allay Irritation on skin srsas exposed to fumes only. For thlp purpose It still finds use at Leverkusen end at the Hydre works f^otory at Berlin. A Special point Is made of fume extraction, end the minimum air speed away from the operator is 1 metro per second. I To check the efflolenoy of the precautions, a thorough exami nation la mads every 4 weeks of every worker coming into oontaet with ehlorlneted hydrooarbons,' and slnoe the enforcement of the precautions, no deaths or symptoms of internal Injury bevo occurred. Ilhoa superfatted soeps have ceased to be available, a cleansing composition containing lUehlor-methane baa been devised. This la so powerful detergent for chlorinated materials that barrier oreams are oonsldered unnecessary, but It Is uncomfortably Irritant to many skins. (3) Cure. : "jhln savers attacks of ehloreons and Internal aioknasa wars enoountfered, In the early years, whan the properties of ehlorlneted materIsis were not wall understood, extensive rest periods had to be prescribed, together with a generous diet, entire abssnoe of further!contamination, and long periods In the open. Bines precautions have been taken to minimise the effects, only a few mild eases of ohloraone have been met. These have been treated with a solution of Beetle and selloylle eolde In methylated spirits!. HONS 058929 -8 - (4) Conclusions ana Reconniamlctloaa. ' t.a. consider that neither toxicity nor akin affection need now hi any deterrent to the uoe of chlorinated naphthalene, and that ehlordlphenyl la If anything leas troublesome, ^Halo people, notably those with fair skins, show distinct , and are beat divertod to other work not Involving contact. florupuloue oleanllness of the skin (Including the face, neck, end earms) and of the olothlng (especially undergarments) la esseatlal and noeds strict enforcement, '.'ashing with hot water end good aoap is sufficient, so long as the aoap la superfatted, alnoe the kin becomes sensitive to irritation by alkali. Barrier oreara should be used on those parts of the skin whlsh. ooms Into oontaet with solid or liquid material, and the area of eoato it should be minimised by the use of protective olothlng end glove where possible. Areas of the Skin which are eonteoted by fumesronly, and particularly those chafed by elothlng (e.g. the nook kdjuoent to the edge of the elothlng) need protection by a suitable soothing powder. k'here fumes are generated, they should he drawn away from the ( operator at an air apaad of at laaat 1 metre per seoond. It may ba found aasentlal to have two duets, one at floor level and one overbead, with exhaust In two dlraotlona simultaneously. |ln ease the precautions sre being evaded, or last there should he some idiosyncrasy, monthly medical Inspection Is desirable. rs ' s11/24/4? ] ( HONS 058930 IT-B-100 From - The Journal of Industrial Hygiene and Toxloology Volume 20, Number 2 February, 1938 TORPHOLOOIChL CHANGES IN THE LIVEli9 OF Ib.fG RESULTING FROL' EXPOSURE TO CERTAIN CHLORINATED UYDROC.diBOfB * Chlorinated hydrocarbons, particularly chlorineted nuohtbalenea and shlorlnuted diphenyl, have bean used extensively In eertaln In dustries. | Their use In the manufacture and prenarutlon of many types of eleotrloal equipment Is constantly increasing. Although it Is known thot| some of these compounds cause acne, only rocently has the possibility of more serloua systemic effects been recognized. The present paper describes the pathologloal changes