Document k96G32oKpn6zMvQdjX5qayDQE

F m Monsanto Chemical Company At St.Louis - Roberts Bldg. Date July 6, 1956 cc R. A. Pohl - WGK Plant T. W. Dalton - WGK Plant To Mr. J. W. Graves At W.G.Krummrich Plant Reference Subject Process for Production of Aroclors, Pyranols, etc. at Anniston and Krummrich Plants. April 1955 by E. Mather I am sending copy No. 6 of the above report for the Krummrich Library. Copy No. 7 is being held in the St.Louis Library. TL C N >0 DSW 257097 STLCOPCB4061216 Copy No. 6 PROCESS FOR THE PRODUCTION OF AROCLORS, PYRANOLS, ETC. AT THE ANNISTON AND AT THE WM. G. KRUMMRICH PLANT April 1955 ---------------------------- E. Mather Distribution List: 1. Mr. J. S. Brough, London 2. Dr. N. B. Dyson, Newport 3. Mr. G. V. Taylor, Newport 4. Mr. G. V. Taylor, Newport 5. Mr. W. E. Hamer, Ruabon ^6. Mr. J. F. Stickley, ---------- Krummrich Plant 7. Mr. J. F. Stickley, ---------- St. Louis Library 8. M. C. L. file at St. Louis 9. Mr. D. B. Hosmer, Anniston 10. Spare DSW 257098 STLCOPCB4061217 TABLE OF CONTENTS TABLE OF CONTENTS (See also the subject Index at the end of the book). INTRODUCTORY NOTE I. II. III. IV. V. VI. VII. VIII. IX. X. XI. XII. XIII. XIV. XV. XVI. XVII. SYNOPSIS OF THE PROCESS CHEMISTRY OF THE PROCESS . PHYSICAL AND CHEMICAL DATA FLOW SHEETS PLANT LAY-OUT PROCESS IN DETAIL COMMENTS ON THE PROCESS CONTROL TESTS SPECIFICATIONS AND TEST METHODS: RAW MATERIALS FINISHED PRODUCTS PLANT OPERATING DATA: CAPACITY YIELDS MATERIALS CONSUMPTION SERVICES COSTS HAZARDS EQUIPMENT AMENDMENTS HISTORY OF THE PROCESS IN MONSANTO OPERATING INSTRUCTIONS ACKNOWLEDGEMENT INDEX DSW 257099 STLCOPCB4061218 INTRODUCTORY NOTE INTRODUCTORY NOTE When the MCC Aroclor process was studied in 1947 in preparation for the erection of a plant in Britain, an excellent report "Dept.246: Aroclor Process" Lyles, Soffranko and Becker, Septemoer 1946, des cribing the Plant "B" (now the Krummrich plant) process, was available. Supplementary information was collected into a report "Notes on the Plant 'B' Manufacturing Process for Aroclors" by E. Mather, April 1947, and soon afterwards the report "Notes on the Anniston Aroclor Plant", E. Mather and D. S. Havercroft, September, 1947* was written. More information came to hand from time to time, including the "Process Description for Aroclor, Dept. 246", C. H. Schwarting, J. P. Neff and J. W. Graves, November 1953, also a revised version of this by Schwarting and Schwartz, March 15, 1955* and visits were paid to the Anniston and Krummrich plants for the purpose of revision early in 1955. Havercroft and Mather briefly reviewed the Pyranol process at plant "B" in 1947* finding nothing to add to the MCC report, "Dept. A-246, Pyranol Process" Lyles, Soffranko and Miller, March 24, 1947. Subsequently the MCC report "Process Description for Pyranols and Inerteens", Schwarting, Neff and Graves, October 1953, appeared. Numerous research reports etc. are listed at the end of section VII, below. The two reports of 1953 are much more condensed than the 1947 reports which they replace; they were drawn up to give just the essentials of the process work. The present report is intended to condense all the process infor mation up to about March 1955* into the form used for MCL process reports. The Pyranol process has been included in the same report because it dovetails so closely into the Aroclor process, and the writing of a separate report for Pyranols would have involved a good deal of repetition. DSW 257100 STLCOPCB4061219 1-1 SYNOPSIS I. SYNOPSIS OP THE PROCESS Aroclors are made by chlorination of diphenyl or of "diphenyl high boilers" (either crude or refined), or of mixtures of diphenyl with high boilers. The chlorination is done with temperature control in the presence of iron as a catalyst. Chlorination is continued until the product contains the amount of chlorine corresponding to the grade of Aroclor required. The crude chlorination product is usually air-blown to remove dissolved gases, and then either is sold as crude Aroclor, or it is worked up into distilled Aroclor. The distilled product Is usually treated with Attapulgus earth. The following table shows which of these step3 are involved in making each of the different grades of Aroclors. All the operations are done batchwise, except that some of the distillation is done in a semi-continuous manner. DSW 257101 STLCOPCB4061220 SYNOPSIS OF THE PROCESS, contd. I-2 SYNOPSIS Grade Diphenyl Crude HB Distilled HB used % Chlorine Airblown Distilled Earth Treated Nature of Finished Product 1142 1242 DP DP 42 42 yes yes no yes (vac) no yes 1148 . DP 1248 DP 48 48 yes yes no yes (vac) no yes 1154 DP 54 yes no no 1254 DP 54 yes. yes (vac) yes 1160 DP 60 yes no no 1260 DP 60 yes yes (vac) yes 1162 DP 62 yes no no 1262 62DP yes yes (vac) 1262M Is 9C$ Aroclor 1262 by welg vt, 1C$ Toluene yes 1168 DP 68 yes no no 1268 DP 68 yes yes (vac) no 1169 - DP" 69 1269 1170 1270 1171 .1271 2565 4065 4465 5060 5460 DP DP DP DP DP 75# DP 25# CHB 6C^_DP 40# DHB 6<# DP 4056 DHB DHB DHB i 69 70 70 71 71 65 65 65 60 60 no no no no no no no yes yes,atm.pr. no yes, atm.pr. no yes, atm..pr no no no no no no no no yes no no yes yes, (vac) no yes no no yes yes, (vac) j no Dark oil Clear oily liquid Dark oil Yellow oily liquid Dark viscous ' liquid Yellow viscous liquid Dark viscous stickv mass Lt .yellow stickv mass Dark sticky mass Lt.sticky resin Dark crystal line solid Dark crystaline solid Dark crystal line sol-i d Flaked . Cryst. solid Flaked Flaked Black brittle resin. Black brittle resin Clear lt.yellow brittle resir jBlack brittle !resin Clear It . yellow brittle resin DSW 257102 STLCOPCB4061221 1-5 SYNOPSIS SYNOPSIS OF THE PROCESS, contd. Aroclors up to and including 1262 are usually spoken of as "liquid Aroclors"; those from 1267 upwards are called "solid Aroclors". If the first digit of the code number is "1" it signifies that the Aroclor has been made from diphenyl. If the second digit is "1" the product has not been distilled, if it is "2" the product Is a distilled grade. In all cases, the third and fourth digits give the percentage chlorine content of the product. Thus 1260 is a distilled grade, made from diphenyl, and containing 60# of chlorine. The manufacture of materials with more than 68# of chlorine was dis continued in 1949, and the equipment for making them was taken down in 1952. This stage of the process required a special gas-heated agitated chlorinator, and a special still. MCL research report 4l6A, 52/1/6, September '55, describes the production of sample amounts of higher Aroclors, but reports that the Newport plant is not suitable for making anything above 1268. Report 1151, NR 55/97/5 February 1954 describes the "topping" of 1254 for a special customer, and 25/11/54 describes the prepard;ion of resinous Aroclors for a special customer. The distillation residues may be sold as "Montars", various grades of these having been set up as shown on page 17 section III, below. The off-gas (HC1 etc.) coming from the chlorlnators is cooled, and in some cases scrubbed with light Aroclor, then either is passed to a department using HC1 gas, or else is absorbed in water to give muriatic acid, which may then be treated with carbon to bring it to "food grade" quality. The preparation of Pyranols (Pyroclors, Inerteens, Askarels) Involves at the most only a blending operation to arrive at the compositions as set out in the following table. . DS\N 257103 STLCOPCB4061222 SYNOPSIS OF THE PROCESS, contd. 1-4 SYNOPSIS Tri Chi.bz. w/w % Tri-tetra Aroclor Chi. bz. 1254 1260 Tin Tetra phenyl Pyranol 1467 1476 1478 1481 1482 1488 1495 Inerteen PPO- * TCP-mixture Inerteen PPOTTCB-mixture 40 - 100 25 - 40 10 40 - - - 60 0.125 55 100 45 0.125 _- - - - - 75 - -_ - - 100 - _ - - 60 -- _ 90- - "- 60- - -- 55 45 - - Glycidylphenyl ether 0.20 0.20 MCL Research Pro 5res-s report 347D, 51/141/12, June 1952 deiscrlbes certain variants of these 1 Pyranols are products for the (American) General Electric Company. Pyroclors are the MCL products corresponding to the Pyranols. Inerteens are made for Westlnghouse. Askarel is the MCC trade mark. The trichloro-benzene and the tri-tetra chloro are used to increase the fluidity of the Aroclors without seriously harming their electrical qualities. MCL Research Progress Report 1151 NR 53/97/8 suggests that TCB increases the solubility of tin-tetra-phenyl in the Aroclor. The tin-tetra-phenyl, and glyeldyl phenyl ether are "chloride scavengers" as discussed in section VII below. * PPO denotes phenoxy propene oxide, a synonym for glycidyl phenyl ether CgH*. 0 CH2 CH*p DSW 257104 STLCOPCB4061223 II. CHEMISTRY OF THE PROCESS II - 1 CHEMISTRY OP PROCESS The main reaction, in the production of Aroclors, is a simple replacement of hydrogen by chlorine, but the product of the---^ chlorination contains trace amounts of halogen-containing; byeproducts, which are less stable than the direct ring-substitution products; for example, they will give off HC1 on being heated in the presence of metallic aluminium. (See the "Inorganic Chlorides" test, pages 77 - section IX, below. See also the discussion on pages 6 - section VII.) Taking the atomic weights: H = 1.008 C - 12.01 Cl = 55.455 we have for direct substitution: M..wt. $ Cl Compare Diphenyl C12H10 154.20 Trichlorodipnenyls C-^H^Cl^ 257.54 41.5 Arcelor 1142, 1242 (42$Cl) Tetra C12H6C14 291.99 48.6 Aroclor 1148, 1248 (48$) Penta Hexa Hepta . C H Cl -io 0 C12K4C16 526.44 560.88 54.5 59.0 Aroclor 1154, 1254 (54$) Aroclor 1160, 1260(60$) C^2H3C17 595.55 62.8 Aroclor 1162, 1262 (62$) Octa C^HgClg 429.77 66.0 Ennea C-^HCl^ 464.22 68.8' `Aroclor 1168, 1268 (68$) Decachlorodiphenyl C,,2Ci10 Terphenyl C-^H.^ Decachloroterphenyls Cl8K4C110 Undecachloro C^gH^Cl^ 498.67 71.2 Aroclor 1171, 1271 (71#) 250.29 574.76 61.8 Aroclor 5060, 5460 (60$) 609.21 64.0 DSW 257105 STLCOPCB4061224 CHEMISTRY OP THE PROCESS, contd. II - 2 CHEMISTRY OP PROCESS The conditions of chlorination (high iemperature>_and local exce^s--^ of chlorine) are such that,for example,Arcelor(126p eontaining("60^, of chlorine,corresponding about so Ci2H4CI6.> will" certainly contain considerable amounts cf C^H^CI^, c12h3c17^ etc. Further, there will probably be a very large number of Isomers of, for example, C12H4CI6 Tnis complexity of composition has the advantage of depressing the melting points of the various components, so that materials of high molecular weight are obtained which have low vapour pressures, but which are still fluid at'ordinary temperatures. It is evident, however, that,though blending, say 2 parts of Aroclor 1260 with one part of Aroclcr 1242, would give a product containing 54$ of chlorine, such a produce would not necessarily be identical with Aroclor 1254 made by direct chlorination of diphenyl to 5^ chlorine content. This is of practical importance because partial crystallization of liquid Aroclors, which has occured, and wnich has given rise to customer complaints, has been ascribed to preponderance of one component which chanced to be sparingly soluble In the general mixture. See pages II- section VII, below. Chloride Scavengers. See the discussion of the action of scavengers in Section VTI, below, pages 6-. Heat cf Reaction (chlorination). Judging by literature information on similar reactions, the heat evolution in the chlorination must be around 40 kg.cal. per g. atom of chlorine combined, (i. s. about 20 kg. cal. per g. atom fed in). The heat of evaporation of Aroclors. Troaton's rule (g. cal/'g.mol = 21 x B.Pt. C. abs) gives, for example, for Aroclor 1260 of M.Wt.about 560 and mid B.Pt. about 395C.(668abs) 14,028 g. cals, per g mol, or 39 g. cals per gram. DSW 257106 STLCOPCB4061225 III. PHYSICAL AND CHEMICAL DATA Ill - I Phys,&Chem. Data Physical Constants of Diphenyl Compiled by W. P. MetznerDates February 12, 1943 Corrected? June 22, 1943 . Correcteds Jan. 11, 1944 _________ _________ \ 5>--\ Beilstein V-576 NAME SOURCE DATE Formula Appearance TJ U 6p c ? MonoclJnic Molecular Weight 154.20 ' Boiling point at j60 mm 255 C. Boiling point at 10.4 mm 118c. Crystallizing point 69.03C. Melting point 69 C. Solution point Specific Gravity at 77/4 C. 0.9896 Specific Gravity at 2C/4C. 1.041 Refractive index at 77.1C. D = 1.56822 Viscosity at 100C. 28.8 Say. Sec. Surface tension at 129.2C. 29.5 dyne/cm Solubility in water at 80C. Insoluble *Nctes Files cf' W. F. Metzr.er, St. Lculs Chem.Rubber handbook 1941 1942 Chem. Rubber handbook Int.Crit.Tables 1928 Swann file #137* Swann curves * 1935 1934 Int.Crit.Tables 1928 Int.Crit.Tables 1928 Int.Crit.Tables 1928 Int.Crit.Tables Swann File#157A* 1928 1930 Int.Crit.Tables 1928 Dqw 1943 DsW257107 STLCOPCB4061226 Ill - 2 Phys,& Chem. Data III. PHYSICAL AND CHEMICAL DATA, contd. Physical Constants of Diphenyl, contd. NAME SOURCE DATE Viscosity at 70C. 31.2 Say. Sec. Swann File #137A* 1930 Solubility In Abs. Ale# Ale.at 19.5C. 9.98 g./lOOg.solvent Seidell 1941 Solubility in 100# Methanol at 19.5C. Benzene at 27.9C. 6.57 g./lOOg.solvent Seidell 137g./I00g.solvent Seidell 1941 1941 Heptane at 26.5C. 20.1 g./lOOg.solvent Seidell 1941 Plash point P. 235P. - closed cup Ind. & Eng.Chem. 255 #P.- - open cup 32,882 1940 Fire point F. Heat of combustion Kg-cal. (15) 124C. Dow 1943 per gm.mol=1504.4 Int.Crit.Tables 1928 Heat of formation Latent heat of fusion Latent heat of vap. at 69.2C. 28.8 gm-cal.per gm. (53.1 BTU/lb.) Lange Handbook 1937 190.9 B.tu.per lb. Swann Pile #137A* 1928 Specific heat at 40C. (solid) 0.387 cals/g 1.6l joule/gm. / Int.Crit.Table s 1928 Critical temperature Critical pressure Dissociation constant -. - __ -- -- Pounds per U.S.gal.at 77c 8.23 lbs.per gal. Swann Pile #137A 1930 Toxicity (l) Dr.McLester .Anniston Plant Report 1937 (2) Percy May "Chemistry of Synthetic Drugs"- 3rd.Ed.p.19 NOTEt Piles of W. P. Metzner,St.Louis. DSW 257108 STLCOPCB4061227 III. PHYSICAL AND CHEMICAL DATA i . Diphenyl Specific Gravity: 0.992 at 75C/4C. The Swann Chemical 'Company'bulletin < data on diphenyl Viscosity of Diphenyl (from Anniston F. Centipoises 160 1.439 170 1.309 180 1.208 190 1.114 200 1.034 220 0.901 250 0.752 300 0.374 550 0.459 400 0.37^ 450 0.313 482 0.283 Specific Heat; (from Anniston files) F. 200 300 400 500 600 700 800 900 1000 B.t.U./lb. 0.416 0.470 0.547 0.616 O.658 0.679 0.686 O.690 0.696 Ill - 3 Phys.& Chem. Data DSW 257109 STLCOPCB4061228 III.PHYSICAL AND CHEMICAL DATA, contd. III - 4 Chem. & Phys. Data I. Diphenyl, contd. Another record gives the following values for liquid diphenyl: C. Sp. Heat cals./gram 100 0.360 150 0.380 200 0.412 250 0.460 300 0.518 350 0.575 400 0.610 450 0.625 Vapour Cp = 0.460 250C. 0.625 450C. (D. A. Roper, Design Data for Units 4 & 5) Density of Liquid Diphenyl (from Anniston files) grams,/cc 75 0.9885 100 0.9695 150 0.9294 200 O.8885 250 0.8470 500 0.8010 550 0.7510 400 0.6918 450 O.618O Heat of Vaporization: 65.4 g. cal./g. at 258.5C. DSW 257110 STLCOPCB4061229 III. PHYSICAL AND CHEMICAL DATA, contd. Ill-5 Phys,,& Chem. Data 2,, Distilled High Boilers Santowax *R contains about 1# diphenyl 10# ortho terphenyl 46# meta terphenyl 21# para terphenyl 22# triorthophenylene, (Anniston Pinal Report 1942) quaterphenyls etc. Upper hold point Lower hold point 137-143C. Changed ) 45-60C. Sept.23/47) 137-145C. 45-63C. The density of the Santowax may be assumed to be the same In both the crude and distilled form. Viscosity also Is the same. Specific Gravity of Crude Santowax; l40C. 175 215 300 1.026 1.000 0.98 0.964 (est. from curve of other points) Viscosity of Santowax R 155C. 225 32.4 Saybolt Universal Seconds 28.5 " " " Molten Santowax flows about like water at 25C. (A.M.Ellenburg1s letter January 6, 1949). (Probably 250C. was Intended). Specific Heats (estimated) Solid Liquid 0.4 0.5 . Latent Heats (estimated) Fusion 63 B. t'. u ./lb. Vaporisation 140 B.t.u./ib. DSW 257111 STLCOPCB4061230 III. PHYSICAL AND CHEMICAL DATA, contd. ill-6 Phys. & Chem. Data 2, Distilled High Boilers, contd. Santowax R, contd. Bolling Range; 360-450C. Flash Point; Cl.open cup 191C. Flame Point: Cl.open cup 238C. Another account gives Flash Point 190C; Flame point 220C. Values assumed In the design of the Santowax still at Anniston: Specific Heat Heat of Vaporization Viscosity at 250C. Viscosity at 350C. - 0.5 - 140 B.t.U./lb. - 5 centipoises * - 2 centipoises * * (Mr. Ellenburg said these values were too high). Terphenyls "Hold Point" B.Pt. at 30 mm Crude ortho (Santowax 0) Crude meta (Santowax M) Crude para (Santowax P) m - p eutectic Ternary eutectic 55 - 55C. 83 - 85 C.) , , 209 -213*0.) nlXtUre ,84.8*0. about 74C. 205C. 240#C. See also Monsanto Technical Bulletin #P-103> January 4, 1947 issue, for the properties of the separated crude Isomers sold. 3. Trlchlorobenzene Dr. Jenkins, January 27, 1954, refers to Ind. Eng. Chem. 39_ (1947) p, 517 for vapour pressure data. DSW 257112 STLCOPCB4061231 III. PHYSICAL AND CHEMICAL DATA, contd III - 7 Phys. & Chera. Data Aroclors The main characteristics of the Aroclors are given in the following table: Grade M. Pt. c. Specific Gravity Sp. Gr. Viscosity coeff. Saybolt per C. Seconds Distilling Range *C. 10 - 9# Pour Hold Point Point *C. C. Softening Point ASTM 1142 1.548 to 1.555 0.0009 65/15.5*0. . .. 1242 1.558 to 1.548 0.0009 50 to 53 65/15.5C. at 54.5*0. 1148 1.412 to 1.415 0.0009 65/15.5*C. 1248 1.404 to 1.414 0.0009 73 to 80 65/15.5C. at 54.5*0. 1154 1.500 to 1.510 0.00095 65/15.5*C. 1254 1160 1.495 ta 1.595 9,90095 ; 44,5 to 47.5- 365 to 390 8-12 65/15t5 at 98.9*0. 1.558 to 1.565 0,0010 90/15.5*0. 1260 1.550 to 1.560 D.0010 90/15.5P. 72 ta 7? 385 to 415 26-34 at 98.9*0. 1162 1.582 to 1.587 0.0010 90/15.5#C. 1262 1.572 to 1.585 0.0010 88 to 100 90/15.5#C. at 98.9*0. 1262M 1168 1268 1169 1269 1170 1270 1171 1271 504C. min. 2565 4065 4465 5060 5460 160 ta 210 at 130*C. 145-165 135-160 225-250 225-255 285-300 66.0 to 72.0 66.0 to 72.0 110.0 to 115.0 100 to 105.5 See also Phosphate Division report 171-102 "Highly chlorinated quater phenyls" sent to Mr. Hamer, March 12, 1948. DSW 257113 STLCOPCB4061232 III. PHYSICAL AND CHEMICAL DATA, contd. III-8 Phys. & Chem. Data Other properties are listed in Section IX, Finished Product Speci fications. MCC Bulletin P-115 gives the following data not included in either of the foregoing lists: -- General description of the Aroclors: (non-oxidising, permanently thermoplastic, chemical inert, will not burn, compatible with most non-hydroxyl!c solvents, good electrical properties and fire resistance, _ adhesive, and non-drying). Evaporation loss data, # loss in: 5 hours l65C. and 6 hours 100C. Flash point Fire point Refractive index. Corrosion data Specific heat 'c. dynes /sq.cm. Surface tension (Aroclor 1254 )< 25 80 50.5 44.0 100 42.0 Thermal conductivities Solubility data for many compounds Vapour pressures (semi-log chart) Viscosity variation with temperature (use of V.I. improvers suggested). Variation of Dielectric constant with temperature Compatibility with lacquer components, structural materials. etc. Suggested uses. The paper by Baxter, Vodden and Davies of Ruabon, J. Appl. Chem. 5 October 1955, page 477, gives a method of determination of thermal conductivity of liquids in general. MCL Res. Prog. Rpt. 555E, 51/91/2, October 1951, makes comparison between Aroclor 1248 and mineral oil as cooling media. Heat of vapourisation is discussed on page 2, Section II, above, also the Heat of Chlorination of Diphenyl. DSW 257114 STLCOPCB4061233 III. PHYSICAL AND CHEMICAL DATA, contd. III-9 Phys,,& Chem. Data Vapour pressure curves for some of the Aroclors are given on pages 72 - 75 of the report by Lyles, Soffranko and Becker, November 1946. More recently vapour pressures for samples of Aroclors 1242, 1248 and 1254, measured by an effusion method at temperatures below 100C. were given In a report from the Southern Research Institute, Birmingham, Alabama. (Report No. 1, project 526, to MCC February 4, 1954). All these data are shown In logarithmic form on pages III-9a&b below. Dr. Roebuck, then at Ruabon, In a letter dated June 8, 1955* recommen ded that vapour pressure measurements should be made by a static method, rather than by effusion, because the Aroclors are mixtures of compounds of different volatilities, and the effusion method might cause Some fractionation. MCC progress reports under Job I7I-IO89, dealing with the vapour pressures of the different Aroclors, and with the measurement of the concentration of Aroclors in air, were sent to MCL at various times, for example June 17, August 15, and September 17, 1955* A final report under this job number was promised July 16, 1955. Newport Plant Technical Committee, December, 1953, recommended investigation into combustion methods of determining the concentration of Aroclors in air. Mr. Benignus, of St. Louis, September, 1953, discussed the dangers of using Aroclors in indoor paints. Dr. Newman at Newport, September, 1953, had files on the question of Aroclors in air. See also under "Hazards" in Section XI, below. Dr. Jenkins, January 27, 1954 said that for th Pyranols containing 53$, or more, of Trichlorobenzene, the vapour pressure of the Pyranol might be taken as equal to that of TCB alone up to about 150C. Above that temperature the vapour pressure of the Aroclor would begin to show up. Viscosity-temperature data for Aroclors are given on pages III-10, and III-ll, below. MCL progress report 1152, DF 5^/l^/9, September, 195^, reports the viscosity of Aroclor 2565 from 100 to 130C. Report 1152, DF 52/26/6, August, 1954, discusses the viscosity, and the viscosity index of a tintetraphenyl blend of Pyranol. DSW 257115 STLCOPCB4061234 C III 05 - e* STLCOPCB4061235 *_____ oq III - 9b h m i \ 4 \ y rlr X 10 to th r STLCOPCB4061236 STLCOPCB4061237 10 to th e j iiu 'h . M h iir e e n t e>l, o III-10 III-ll Phys.