observed in rats thatlhad been exposed to various chlorinated naphthalene com pounds and to chlorinated diphenyl. Compound G (chlorinated diphenyl) wee administered to two grouts of anlmele in low concentrations. An average concentration of 0.57 mfpta. per eu. m. wee employed 16 hours dally for 134 days In the first i experiment. In the second experiment (employing sn average sir con centration of 0.93 mots, per eu. n.) the animals pare exposed 8 hours dally for 143 days. The present experiments demonstrate that ehlorlnated naphthalene compounds end chlorinated diphenyl are capable of nroduclng marked liver dernsoe in the white rut without demonstrable mloroacoole changes oppcnrlne In the other orp/.ne. Furthermore, the characteristics of the liver lesions resulting from comparable amounts of any given coxy pound are the same, regardless of the method of administration (inha lation, feeding, or auboutaneoue lnjeotlon). Of the various chlorinated hydrocarbons tested, chlorinated di phenyl gate evidence of being the most toxic, 'then administered by Inhalation la very low concentrations (overage 0.57 to 0.93 mgma. per ou. mj) liver cell ehungoa were very pror.ouneed after the first exposure jwrlod. The most striking change was the hyallnlzetlon of t the oell cjytoplesm (see fig. 6, plate III). 3uoh cellular alterations were essentially unchanged after a 2 month recovery period. In these anlmele smell eublethal doses of oarbon tetreehlorlde and alcohol uni formly produoed extensive liver neeroslo end was highly fetol to then ' (figs. 1 and 2, plate VII). Chlorinated diphenyl fed In small doses produced similar but more marked liver injury (see fig. 5, piste III), In large doses this compound was hlgily fatal. The liver chanpea In animals dying after short exposures ware lnocnsctouous and sonslsted \ mainly of swelling of oelle and active regeneration (see fig. 4, plate III). However, animals removed from exposure before being fatally MGNS 058931 -2 poisoned, subsequently developed hyaline degeneration of liver oelle similar to that produced by prolonged administration of small doses of this oompound. Thus tho roaulte of the ireeent study, as vie11 as certoln field studies that have been nude (1) surest that the solution of the In dustrial hazard Involved is dependent largely on a reduction of the sir oonesntretlon of these compounds to a level that will not produoe liver damage. The present experiments Indicate that loner air con centration^ must be obtained In the ease of the more highly ohlorlnated naphthalene compounds and ehlorlnated dlnhenyl than for trlehloruaphthalen^e If a safe environment for workmen Is to be essured. Roouuse of the pronounoed toxlo effeot of small doses of carbon tetra chloride on the livers of animals already Injured by oxnosure to ohlorlnatca naphthalenes and ehlorlnated diphenyl, its use as a sol vent for these compounds viould appear to be very hazardous. rs 8/3/40 HONS 050932 *f*--- w-- ' ' T I i ,| ( j ' .I . jr-i: a--COO ]iut j,l I<& :>o\' i iTo ! v . Pinal Rcpxrt on "Evaluation of Monaant i Materials as Plantloiaors", ?eb Bo, DS. AROCLOR 1232 I Colculatod molecular 283 Kofructivo index*: 1.620 ct "CC. | Saponifloot ion equivalent* : none | Crystallization point*: -32.5*0. i Boiling point*: 290-525*C. at 760 mm. j Acidity*: .01 milligrams KCH/ga. I Acidity after heat: none j Color (Oorfner standard): 0 ' j Color after heat: 0 I Color after llgjvt: 11-12 Speelfio gravity*: 1,2623 at 