& Chem. STLCOPCB4061238 j^ l<7 r - , > i| o t <) | III-12 Phys.& Chern. Data ' III. PHYSICAL AND CHEMICAL DATA, contd. Specific Gravity-temperature data are given on page 11 of MCC Bulletin P-115, also on pages 13, 14 and 15, of Section III, below. The coefficients of fall of specific gravities of the Pyranols with increasing temperature in the range between 45 and 85C. are as follows: 1467 and 1488 - 0.001 per 1C. 1495 0.00285 per 1C. (Lyles, Soffranko & Miller page 43) DSW 257120 STLCOPCB4061239 III. PHYSICAL AND CHEMICAL DATA, contd. III-13 Chem.& Phys. Data Specific Gravity of Aroclors at Various Temperatures For 1242 Temp . C. 60 65 70 75 80 85 90 95 100 Sp. Gr. 1.347 1.344 1.338 1.335 1.332 1.329 1.324 1.319 1.315 Lbs. per Gallon (US) 11.23 11.20 11.16 11.13 11.10 11.07 11.03 11,00 10.96 1248 60 65 70 75 80 85 90 95 100 1.413 1.410 1.403 1.400 1.397 1.39^ 1.390 1.385 1.381 11.78 11.75 11.71 11.68 11.65 11.62 11.58 11.55 11.51 1254 or GE 1476 60 65 70 75 80 85 90 95 100 1.505 1.500 1.495 1.490 1.485 1.480 -1.475 1.470 1.465 12.55 12.50 12.46 12.42 12.38 12.34 12.30 12.26 12.21 contd... DSW 257121 STLCOPCB4061240 III-14 Phys,,&Chem. Data III. PHYSICAL AND CHEMICAL DATA, contd. Specific Gravity of Aroclors at Various Temperatures (contd. ) For Temp. C. Sp. Gr. Lbs. per Gallon(US) 1260 or GE 1482 60 65 70 75 80 85 90 95 100 1.584 1.580 1.575 1.570 1.565 1.560 1.555 1.550 1.545 15.21 15.17 15.15 15.09 15.05 15.01 12.96 12.92 12.88 1262 60 65 70 75 80 85 90 95 100 1.604 1.600 1.597 1.595 1.588 1.582 1.577 1.572 1.568 15.40 15.56 15.52 15.28 15.24 15.19 15.15 15.11 15.07 DSW 257122 STLCOPCB4061241 L500 STLCOPCB4061242 III. PHYSICAL AND CHEMICAL DATA, contd. III-16 Phys.& Chem. Data . Solubility Data MGC Bulletin P-115 includes data- on the compatibility of Aroclors with numerous solvents. MCC report 2949, October 28, 1955, deals with the compatibility of Aroclors etc. with mineral oils. Newport complaint N 464, January 1954, arose from the alleged incom plete solubility of 4465 and 5460 in Dutch Shell Co.'s Risellaoil. See also the discussion of "Partial Crystallization" in Section VII, below. The solubility of gases in Aroclors is of importance in connection with the use of Aroclors as lubricants in compressors. Reference is made to Monsanto Bulletin P-128 on this use of Aroclors. MCC Central`Research Report 545 "Studies on Light Stability etc. of Aroclors" White and Ruehrwein, January 1949, states that the solu bility of oxygen in 1254 at 25C. is about 1 x 10"^ moles of oxygen per gram of Aroclor. On December 29, 1953, Dr. Gardner enquired for data on the solubility cf gases in Aroclor up to 7000 pslg, but MCC could not supply any data. The following MCL Research Reports deal also with questions of compatibility: - Job 1152, 51/141/20 etc. "Effect of Pyroclors on electrical wire insulation"-- softening and loss of break-down strength -- Pyroclors unharmed.. See also under "Gaskets" in Section XII, below. Job 1151, DP 55/86/1, September 1953. "Solubility of methyl anthraquinones etc. in Aroclors". Job 1151, NR 55/97/8 "Solubility of TTP in Aroclor 1248" Also MCC report 2272, "Solubility of Aroclor 5^60 in various solvents", Wade, December 1948. Variation of Resistivity with Temperature It was stated in a report on Complaint NJ/21, November 11, 1954, that a volume resistivity of 17 to 47 x 109 at 120C. corresponds to about 85 x lO^ at 100#C. (Aroclor 1254 - - MCL Specification 500 x lO^ ohm/cm3 minimum at 100C.) DSW 257124 STLCOPCB4061243 III. PHYSICAL AND CHEMICAL DATA, contd. III-17 Phys.Sc Chem. Data ' M 0 N T A R S (1946 data) Softening Plash Fire Penetration Chlorine Iron Calcium Acidity Irade Point Point Point 25Og.weight % % oxide mg NaOH ASTM C C. C. at 75C. % per gram 1 - -- - -- - 2 - -- - - -- - none 3 130-160 298 at - 51.6 0.31 3.47 SI. 343 basic 4 191-208 - - 0 - .- - - 5 165-180 - 2 cm x 10""2 per minute 57-59 0.12 1.6 max. max. 6 168 -- - 599 0.13 2.0 - 9 140-160 257 304 - 0.18* 0.21 0 0.104 10 139 - 47 cm x 10~2 per 5 secs. - -. - * Montar #9 is the residue from the diphenyl process; - data on it included here only for convenience-. No data found on Montar #7. - DSW 257125 STLCOPCB4061244 <CNO v lNO. CN| <: aco STLCOPCB4061245 12 HCl 2 .0 2 .0 lo s s fro m a b s o rp on syste m a t in te rv a ls , w o rk in g lo s s e s o A ro c lo r; X^ * --'--' O ft 0 ct T3 ct 1-- ft *- CL ft Ct H* CD O' o C ct ro NJ1 Ct 3* ft 3 a ft a ct p CR ft 3 Q, U> Cn 3 S' ft * ft ft t-*> 3 H> 3 CR ft ct P 33 3 > ON U> CD NJ1 NO M U) ro 4=- VJ1 o Xr -4 45T -ter -4 -Cr NO 4r CO w <-- 00 * U) ro NO M ro \j> NO H* ro O VO Ui *o M o CD vn Mo CD U1 U3 M O ro Cn O Cn ro Rh VO Moo V-* O o U1 oIo-* M U1 O >- NJ1 W Oo o ON --* o X U1 ---- > H 1 ct 3 ft ct ft p p *c1t `2e 3* I--1 OR 3 a o p i o' o 3 p ct ft NO -Cr CD t- ro ro CD ro ON CD ro ro o ON CO o ON ro ro oO o Ut o Cn 'O o NJ1 O o NJ1 o o ai > 1 oft y-> O NJ1 O vn o M o 00 n_h NJ1 M O CD Cn vjn Mo ro NJ1 ro 4=t- O O M O O M O M Moo b on o NJ1 O 3 l-* 0 h1* 3 ft NO ro M -t i -0 p ft 4r ft O TJ 3 ft 3 ON U> CD v_n 4r -4 1 P 4= o ft --eg--------pc -4 p ft XT ft ON -3 p I-* ft ft -pr M U0 45T >--1 CO -fir O LO M o -3 i p ft ft 3 8 ft Oft --< ct > C 1 TJ ft TJ 3 p *i ct 3 O H X ct 3H* Hft 0) CD ct ft TJ ft ft H-> 3O ct O * a*hCO ct t- ft CD CO O O3 <T > ON 3P"1* OOM a o"1 t- O M U) I-* 3 4= a 2> c Ooct -J ft M M Ct O NJ1 M ON M -4 3 M ct ftCD 3* a M CD NO 3ft ro <p< O 1ft o3 ro ct ftm 3* ft ftro ct ro ro CO ro pr ro -J ro NO uoi CO H> CO ro u> XT 03 TJ 3fftt* O< ct ft 28 DSW 257127 STLCOPCB4061246 From f CM Trichlprooenreng CT* o%u.( ' o%u.q STpre Tanks Pwmp^ P-o*u* " OS*i DSW 257128 STLCOPCB4061247 I l*70 lull - <L FLOW SHECT QF EQu i on s* f^Ranols and INE R" E NS Pou^My I % ~0 TV Aroclor btod*r CT-OfTq fluftifl D ' O l 7 5" 7 a^o ji iTtr at* F ' Ol >5 for Pyran oi t * 6' Ground ltyl DSW 257129 STLCOPCB4061248 n T>\ ftfre r> y( Store Tanks ' o 7* % - Th*<} CT- 07*7 Pvh DSW 257130 STLCOPCB4061249 CVt^onn^tOrt CT* o-T^ OuS 0 1 5O o ii ti o Cnlonnot'' ftjwKi p*--$*ooS4te7oi<n7T feOChl^ CyClonfS CohnunS CT* etaiq T'tr-oao* oUto CT- q-riq -Oil*' '07*'- on fco -CM 1 vx - 012-5^ . - lOI frlor* CT-OiOf Got, Chtv^bcr CTo* H* ^cruPbqrT** CT* o7u o*ars* O0 7lD5*l^ CT- 07*** -07** Mill Con-fCvor V-0***oi** V-o*****- o*r r wei^Kir^ kj nAr !ev*Tor D *011 L-Ofti *-*l ^CfvbbcrTfc- C^wnh* p- 0096717545 Atr feto*** Th% CT- 0750 CT02*fe * DSW 257131 STLCOPCB4061250 CT 01*5, Tk 'kb n E jtctor FLOW SHEET OF aroclor EQUIPMENT. iff *7 '** tf-3 fUw Sk tt7 of Plaer____\Ullk. Still PvmJb P" osqb 'O-ftT Stl\ C/d on CT'Om-uS Wultv Tkv CT-^bb Wn!w P-OM* Pvmf, Poib5* Coke ^crvfeB.rj CT-07SJ CT-ol 9* Pvt*' p P-0971 #n7 Aroclor Store Tk% Batch TVs CT- Ot&S oTfcq omo CT--0P7l%**o F\*nhS p.oMl 0*1 > OS^ Crvd Aroelor St-Tfct CT-o7**-q 07**t r-foH-^err *o* f' a^hrvi/ 11 DSW 257132 STLCOPCB4061251 V, PLANT LAY-OUT V-i Plant Lay-out The equipment at the Krummrich plant (formerly plant "B") had been fitted into a tall narrow building remaining from the 1914-1918 war period. The still and flaker for solid Arcclors, and some of the units of equipment for Pyranols, were accomodated in a lean-to building against the West wall of the main building. Store tanks, and the HC1 absorption and treatment equipment were located in the open air alongside the building. The following drawings, which were sent to London, April 25, 1947, relate particularly to the lay-out of the plant. ' P 570 P 573 F 374 F 386 C 815 E 877 E 6838 C 6942 c 6943 E 6952 D 6956 D 10292 . The building had been constructed with most of its structural steel outside the brick shell -- a special war-time requirement and the external steel work is now very badly corroded, also the roof of cement slabs has corroded away near the vent stacks, letting in the rain, While the interior of the building was dry, there was very little corrosion of steel equipment and internal platforms, out the moist conditions now prevailing appear to be having a very damaging effect, A proposal has been made to roof the building with trans lucent plastic, and to do away with the-windows in the side walls, because they require so much upkeep. A fourth chlcrinator was installed since those drawings were made, and more recently a fifth one has gone in. DSW 257133 STLCOPCB4061252 V. PLANT LAY-OUT, contd. V-2 Plant Lay-out The equipment for making solid Aroclors fell into disuse in 19^9, and was pulled down in 1952. The equipment at the Anniston plant is laid out in, and around, a rather lower broader building, with the chlorinators and their pumps ir. an open (roofed) structure nearby. Here again, most of the store tanks are outdoors. The HC1 absorber also is outdoors, at some distance from the Arcelor building. There is no equipment for making solid Aroclors at Anniston. Both plants have railway tracks alongside the main building. DSW 257134 STLCOPCB4061253 VI. PROCESS IN DETAIL VI - 1 Process in Detail ' Handling of Diphenyl and High Boilers Diphenyl and the Diphenyl High Boilers are made at Anniston and the Anniston Aroclor plant is supplied mainly by inter-departmental transfers. The Krummrlch plant Is supplied mainly from Anniston, but has been supplied to some extent also by purchases. Diphenyl arrives at the Krummrlch plant in rail cars, which are fitted with internal steam coils, and on arrival the material has to be melted with the usual precaution of first melting a hole down to the bottom of the tank by means of a bayonet or vertical coil to prevent develop ment of pressure from the main coil of the tank, (note the possibility of development of full mains pressure in the shell of the rail tank if the coil should leak, or if there should be water on the bottom of the tank, note also that the diphenyl expands on being melted). The molten diphenyl is then discharged over the top of the tank (by the use of dry compressed air) into storage tanks CT-0748, -0749 and -0347, which are underground in the open air. These tanks are automatically maintained by steam heat at about 90C., and their connecting pipes and vent fittings are steam traced. Their temperatures are automatically recorded. The diphenyl is pumped from them by submerged pumps P-O585, -0592, to the overhead feed and measuring tank 0T-O767. This tank is steam jacketed to keep the contents at 85C. or a little higher, by hand control, and it has overflow lines, at the 1800 lb., 2800 lb., 3600 lb., and 4000 lb. levels. The overflow lines are steam traced and the over flew can be directed to whichever store tank is in use. Prom CT-O767 the diphenyl charges can go by gravity to any of the five chlorlnators CT-0744,-0745, -0833* -0l83,or (No. 2, 1, 3 4 and 5 respectively). and -Ol4-32 At Anniston the arrangements for measuring the diphenyl charges are less convenient; the charges are simply pumped from a tank on the floor of the building, the amount being measured by dip in the tank. The same tank has to be used alternatively for Santowax charges, so that it has frequently to be drained out into shallow trays, a pro cedure that Is troublesome, and not very safe in view of the inflammable nature of the vapours. DSW 257135 STLCOPCB4061254 VI. PROCESS IN DETAIL, contd. VI - 2 Process in Detail Handling of Diphenyl and High Boilers, contd. The crude and refined diphenyl high boilers,when, formerly used at the Krummrich plant,arrived there in lumps in 75 lb. paper bags, or as material which had been melted into 550 lb. barrels. The barrels were broken open and the block of material cut up with axes as needed to get it into the melter CT-0765. The melted material was blown from there,by air pressure,to one of the chlorinators. As far as possible, only the chlorinator CT-0745 was used for the higher Aroclors, to prevent cross contamination of the different kinds of Aroclors. Before a chlorinator was changed to the production of Aroclor 5060 or 5460, it had to be rinsed through with distilled high boilers. Throughout the handling of diphenyl, care must be taken to have the pipe lines hot (M. Pt. 69C.) and to make sure that the tank vents are not blocked with sublimed material. If the charge in the diphenyl measuring tank is allowed to cool, crystallization may occur n the walls of the vessel, resulting in incorrect charging of the chlorinator. 'Handling of Chlorine At the Krummrich plant, the Aroclor department is supplied partly with revapourised liquid chlorine (the chlorine simply being allowed to evaporate into the chlorine main, from the liquid chlorine store vessels which are sprayed with cold water; the vapourizer CT-07^5 is no longer used), but the main supply is direct cell gas, dried, and compressed to about 50 psig. Actually, the Aroclor plant is able to take all the "snift" gas, and low-grade chlorine generally, without ill effect, though any considerable proportion of air in the chlorine may confuse the operator because the chlorinators will not show a heat evolution corresponding to the flow of gas. Air dilution also is detrimental in the HC1 absorbers. D3W 257136 STLCOPCB4061255 VI. PROCESS IN DETAIL, contd. VI - 3 Process In Detail Handling of Chlorine, contd. Conditions are similar at the Anniston plant, though the liquid chlorine used there is purchased material, which is passed, as liquid, into a simple vapourizer, made from old gas cylinders set vertically in a water bath automatically controlled at about 95 C. The cell gas at Anniston is compressed only to about 15 psig, which is inconveniently near to the back pressure of a full chlorinator, so that the gradual increase of head of material In the chlorinator as the volume and density of the charge increase during the chlorination, necessitates close attention to the regulation of the flow of chlorine, and to the sharing of the chlorine between up to eight chlorinators, some at different stages of chlorination. Ordinary chlorine valves have been used for this regulation, but more recently, "Durco" cocks, with Teflon lined bodies, and Durimet plugs, have been found more convenient at Anniston. ' There are no flow meters on the chlorine feeds at Anniston, and the operator hasto be guided mainly by the temperature behaviour of each chlorinator. At the Krummrich plant there Is a branch from the chlorine main for each of the five main chlorinators (formerly also one for the gasfired chlorinator). Each branch starts with a rising stem control valve, followed by an orifice plate (1.1 round-opening) with an U. gauge containing 60 Bd HaSOi|, then there is a pressure gauge on a branch line. The main pipe then rises to a level above the top of the chlorinator, and falls again to the inlet fitting, low down cn the side of the chlorinator, where there Is another rising stem valve. The U tube of the H2SO4 manometer has a cross connection near the upper ends of the two legs, this connection being closed by a stop cock (A) when the manometer is in use. There are also two stop cocks (B & C) one at each end of the U tube. When the flow of DSW 257137 STLCOPCB4061256 VI - 4 Process in Detail VI. PROCESS IN DETAIL, contd. Handling of Chlorine, contd. chlorine is first to be started, B and C are closed and A opened, otherwise the acid may be jerked out of the U. Then B and C are opened, and A gradually closed. Between batches, B and C are left closed, and A open. -------------------------------------- - Bk -* A :: c See also the description of the flow controller to No. 5 chlorinator on page XII-5 below. Chlorination The chlorination procedure is essentially the same for all Aroclors up to 68chlorine content, so there is no need to give a separate description for each grade. The charge of diphenyl has to be a little less for the more highly chlorinated grades, because the increase in volume during chlorination is greater, also the time temperature schedule, and the end point of the chlorination have to be varied, all as set out in the table on page 5, Section VI, below. Note, however, that chlorination is often started at as low a temperature at 100C. gaining a little cooling effect, and so saving a little time. DSW 257138 STLCOPCB4061257 o ON O ON O CD o o U> ON O o ON CD u> CD ON oo oo O o o ro O o o o o 00o o ON -5 CO NO ro o ro M -J o U1 ft S3 W) M 3* et O 0 0 H 3 0 QO 0 3 a T3 M a) M H* H*0D m3m 0 3 3^ H ft < fto M O3< 00 I 3 O H* fo 3 I ON M ft H oo CD UN ao (to o O ct M t--* a> t-- M3 O Oh* 3 a a a ft )- O ET M 9 UN 30 O ct -J O -J ft 3 OM .3 w O ft M O 3*. M <* UN 330 ft O ct ONO CD a io 3 *3 OM 3-- Ml O o 3M Ct M ON O CD -> ft M 3* CD JN 3 13 M m3 OB UN M M 0 ft O B S' o COfi M3* B ro O* m . O 1 et O a < ui CD O B t a eMO O ft < M 3^ B M 3 9 ^ UI ct BO OM 3 ro O S' ** ft 3* 9M 3 Ul O "3 ft M M O S' tt'H* 9 UN UN 3 3 ft O o o a& o ro o Ui o o -g 00 oo CD o UN oO ON ON CN> vO o UN oO OHOHOCB 9 CD O O Q ft-a 3* r< 9 <^ 5^~vui p1 an h53 1 7j hO H # CD CB et A 9 9 9 3 mO O ft CD 3* I 0 3 B CD 3 3 *3 ^ 9 0 *0 M B h*3 het M O ft 3 CD ON h* M a. 3 O 3 3 o an 3 *-03 BOB a 9 B O B ctD ft PC' ct B I--* CD CB ft -* 3 H O M H* B 99 O I >3 9 3 M O M O 3 3 ! 3 (N0 H 9 < *3 CD 3 3 ON 3 rt a >k <3 M 9 < M XX ft O 33 0 0 9 B ft 3 ct O CD 0 3" ` ft et cd . 3 M CD ft 3 9. JQlH*H H* M H* O CD CD .O 3* CD wO* C CD ft B CD ft 3 * CD <D 3 H S' 9 3 ct a 3 < 9 3 3 0 0 J 35JSM 9 O <D n 3 3 a h B NO C 3 CD 3* --Jrt cd a 133 "l* , S' ft *3 O 3 Ct 0 ft 3 CD CD 3* CD C . CJN H> 3 B i* O *0 _3' &a33- ,, i* O rz\i O 9 O CD3 3 ft 3* 3 . T3 S' T3 B 1 O ft mb O O ft 3 O M CD O M3 3 Ot O 3 1 3 O <D ft 3 O' ft o B O Co o rt O t O Ct O 3 3 " 3 03 *S 3 et 1 Ct M ?! 0 det 3 ro CD ro 0 o*O 9 JN 3* o -U 0 JN 3* M 1 M 1 M o o ro o fOO vo 3 B UN M Onm M 3 3 3 3 B O B ab H* Ct " H 9 ( 3 f\J 3 too* 3 3cr m S' 3 3 m_ B a a 3* fOM 3 M* M ro m 1 Ba ct ro et 0 ft ro a O ct JJ ct rroo acd ro cd un a. 0 1 o u> o jJ 3* ro 3* ru m VJN M _n o o 1 o 3 o o o && o ctW ^ J 33 9 999 M M--B NO 0 9 O' Jl ft X Q *t M ft C O 9 et O 33roS aB 3 ct M 3* 3 O et 99 C m BO 3 3 3 o a oq 39 3 a a a ct 2,0 a 3* 9 ft H* ft 3* O M 93 0 h* 3 3a CD 3a O3 CD O O CD 3 S3 aa 0 g. 33 o 9a 30 3 a h* 3? a M ft 0O S3 o O >-3 3 C MM 333 a cd B ao a 3 3* ma m cr a o a33 'O H ct 3 H* CD 3 T> 9 3 B a H, pf 3 03 3W a0 0 0 CL 3a. 9s' I-- Cd o 03 9 >-- ?0r 30 -3 fot z3 o < UN 93O 0O' S 3H OnO no ON .fi- ONO -DTd 3 O 3 M 3 CO o o 3 ?s- M a* et H* -0 <3 33H O o9 I 00 ft M UN 33 a DSW 25713S STLCOPCB4061258 VI - 6 Process In Detail VI. PROCESS IN DETAIL, contd. Chlorination, contd. ' Before a fresh charge Is put Into a chlorinator, which has been emptied after a preceedlng batch, the chlorinator Is allowed to cool to 150C., or lower, this, of course, to diminish sublimation into the gas exit. The charge is admitted from the diphenyl head tank, or from the high boiler melter, or both, as required, (see the table on page 5 Section VI, above), and the temperature in the chlorinator is adjusted to 120C. (Recent instructions say 100cC.) Circulation of Aroclor is started on whichever of the scrubbers CT-0759 etc. corresponds to the chlorinator concerned, and the feed of water to the HCl absorber is adjusted to correspond to the expected flow of HCl, also cooling water as needed is put on to the absorber, then chlorine is admitted into the chlorinator. Usually the circu lation of light Aroclor over the scrubber is not interrupted between batches unless a long delay is expected, but the valve in the line between the scrubber and the HCl absorber is kept closed until the diphenyl has been charged. Circulation of the charge in the chlorinator itself is not started until the chlorination has been running for about 4 hours, this delay being practised in the hope of diminishing sublimation of the diphenyl into the off-gas line. Chlorine is passed in as fast as possible, having regard to the chlorine availability, the capacity of the HCl absorber, and the cooling capacity of the chlorinator. 