25/25*0. viator solubility: .001651 at 23*C. Stability to hydrolysis*: essentially not* I Odor: ohloroaroisatle Viocoelty: 23*C. - 6.24 centlpolse 0*C. - 65 oentlpolse j -20'C. - 627 oentlpolse j Solubility: Soluble in: octyl alcohol, ucetono, ethyl I acetate, benzene, 3'.:ollysolve C, Okellysolve H, turpentine, oaator oil, cotton seed oil. Partially soluble la: methanol, ethanol, fly- oerol, linseed oil. Insoluble in: glycol re 8-20-48 HOMS 058933 I-A-5-300 ; ' TASTJ I i dBwsrrr and spec mo voipmb of aroclors Toi tperatura (0.) 49.9 102.2 150.3 201.7 254.0 296.2 waaasLMtt Density U./ml.) 1.3546 1.3051 1.2587 1.2080 ' 1.1549 1.1071 '" Specific Volume . (ml./g.) 0.7382 0.7662 0.7945 0.8278 0.8659 0.9033 Tempera tun 1(*0*) 1 25.1 49.9 ! 103.3 | 150.1 ! 201.7 1 254.0 1 298.2 ARXUS-l^g Density (C./ml.) 1.4439 1.4192 1.3673 1.3210 1.2691 1.2148 1.1664 Specific Volume (ml./ft.) 0.8926 0.7046 0.7314 0,7570 0.7880 0.8232 0.8573 AROCLOR 1254 Te mperature (0.) 25.1 49.9 102.9 j 150.1 : 201.8 i 05.5 1 298.2 --J-------------------- Density (R./ml.) 1.5392 1.5139 1.4607 1.4127 1.3595 1.3096 1.2546 speciflc Volume (ml./c.) 0.6497 0.6605 0.6846 0.7079 0.7356 0.7636 0.7971 HONS 058934 I-A-b-300 TABU I Cont'a DENSITY AND SPECIFIC VOLDHE OF AR0CL0R3 Temperature ! (*C.) affix 1 49.8 102.8 150.2 801.9 851.0 298.3 AROCIOR 1860 mmoKiasssssi Density Specific Volume (g./ml.) (ml./g.) t'nwiMiiwi miWMajimMtBBnrmrawmmtaamtaajs'Vma 1.5996 1.5484 1.4931 1.4386 1.3854 1.3322 0.6267 0.6483 0.6698 0.6951 0.7218 0,7506 i ! D. Ward i Central Researoh Department 1 December 81, 1948 Copied by1 re 1-20-49 ! i i I HONS 058935 xix-oa.ri' - 2iv Tf!W .i.'.v; ov w,JvT-n St. 3, Pow, ti. St. V'cmkc and H. E. Mew g. in the Purne?lwa'ia Sts to Collars Infrctrlnl end r tore-ring Che-ail stiT Vol. as. JOVi'i-4.0, (ltt.7) The following Cota ora taken fWM tables In th# sybicl-j ir.d shcml) be- tlotip critically. Specific teat fletn are o-ii of line v.ltl: ou; As'oolor flguraa. . TA1.M X sp. Ht. Arbeior. Cnl.//CL' 1840 1854 0.93 1.43 Coni !-Iplaes Vine, Vi ae. aoc. 7JL".\ 129 2740 e.7 4 Vincentfcy __ XnCot _ -614 -1903 Donelty 3C)C. 1.445 1,540 Obaervofclona vsero nclo that tho lnerocss In yioeoslt/ with preasm: wna Tory CP'ont with tho Avoclovo a:ifi A* o '.lor IBS ', ex..:.hit one of t:: hl-'d highest; ratio of licroaai. known for er. oil. i HONS 058936 I-A-s-400 MILE II ' VISCOSITY VVJtlATIOP '.YI'iM JiTiTJSSCmE Proi aura _ Pj l__ 14.2 1 00 xc 00 IE 00 C 00 8S 00 3C 00 8! 00 4< 00 SC 00 6C 00 7C 00 00 B( 100 XCO( 100 1E,( 100 14,( 100 16,1 >00 is,' >00 20, 100 28, >00 24, 100 26, 500 28, >00 30, 500 32, 500 80_C 1248 1204 125 ops -- 133 -- 181 -- 225 287 384 SD3 833' 1270 1950 2940 2740 Ops 3140 4020 5670 8740 14300 25600 40500 --- --... ---- 1348 8.7 opt -- 9.3 -- 10 11 12 13 18 17 19 21 24 30 39 53 75 111 176 300 494 816 1350 2196 1234 24 eye -- 25 -- 26 -- 29 -- 33 40 48 59 73 92 117 198 343 642 1290 2580 Cop Led by ra 7-1 !-18 ' HONS 05893 7 Temper ature 1*0 .) 