2" - 3" H2S0^ column differential on the 1.1" orifice is a good starting rate, to be increased as circumstances permit. See also the table on the next page. DSW 257140 STLCOPCB4061259 VI. PROCESS IN DETAIL, contd. Chlorination, contd. VI - 6a Process in Detail lb.Cla /hr. Gauge pressure lb ./sq. in. 300 400 500 600 700 800 900 1000 1.7 3.0 4.7 6.8 9.3 12.1 15.3 18.9 1.6 2.8 4.3 6.3 8.5 11.1 14.1 17.4 1.5 2.6 3.9 5.8 7.8 10.2 12.9 16.0 1.3 2.4 3.6 5.3 7.2 9.^ 12.0 14.7 1.2 2.2 3.4 4.9 6.7 8.7 11.0 13.6 1.2 2.0 3.1 4.5 6.1 8.0 10.2 12.6 1.1 1.9 2.9 4.2 5.8 7.5 9.5 11.7 1.0 1.8 2.7 3.9 5.3 7.0 8.8 10.8 1.1" orifice 60 Be V4 Gauge 0.9 1.7 2.5 3.7 5.0 6.5 8.2 10.1 The gauge readings are not recorded. The mercury manometer readings, which appear in the column "Chlor. Back Press. PSIG" on the daily record sheets, refer to the off-gas pressure, as discussed below, and, therefore, reflect the working of the HC1 absorbers, rather than that of the chlorlnators. Recent Krummrich plant instructions call for a chlorine feed rate of about 400 lbs./hour for the first 4 hours, then 600-700 lbs./hr., with water cooling on the external circulation line. If Aroclor should get back into the feed line, as a result of some variation of pressure conditions, it should be quickly purged, by means of a short shot of chlorine, otherwise there may be local overheating and DSW 257141 STLCOPCB4061260 VI o PROCESS IN DETAIL, contd. VI - 7 Process in Detail Chlorination, contd. severe corrosion around the gas Inlet valve. There Is a pressure test branch on the off-gas line, with a connection to a mercury manometer located near the chlorine control valve, so that the operator can control the feed to give not more than 6" Hg pressure In the off-gas line, 1. e. he can keep within the limited capacity of HC1 absorption equipment. The temperatures must not exceed those set out In the table on page VI-5, above. After four hours, the circulation Is started, and samples are drawn from the circulation stream, at intervals of 2 hours, for tests of specific gravity, hold point, or softening point, as set out in the table. (Test methods are detailed in Section VIII, below). If the chlorination is carried beyond about the 1162 level, the product becomes first sticky, then gummy, and finally solid (at room temperature). The density of the scrubber liquor increases much more rapidly during this chlorination to higher values, because the efficiency of absorption in the chlorinator is less,' and the chlorine passes through into the scrubber, where it is absorbed by the lighter Aroclor used for scrubbing. Chlorination beyond 1162 was confined,as far as possible, to No, 1 chlorinator to prevent contamination of liquid Aroclors with solid Aroclors. As the required test limit is approached, the control tests are made at shorter intervals, and when the correct end-point is reached, the chlorine feed is stopped, the chlorinator vent line is opened, the line to the HC1 absorber closed, and the stream from the circulation pump diverted to the aeration vessel CT-0750 (for Aroclors up to and including 1162). Aroclor 1168 went directly .to the vacuum still, the bottom outlet line from the chlorinators being heated with gas flames, and formerly, when Aroclors containing more than 68 of chlorine were made, chlorination would be carried to a hold point of 185 to 195C. in the main chlorinator, then the batch dropped to the "chlorinator pot" CT-0808, for further chlorination, as indicated in the table on page VI-5, above. DSW 257142 STLCOPCB4061261 VI - 8 Process in Detail VI. PROCESS IN DETAIL, contd. Chlorination, contd. Especial care is needed to prevent freezing during transfer of the higher Aroclors. Care must be taken that the chlorinator vent is open and free when the chlorinator is being emptied, otherwise the batch may be con taminated with liquid sucked back from the'scrubbing system. The mercury manometer on the off-gas line will give an indication of any drop*in pressure in the chlorinator. Typical record sheets are given at the end of this section. Chlorination beyond 68#, i.e. for Aroclors 1169, 1170 and 1171 These products are no longer made, but- the following description of the former method of production may be of interest. Chlorination was carried on in two stages, the first(in one of the ordinary chlorinators as for Aroclor 1168, and the second stage in the gas heated, agitated chlorinator CT-0808. As the chlorinfttion in the main chlorinator passed beyond the 1168 stage, external gas flames on the chlorinator body ^md on the circulating lines were needed to keep the charge always 25C., or so, above the "hold" point, and the chlorination was continued in the No. 1 chlorinator to a hold point of I85-I950. Towards the end of this stage, the gravity lines from No. 1 chlorinator to CT-0808 were checked to make sure they were clear, and -O808 che&ked to make sure there was room in it, then at the proper moment* the charge was dropped to -0808, and the external flames kept on for about 5 minutes to drain the mainchlorinator and the gravity lines. No. 1 chlorinator would not be recharged until it was certain that the gas heated chlorinator would be empty again in time to receive the next charge, partly because the same scrubbing system served No. 1 chlorinator and the gas heated chlorinator. DSW 257143 STLCOPCB4061262 VI. PROCESS IN DETAIL, contd. VI - 9 Process in Detail Chlorination beyond 68$, contd. Chlorine was passed into CT-08o8,by way of a dip pipe,quickly enough to raise the hold point by about 15-20C. per hour, the charge always being agitated and kept 25-50C. above the hold point, until the final test was attained as set out on the table on page VI-5 for the different Aroclors. The heat of reaction would usually main tain the temperature even with the furnace doors open, and the gas burners off. When the end point was reached, the burners would be put on to keep the charge molten, until it could be run off into finished product packages, or into the distillation pots of the solid Aroclor stills R-026 and 027, ftesaribed1 in Section XII, below. <4L The off-gases from the gas fired chlorinator went through inter ceptor CT-01258 to trap subliming material, and then through the Aroclor scrubbers belonging to No. 1 chlorinator and so to the HC1 absorber. The Interceptor was cleaned after each second run, the cleanings being put into CT-0808. ' Solid Aroclors .* The gas fired chlorinator, CT-0808, and its ancillary`vessels, have been taken out, also the still R-026 etc., the flaker D-012, and the mill, ML-045. The lean-to part of the building, which formerly housed most of these units, Is now mainly used as storage space for full and empty drums. Scrubbing of the Off-gas from the Chlorlnators In the early part of the chlorination, the off-gas,which leaves the chlorinator, carries the saturation amount of diphenyl, or light Aroclors, at about 150C.-, as the chlorination proceeds, there is less of these materials in the vapour, but there will be heavier Aroclors, and as the chlorination approaches a high value, free chlorine will begin to come over. ' At the Anniston plant, the ofi'-gas handling is simpler than at the Krummrich plant, but it appears to be quite satisfactory. Usually there are two steel cyclones in series for each ftair of chlorlnators, (see sketch). The cyclones can be drained at intervals into opentopped drums,'and the material recycled. page VI-9a. sw 257144 STLCOPCB4061263 CYCLONES or. the CHLOR1NATOR OFF VI - 9a Process In Detail GAS ~ system (Arodors) Ar:;.;stn ; March, 1955 STLCOPCB4061264 VI. PROCESS IN DETAIL, contd. VI - 10 Process In Detail Scrubbing of the Off-gas from the Chlorlnators, contd. At the Krummrich plant the off-gases are scrubbed with a light Aroclor, at a moderate temperature, to trap the volatilizing materials and any unused chlorine, and to purify the HC1 gas. The scrubbing Is done by passing the off-gas up one of the Raschlg columns CT-0759* -O76O, -0761, 01014, or TW-0206, counter current to a `Stream of light Aroclor circulated from one of the pump tanks CT-0754, -0755, -0756, 0968, -01015. See the sketch on page 10a Section VI. About a 5/4" stream of liquid Is used. If diphenyl Is picked up by the circulating liquid, then the density of the liquid falls, but if heavy Aroclor, or chlorine, is absorbed, the density rises, and the liquid may become too viscous for easy pumping. The density, therefore, is tested at intervals, and if It falls outside the limits 1.200 and 1.400 at 65C. (more recently the limits have been given as 1.525 - 1.450 at 65C.), or If the volume increases too much,a note is made of the volume of liquid in the scrubber circulation tank, a sample is taken for specific gravity test, and the liquor is dropped to chlorinator No. 1, and the scrubbing system recharged with fresh crude Aroclor of medium specific- .gravity. The weight of the discarded liquor is calculated, and the # chlorine content read from the curve of specific gravity vs. chlorine content on page III-15y see also pages VI-48 and 49. The equivalent amount of diphenyl is calculated(assuming theoretical chlorination), and the charge made up to the equivalent of a normal chlorination batch by the addition of fresh diphenyl. Pages VI-10b,c,d give*1 a ready reckoner for the calculation of the gross weight and the diphenyl equivalent of the liquor. In recent years at the Krummrich plant the heavier Aroclors have not been made, and the general tendency has been for the scrubber liquor to fall in density during use. I. The scrubbing liquor is not heated while in use, unless it becomes too viscous. The gas leaving the scrubber passes through one of the cyclones CT-01279* -01280, -01281 etc. and so into a main leading to the HG1 absorbers,which are just outside the south wall of the building. Any liquor collecting in the HC1 main drains to a drum outdoors. DSW 257146 STLCOPCB4061265 I^*rhin- CNi 5 CDO STLCOPCB4061266 VI. PROCESS IN DETAIL, contd. VI - 10b Process in Detail Dept. 246 Scrubber Liquor Diphenyl (8-13-46) The table below lists the approximate range of Sp. Gr. of Aroclors that may be found in scrubber liquor. In addition to the Sp. Gr. the equiva lent Aroclor as well as the pounds of solution per gallon is shown. The top Not represents the total pounds of liquor and the lower figure re presents the equivalent pounds of diphenyl in the scrubber liquor. Sp. Gr. at 65C. 1200 1225 1250 1275 1300 1.325 1.350 1.375 1.400 Equivalent Aroclor 1126 1129 1132 1135 1138 1140 1142 1145 1147 Wt.Lb./U.S.Gal. 10.00 10.21 10.42 10.63 10.84 11.05 11.26 11.46 11.67 Scale on Side Sheet Approx. No. of US Gal. Heel 1" 2 3 4 5 6 7 8 9 10 11 12 73 83 93 103 113 123 . 