84 .80 25 .10 85 .41 49 .9 99 .4 15t).S 200.4 851 .8 891 .7 I I-A-g-400 TABUS II viscosrnr or aroclors issem-iMs Kinematic viscosity (Centlstokes) 151.0 144.7 140.8 18.27 3.04 1.857 0.777 0.533 0.418 Absolute Viscosity (Centlpolses) 818.1 208.9 208.4 85.93 4.17 1.660 0.967 0.649 0.488 Temperature (<) 84..80 25.41 49.9 OCj.l 98.7 150.6 200.4 250.3 851.8 897.6 Kinematic Viscosity (Centlstokee) 585x10 505x10 96.7 95.9 5.86 1.785 0.991 0.658 0.652 0.485 Absolute Viscosity (Centlpolses) 901x10 777x10 146.4 144.9 8.59 2.521 1.349 0.863 0,853 0.608 I Copied by r 1-80-49 j D. Ward Central Research Department December 21, 1948 MOMS 050938 I-A-s-300 HOE-r^iigMOB dieedcbuc ouo-anic co vcctds F. tl. Clurlc - Qenorel Electric Company Industrial and Engineering Chemistry Vol. 89 , 698, (IPS?) i Chnrastt-rltitlaa of Dlaloctrle Mould Compounds I i Property Fantaehlor Pontashlor Hexaohloro Fti^hftchlor- dlplionyl diphenyl. diphenyl- Triohlo' Biphenyl Oxide Kotore Ku+,hnno Btnacr-3 Bum Point Sp. Or. (C/lO.b-C ) Viscosity, SOS, 'C Pour Point, *C. note, Inflox (20*0. Dlslectrls Strongt l, Kv. Dielectric Conator t (2S'C. Are formed Oases Sludging Free Add Distinction Ruuqo . *c N.F. 1.51 (65) 45 (98) 10 1.6330 40 0.1 N.E. NOhO none 360-100 N.F. 1.59 (100) 390 (37,8) 0 1.0220 40 5.0 n.tt. Tone Bone 230-850 (15 mm) N.P. 1.43 (100) 54 (100) + 15 1.6370 40 0.0 N.E. None None 250-300 (25 mm) N.F, 1.52 (100. 84 (100) 20 1.0370 40 4.3 N,E. None Nona 290-340 (25 rm) N.F. 1,46 (5) 30 (37,8) 0-10 ,,P. 1.5700 40 4.8 N.E. None Hone 200-820 H.F. - Non-rinnsahlo. N.E. - Nou-oxplocivo. Aroolor 1,354 Viaconity - llotltohoal - Centlpol saa Temperature - *C. 20 31 ! 40 j 50 J 80 | 70 ! 80 ! 90 i 100 Viscosity - cpa. 60C0 ' 3C00 700 180 . 70 38 86 19 17 Copied by re 7-18-48 | HONS 058939 St, Loulaj Dr. R, L. Jenkins Mr. 0. B, taurgln Anniston | May 25, 194S II3-0-\00 Moccro. Edgar E. Hardy - Arm1 aton A.M. Ellenburg - Anniston Paul Bogus T.H. '.Tonelook Aroalor--Sllaotlo Facts Attaolied ajre two copies of tbs No. 5 series about silastic Facta. Reoontly Dow Corning submitted tbs following Inforimtlon to ua: "311astlc la swollen gaits badly whan subjected to most organio aolsantw aush sa toluene, benzene, etc. However, our laboratory submitted a report concerning the effects of chlorl- neted diphenyl on Sllustlo, silastic Immersed In ohlorlnatad diphenyl for seventy hours at ISO'C. The change In tho physical properties wore noted and the figures Indicated that Sllnstlo la remarkably resistant to deteriorations from contact with the hot ohlorlnatad diphenyl. The changes In tho propcrtlaa are similar to those produced by hot lubricating ells and can be summed up as follows: (1) Dowering of tho hardness by about 3 points. (2) In;iroromant in the elasticity by several points. (3) Prnetlcelly no change In tensile strength. (4) An appreciable Increase In the ultBoats elongation." Western Felt Manufacturing Company at Chicago, Illinois, quoted 11110000 100 In shedt fom as follcsra: 8x8" sheet, 1/4" thick 20x20" Sheet, 1/4" thick 24x24" sheet, 1/4" thick $11.25 63.30 89.50 Apparently the greatest drawback pa the use of silicone as a gasket material for hot Aroolors la the high price of the plastics. anes Copied by ra 9-24-48 Renlgnus MGNS 056940 HAWPI.DK? aroclors in-o-ioo Gaskets - Aroo.lor and Pyranol Latter T. B. Zlea^y to H. II. Hltchenj - 9-20-48 "At a recant- meeting It was stated bjr Dr. Suits of General Eleotrlo that sill sour rubber gn rivet a were found to hold Fyranol effectively under oondltlonaj where other geekat materials gave poor performance with lespoot to freedom from leaks." .'MUSS DEVELOPMENT REPORT P. G. Benlgaua - 2-18-48 Pi'oolsloti Dio Casting Company, Cleveland, Ohio "Ball-bearing swing Joints made by Chlkean Tool Company ot Brea, California used on flexible ooimeotlone with Aroolor Installations. "0. I. Qlyntal # i! Red la excellent for sealing fluid on epplloetloc to threaded pipe." rs 9-84-46 i i i MONS 058941 H Z oo- \ m? ooc