133 143 153 163 173 183 193 730 540 830 6l4 930 688 -1030 762 1130 836 1230 910 1330 984 1430 1058 1530 1132 1630 1206 1730 1280 1830 1354 1930 1428 745 529 847 601 949 673 1051 J4 5 1133 817 1255 889 1357 961 1459 1033 1561 1105 1663 1177 1765 1249 1867 1321 1969 1393 760 517 865 588 970 659 1075 730 1180 801 1285 872 1390 943 1495 1014 1600 1085 1705 1156 1810 1227 1915 1298 2020 1369 776 504 882 573 988 642 1094 711 1200 780 1306 849 1412 918 1518 987 1624 1056 1730 1125 1836 1194 1942 1263 2048 1332 791 490 900 558 1009 626 1118 694 1227 762 1336 830 1445 898 155^ 966 1663 1034 1772 1102 1881 1170 1990 1238 2099 1306 806 484 917 550 1028 616 1139 682 1250 748 1361 814 1472 880 1583 946 1694 1012 1805 1078 1916 1144 2027 1210 2138 1276 822 837 477 460 935 951 542 523 1048 10b5 607 586 1161 HHTS' 672 649 1274 1293 737 712 1387 1407 802 775 1500 1521 867 838 1613 1635 932 901 1726 1749 997 1839 1062 964 1863 1027 1952 1977 1127 1090 2065 2091 1192 2178 1257 1153 2205 1216 852 452 969 513 1086 574 1.203 635 1320 696 1437 757 1554 818 1671 879 1788 940 1905 1001 2022 1062 2139 1123 2256 1184 * on each panel DSW 257148 STLCOPCB4061267 VI. PROCESS IN DETAIL, contd. Dept. 246 Scrubber Liquor Diphenyl, contd. (8-13-46) VI - 10c Process In Detail 13 203 2030 2071 2125 2154 2208 2249 2291 2319 2373 1502 1465 1440 1401 1374 1342 1322 1279 1245 14 213 2130 2175 2230 2260 2317 2360 2404 2433 2490 1576 1557 1511 1470 1442 64o8 1387 1342 1306 15 223 2230 2275 2335 2366 2426 2471 2517 2547 2607 1650 1609 1582 1539 1510 1474 1452 1405 1367 16 233 2330 2377 2440 2472 2535 2582 2630 2661 2724 1724 1681 1653 1608 1578 1540 1517 1468 1428 17 243 2430 2479 2545 2578 2644 2693. 2743 2775 2841 1798 1755 1724 1677 1646 1606 1582 1531 1489 18 255 2550 2581 2650 2684 2753 2804 2856 2889 2958 1872 1825 1795 1746 1714 1672 1647 1594 1550 19 263 2630 2683 2755 2790 2862 2915 2969 3003 3075 1946 1897 1866 1815 1782 1738 1712 1657 1611 20 275 2750 2785 2860 2896 2971 3026 3082 3117 3192 2020 1969 1937 1884 1850 1804 1777 1720 1672 21 283 2830 2887 2965 3002 3080 3137 3195 3231 3309 2094 2041 2008 1953 1918 1870 1842 1783 1733 22 293 2950 2989 3070 "3108 3189 "3248 3308 3345 3426 2168 2113 2079 2022 1986 1936 1907 1846 1794 23 303 5030 5091 3175 3214 3298 3359 3421 3459 3543 2242 2185 2150 2091 2054 2002 1972 1909 1855 24 513 5130 5195 3280 3320 3407 3470 3534 3573 3660 2316 2257 2221 2160 2122 2068 2037 1972 1916 25 523 3230 5295 3385 3426 3516 3581 3647 3687 3777 2390 2329 2292 2229 2190 2134 2102 2035 1977 26 333 3330 5597 3490 3532 3625 3692 3760 3801 3894 2464 2401 2363 2298 2258 2200 2167 2098 2038 27 343 3430 5499 3595 3638 3734 3803 3873 3915 4011 25 58 2475 2434 2367 2326 2266 2232 2161 2099 28 5550 3601 3700 3744 3843 3914 3986 4029 4128 555 2612 2525 2505 2436 2394 2332 2297 2224 2160 29 563 5630 3703 3805 3850 3952 4025 4099 4143 4245 2686 2597 2576 2505 2462 2398 2362 2287 2221 30 575 5750 3805 3910 3956 4061 4136 4212 4257 4362 2760 2669 2647 2574 2530 2464 2427 2350 2282 31 583 3830 5907 4015 4062 4170 4247 4325 4371 4479 2834 2741 2718 2643 2598 2530 2492 2413 2343 SW 257149 STLCOPCB4061268 VI. PROCESS IN DETAIL, contd. Dept.246 Scrubber Liquor Diphenyl (8-15-46), contd, VT - lOd Process in Detail 32 3930 4009 4120 4168 4279 4358 4438 4485 4596 393 2908 2813 2789 2712 2666 2596 2557 2476 2404 33 403 4030 4111 4225 4274 4388 4469 ^551 4599 4713 2982 2885 2860 2781 2734 2662 2622 2539 2465 34 413 4130 4213 4330 4380 4497 4580 4664 4713 4830 3056 2957 2931 2850 2802 2728 2687 2602 2526 4230 4315 4435 '4466 4606 '4691 ~W!T 4827 4947 35 423 3130 3029 3002 2919 2870 2794 2752 2665 2587 36 433 4330 4417 4540 4592 4715 4802 4890 4941 5064 3204 3101 3073 2988 2938 2860 2817 2728 2648 37 443 4430 4519 4645 4698 4824 4913 5003 5055 5181 3278 3173 3144 3057 3006 2926 2882 2791 2709 38 453 4530 4621 4750 '4804 4933 5024 5116 5169 5298 3352 3245 3215 3126 3074 2992 2947 2854 2770 39 463 4630 4723 4855 4910 5042 5135 5229 5283 5415 3426 3317 3286 3195 3142 3058 3012 2917 2831 40 473 4730 4825 4960 5016 5151 5246 5342 5397 5532 3500 3389 3357 3264 3210 3124 3077 2980 2892 41 483 4830 4927 5065 5122 5260 5357 . 5455 5511 5649 3574 3461 3428 3333 3278 .3190 3142 3043 2953 42 4930 502Q 5170 5228 5369 5468 5568 5625 5766 493 3648 3499 3402 3346 3256 3207 3106 3014 43 503 5030 5131 5275 5334 5478 5579 5681 5739 5883 3722 3605 3570 3471 3414 3322 3272 3169 3065 44 513 5130 5233 5380 5440 5587 5690 5794 5853 6000 " 3796 3677 3641 3540 3482 3388 3337 3232 3126 45 523 5230 5335 5485 5546 5696 5801 5907 5967 6117 3870 3749 3712 3609 3550 3454 3402 3295 3187 46 533 5330 5^37 5590 5652 5805 5912 6020 6081 6234 3944 3821 3783 3678 3618 3520 3467 3358 3248 47 5^3 5^30 5539 5695 5758 5914 6023 6133 6195 6351 4018 3893 3854 3747 3686 3586 3532 3421 3309 48 553 5530 5641 5800 5864 6023 6134 6246 6309 6468 4092 3965 3925 3816 3754 3652 3597 3484 3370 49 563 5630 5743 5905 5970 6132 6245 6359 6423 6585 4166 5037 3996 3885 3822 3718 3662 3547 3431 50 573 5730 5845 6010 6076 6241 6356 6472 6537 6702 4240 4109 4067 3954 3890 3784 3727 3610 3492 51 583 5830 5947 6115 6182 6350 6467 6585 6651 6819 4314 4181 4138 4023 3958 3850 3792 3673 3553 52 593 5930 6049 6220 6288 6459 6578 6698 6765 6936 4388 4253 4209 4092 4026. 3916 3857 3736 3614 53 603 6030 6151 6325 6394 6568 6689 TBIT "6879 7053 4462 _ ^325 4280 4l6l 4094 3982 3922 3799 36.75 DSW 257150 STLCOPCB4061269 VI. PROCESS IN DETAIL, contd. VI - 11 Process in Detail HC1 absorption. The Aroclor department at the Krummrlch plant had a set of Silica tourills and a Tantalum unit, used, more or less, in parallel. The feed of city water was hand controlled, through a Rotameter, to give 20.2B acid measured at 65C. The tourills were cooled by being sprinkled externally with well water, and the Tantalum unit had well water through its jacket. Gas is sometimes passed to another department, and at other times, gas is received from other departments, for absorption in the Aroclor department units. The operation of the chlorinat-ors has to be regu lated to some extent to suit the capacity of the various recovery units, and close cooperation is needed between the different departments The tourills on the HC1 off-gas line have been taken out, and a second tantalum-Karbate unit, TW-0312, installed alongside.the old one. The HC1 treatment vessels are of Haveg, and the store tank for finished acid is rubber-lined steel. ' About 50 lbs. of Cliffchar carbon are used for 3000 U. S. gallons of acid, agitated by air for half an hour (off-gas to a drowning tower) then left 24 hours, or more, to settle, and the clear acid decanted, by means of a Karbate pump, to finished product storage. The treat ment tanks are cleaned out to the sewer about once a month, and the system is working surprisingly well. A project has been set up, however, to install a small clean-up filter for the settled acid. The old Haveg sand filter has been taken out; it had cracked, and the acid- soaked Haveg could not be cemented. The various vessels have Pneumer- cator depth gauges, with the indicators in a tall glass-fronted cup board. . Off-gas Treatment at Anniston (March 1955) At Anniston, the gas streams, from all the cyclones on the ehlorinator exits, combine into a header leading to a coke tower 4'0" diameter, ?'6" high. A little organic matter lodges in the tower, but there is no trouble due to the presence of organic matter in the absorption unit which follows. In particular, a rubber-lined store tank for muriatic acid gave good service and was taken out for repairs only after 18 years. The coke tower is outdoors, at the end of a long out door header, and the gas is quite cold by the time it arrives at DSW 257151 STLCOPCB4061270 VI. PROCESS IN DETAIL, contd.. VI-12 Process in Derail Off-gas Treatment at Anniston, contd. the tower. The coke in the tower is in about fist-sized lumps, and it is renewed about once a year. The HC1 absorber now in use at Anniston is a Karbate unit, somewhat modified since first installed. It has a vertical tubular Karbate heat exchanger-contactor, followed by a Karbate tail-gas scrubber, packed with 1" porcelain Raschlg rings. The gas goes down the tubular unit, then up the tail-gas unit. The water enters the top of the tail-gas unit, then flows through a seal bend to the top of the tubular unit, down the unit, concurrently with the gas, and sc to the catch tank. There is a Brown ratio controller, which automatically proportions the flow of feed water to the flow of HC1. It is manually pre-set to give about 20.8B, which leaves a little in hand, above the strength desired. When the absorption unit was first Installed, it had provision for recycling the solution through the heat-exchanger section, so that the tubes would still be properly wetted when the flow of gas, (and conse quently the feed of fresh water), was very low. The unit was designed for 2500 lbs, HC1 per hour, and below about one quarter load, the wetting was inefficient without recycling. However, when the re cycling pump failed, it was not replaced, though the exit of the unit smokes somewhat at low loads. Some of the muriatic acid made is sold without further treatment, but some is treated with carbon, to give the "food grade" quftli ty. For this treatment there is a rubber-lined pre-ooat tank, a rubber lined treatment tank, an Adams filter with 18 tubes, a Karbate Wil- fley pump, and various rubber-lined store tanks. Saran lining has not been so satisfactory. 10 to 15 pounds of Celite are suspended in muriatic acid (or in water) in the pre-coat tank, pumped on to the tubes in the filter, then the carbon-treated acid is pumped in without interrupting the flow, so that the Celite does not drop off the tubes. . Any acid produced in excess of requirements is put, untreated, to the sewer, by way of a limestone pit, which also takes the spent carbon. ' DSW 257152 STLCOPCB4061271 VI-. PROCESS IN DETAIL, contd. VI-15 Process in Detail Changing from One Aroclor to Another. The crude Aroclors fall into four main groups: - 1. Liquid Aroclors from Diphenyl (1142 to 1162) A 2,, Solid Aroclors from Diphenyl (1168, and formerly 1169 to 1171) 3. Aroclor from crude or distilled high boilers (5060) 4. Aroclors from mixtures of diphenyl and highboilers, (2265 and 4065), and in addition the material from the scrubbers on the off-gas has to be worked up through the chlorinators. it may contain some products derived from highboilers. In changing to 5060 from any of the other Aroclors, it is necessary to give the chlorinator two (or more) successive washes with distilled high boilers, using 2,000 lbs. each time, and circulating the(hot) material for 10 - 12 hours each time to give thorough washing of. the catalyst. The first washing can be re-used several times, then used for making 2265 or 4065. The second washing, if its density indi cates less than 0.3# chlorine content, can be used for making 5060. Washing should be continued down to the 0.3# chlorine level. Rinsing Is not thought necessary at other changes. See also the comments on page VI-25. Air-blowing of Chlorinator Charges. At the Krummrich plant, the crude Aroclors are alr-hlawa for 4 hours in CT-0750 or CT-02086, both of which are.vertical cylindrical steel vessels with dish bottom and flanged covers. They have steam coils for maintaining the temperature of the charge, by hand control, and "spargers" for dry air from the "Lectro-dryer." The off-gases are simply vented by wide Haveg stacks to the open air above the roof cf the building. At Anniston there are 3 air-blowing vessels, and the vent stacks are off-set from the air-blowing vessels in two cases,so that nothing can drip back from them into the charges. The blowing vessel at the Krummrich plant Is large enough to contain 3 chlorinator batches at one time, and it may be necessary to put DSW 257153 STLCOPCB4061272 VI. PROCESS IN DETAIL, contd. VI - 14 Process in Detail Air-blowing of Chlorinator charges, contd. unblown charges on top of blown material, in which case the air blowing must be repeated. The steam coils are not used during the air-blowing of Aroclors up to and including 1148, but the higher Aroclors need temperatures of l40C., or more, depending on their softening points, 80 psig steam is used in the coils for 2565 and 4065, but 200 psig was needed for 1168 and 5060. A sufficient flow of air is used to cause the contents of the blowing tank to "roll". A fHolering of the needl^ of the pressure gauge on the air-inlet line will indicate that air is bubbling into the vessel, Arcelor 2565 is not distilled, but is sampled in the air-blowing vessel, checked for acid number and softening point, and if correct, is dropped directly into cans for sale. Distillation* 1 There are two vacuum stills for Aroclors at the Krummrich plant, both being vertical steel cylinders 6'0" I.D., with bulged tops and bottoms, as detailed in section XII below. S-043 is 5'6" deep on the straight side, and S-062 is 11'-10". Each still has the following fittings; - 1. An external heating coil, set in a gas-fired furnace. 2. A submerged pump to circulate the charge through the coil and back to the still. The pump shaft has a water-cooled stuffing box, and there is an indicating ammeter on the driving motor. 3. An inlet with sight-feed coupling, for charges from the air blowing vessels CT-0750 and CT-02086. 4. An inlet from the chlorinators, normally blanked off. 5 A hand hole with a screw cap, for charging hydrated lime. DSW 257154 STLCOPCB4061273 VI. FROCESS IN DETAIL, conta. VI- 15 Process in Detail ' Distillation, contd. 6.. {Formerly) Emergency lines to and from Aroclor store vessel 01-0749. 7. A Manlid low down on the side wall, for maintenance work. 8. A thermo-recorder well through the side wall, about 7' below the rim of S-062 (disused). 9. A bottom outlet which will drain the still. 10. An outlet which will leave in a "heel" of about 80 U.S. gallons., just filling the bottom dish of the still. These outlets are equipped for gas heating. 11o A vapour outlet, to one of the condensers CT-0770 and 01578. The vapour duct has a dial vacuum gauge, a mercury manometer, and a thermo-recorder well. Each duct has a spray separator (differ ent in each case as detailed in Section XII below.) The condensing systems have only monel exposed on the descending sides. At the Krummrich plant, the condenser is cooled by distilled water, which is allowed to boil off into heat exchangers CT-085 and 01491; the condensate from the exchangers returning to the Aroclor condensersby way of one of the buffer tanks CT-O766 and -01596. Wastage of the distilled water is made up by bleeding steam into the system at a convenient time. ' Former!^!.for* the higher boiling. Aroclbrs the distilled water was replaced by Aroclor 1242, circulated through the same system by pump P-0595. Each buffer tank has an internal coil for water and steam. The whole system, whether used in water or in Aroclor is at atmospheric pressure, though it was designed to be worked, if necessary, as a closed system under pressure. The Aroclor circulation system was out of use in 1955, because higher Aroclors were no longer being made at the Krummrich plant. The Aroclor condensers lead to the vacuum receivers CT-0771, -01577, which have the usual fittings. Including a connection to the 5-stage vacuum jets MSC-O76O, -01592, -OI685 by way of the coke scrubbers CT-0755 and -01596. DSW 257155 STLCOPCB4061274 VI. PROCESS IN DETAIL, contd. VI - 15 Process in Detail Distillation, contd. Although still S-0o2 at the Krummrich plant is about twice as deep as S-045, it is given only the same charge (about 10,000 pounds) of crude Aroclcr. The greater depth of S-062 was designed only to give .Tiere disengagement space for the vapour. See the comments on this feature under item S-04j in Section XII below. The charge is sucked to either still, or is pumped by P-O58O from the air-blowing vessel CT-0750, then two cocks on the transfer line are closed, to prevent leakage of crude material into the still during the distillation. The internal pump in the still is started, if it is not already running, and 50 lbs. of lime, (formerly 50 lbs.), hoisted in bags to the operating platform, are added through the charging nozzle on the cover of the still. The amount of lime may be increased, up to 100 lbs., if the crude Aroclor is believed to contain an unusually large amount of HC1. The vent on the still is closed, and the vacuum jet started to reduce the pressure in the still to 7 mm (or less) Hg; absolute pressure, The pilot lights, and a low flame, are usually kept going in the gas furnace between batches, and when the charge is seen to be circulating correctly, the main burners are adjusted to givQ a temperature rise of about 20C. in the material as it passes through the heating coil. The operator has a table of gas pres sures at the burners, corresponding to different operating re quirements, but he must also use judgment in controlling the distillation. The higher Aroclors require considerably more gas. Cooling of the condenser is not started until the distillation has well commenced, because over-cooling of the first distillate might cause blockage with frozen, or very viscous, material. Judgment is required throughout the distillation, to give sufficient cooling without cooling too far, and the rate of distillation is limited so that dark material is not entrained into the distillate. The whole distillate goes into one receiver, no cuts being attempted unless the distillate is seen to be off colour for a time. Typical record charts are given at the end of this section. DSW 257156 STLCOPCB4061275 VI ~ 17 Process in Detail VI; PROCESS IN DETAIL, contd. Distillation, contd. The end of the distillation is signalled by a quicker rise in temperature of the material (at a steady pressure, around 6 mm Hg, absolute), and by a greater temperature "spread" between the coil inlet and outlet, or between the coil inlet and the vapour outlet from the still; about a 40C. spread through the coil is taken as an indication to stop. Any darkening of the distillate stream would also be an Indication. Mr. Pemberton, reporting on his visit to Anniston in 1950, mentioned a colour standard, which the operator may use to check the colours of samples of distillate drawn from the sampler between the con denser and the receiver. Distillation should in any case be stopped before the volume of bottoms has dropped to a point at which the internal pump will be "starved". This is liable to happen with the first batch in a clean still. If the bottoms become too viscous, the pump will "kick out", and the furnace coll will become overheated, and either damaged, or at least blocked with coke. If the ammeter indicates overloading, some light Aroclor should be put into the still to prevent trouble. The internal pump is left running, but the gas flames are cut down to a point just sufficient to keep the "heel" of residue hot enough to circulate freely without coking in the coil; while there is any heel in the still, the internal pump must be kept running (there is an alarm which sounds if the pump shaft stops), and the ga3 burners kept on their low setting. Mismanagement at this stage may cause a freeze-up of the whole system, or may cause coking in the coll. It is important, also, so to arrange the work, that there will be a fresh charge waiting to go in on top of the heel, so that the : pesidue in the still is immediately diluted with more mobile material. After about four batches, more or less, depending on circumstances, the bottoms are drained off through the upper drain opening, leaving a heel of about 80 U.S. gallons in the still. To stop the distillation, a little air is admitted to the still. DSW 257157 STLCOPCB4061276 VI. PROCESS IN DETAIL, contd. VI - 18 Process m Detail Distillation., contd. The outlet cock Is heated. In good time, with a gas flame, a little air sucked in through the cock to make sure the way is clear, then air is let into the system by way of the vent cock on the receiver, and the residue is run out into open-topped cans. The residue is very hot, and gives off an irritating vapour, so the cans are placed on small wheeled trucks, under a canopy with a good exhaust system. Some little of the residue is run into packages for sale as Montar, but the greater amount is allowed to go solid in the open-topped cans, then broken out, and thrown away. If the material is not to be sold, the cooling may be hastened in some cases by using a fine mist of water from a distance of about 15 feet, to cause the upper layer of the material to freeze. Some discretion, however, is needed in doing this, because if the water sinks into the hot material, it will vaporise explosively. For this reason, the water spray is not used for residues from 1242, or 1248, which have a lower density. It is not even used for residues from 1254, 1260 or 1262, unless the batch has been well worked down in the still (temperature spread in the ceil at least 55cC.). If water is not used, the drums are lightly covered during cooling. As already mentioned, the still should be recharged without delay, to thin out the residue left in it. While the new charge is circu lating, but the furnace burners are on the idle setting, the thermo couples at the inlet and outlet of the coil should show the same temperature -- this checks them one against the other, so that the temperature "spreads" observed during the distillation will be dependable even if the readings are not correct in an absolute sense. If the still is completely drained, through the lower discharge cock, so that the pump circulation must stop, the heating coil must be sucked empty. "5Tb facilitate this, two cocks have been installed on the highest part of the circuit with a 1" branch with cock and screw cap between them. With this arrangement, air can be pulled Into the still in either direction along the pump circuit. DSW 257158 STLCOPCB4061277 VI. PROCESS IN DETAIL, contd. VI - 19 Process in Detail Distillation, contd,, The shallower still, S-045, is being worked semi-continuously at the Krummrich plant, but there is very little to add to the des cription of continuous working, as given in my report of March 29, 1955* on the Anniston visit. The material is continuously moved from-the air-blowing vessel to the still by the vacuum in the still. A sight glass has been necessary in the cover of the still receiver. A feature worthy of note is that the. intake of each of the sub merged pumps in the stills has been fitted with a shallow basket, about 10" diameter, 2^" deep., of steel plate, with round per forations set nearly as closely as possible over the whole surface. The purpose of this is to trap stones etc. which might get in with the lime. The pumps are still of the 2" delivery size, and the furnace coils are of 2" pipe. It Is doubted if the Anniston 5" coils offer more surface, because, of course, the turns of the 2" coils can be at closer pitch. The furnace setting with a central steel dummy would appear to be better than that with the central fire-brick dummy, because It will retain less heat. The gas burners are Interlocked, to shut off If the pump shaft stops, but it is suggested that a more rational arrangement would be to have the stoppage worked from an orifice plate, in the circulation line, and so set as to cut off the gas as soon as the flow fell below a certain level. This could be better since it would shut down the gas if, for example, the circulation line should become partly blocked. The stills at the Krummrich plant are worked at the highest available vacuum. A small operating trick is mentioned. As a still batch approaches the end, as Judged by the temperature "spread" between the inlet and outlet of the coil, the burners should not be cut back until the end point is reached . If they are, then the temperature spread falls correspondingly, and there is risk of working the bottoms too far, in an attempt to attain this specified spread, and the bottoms may become too thick to tap easily. The last receiver-full, when the bottoms of a continuous run are being worked down, will be rather heavier Aroclor, and will need blending off into the bulk of distillate. * See also pages VI-20- of the present report. DSW 257159 STLCOPCB4061278 VI - 20 Process, in Detail VI, PROCESS IN DETAIL, contd. Distillation, contd. At Anniston there are two vacuum stills, each of the shallower type, 610" in diameter, 5'-6" deep on .the straight side, like S-043 at the Krummrich plant, and the heating and condensing arrangements are generally similar to those at the Krummrich plant (vertical monel condensers, cooled only by recycled distilled water). The submerged pumps now used in the stills are Taber pumps with Z>" outlets, and the furnace coils are of 3" piping, nine turns at 5" pitch, 24" diameter, to centres. Each coil stands on four short legs on the bottom of the furnace, and there are short steel distance pieces welded between the turns of coil at four points on the circumference (see sketch).* Each furnace is brick lined and has a central hollow cylindrical steel core to confine the flue gases. Stainless steel gives better service as the core. Each furnace has four burners for natural gas, directed horizontally and tangentially, just below the lowest turn of coil, the four burners being equally spaced around the circumference. The furnace is set as close as is possible to the still body, without hindering removal of the still cover; the stream of Aroclor from the sub merged pump in the still goes by a short horizontal pipe to the bottom of the coil, upwards through the coil, then back to the still, by a pipe projecting just through the cover. The lowest turn of the coil is the only part which burns out. The bearings on the shafts of the submerged pumps gave a lot of trouble, and various changes were tried. Finally the master mechanic suggested trying thinner shafts (l"), and these give trouble-free service for a year, or so, before the bearings need attention. The bearings are lubricated by Aroclor fed back from the pump stream, (see sketch). Note Newport's use of a universal coupling on the pump shaft. From the still cover, the vapour rises about 12'0" in 12" pipe, then turns downwards through a tubular condenser, J'O" long, by about 10" O.D., set vertically. From the bottom of the condenser, the distillate goes by a sloping jacketed line to a sight glass. (see sketch).* ' * page VI - 20a. DSW 257160 STLCOPCB4061279 lo st o j i intnoa STLCOPCB4061280 VI. PROCESS IN DETAIL, contd. VI - 21 Process m Detail Distillation, contd. The 12' pipe from the still cover is of steel, but beyond that point only monel is used. The cooling water for the condenser is distilled water coming from a vented head tank high in the building. The water enters the bottom of the condenser shell by a 1^" valve bye-passed by a line having a valve for fine control. The water, (and/or steam), leaving the top of the shell, returns to the head tank by way of a heat exchanger which can cool or heat the return stream, as required. Any make-up water required for the circulating stream, is supplied by bleeding steam into the stream just before the heat exchanger. . The water circulation system had been planned to work under pressure, with a pop valve on the head tank to relieve excess pressure, but it has been found more convenient to run it under atmosphericpressure. Even so, some skill is required to get proper condensation of the Aroclor without cooling so far as to freeze the heavier Aroclors in the condensers. Each of the two vacuum still receivers at the Anniston plant has a sight glass in the cover, through which the operator, by using a flash lamp, can see the level of liquid. The condensate can be run off to drums under a draught hood, or it- may be run to a Blackmer pump,' on the ground floor, about ll'O" below the bottom of the receiver. Thi3 pump moves the distillate to the treatment tank, or elsewhere as required, and it will work, though not very well, with the receiver under full vacuum. The pump and connections are steam traced, and the same pump serves the receivers of both stills. By using this pump without stopping the still, it is possible to work the still in a semi-continuous manner, instead cf purely batchwise, so a level controller has been fitted through the cover of each still, -and the crude Aroclor is fed, by steam Jacketed lines, continuously into the still, keeping the level in the still at about 55" outage. The level controller is of the differential bubbling type. The arrangement is working very well, and distillation can DSW 257162 STLCOPCB4061281 VI - 22 Pro:ess Detail VI. PROCESS IN DETAIL, contd. Distillation, contd. be continued until the equivalent of up to 13 normal batches has been distilled, before the accumulation of bottoms begins to cause darkening of the distillate stream. The feed is then stopped, and the bottoms distilled down until the distillate stream becomes too dark for blending, then the still is tapped to open-ended drums under a draught canopy. The open-ended drums,into which the still bottoms are tapped, are placed on the ground floor, under a steel canopy, about 8 1 0" diameter, coming down to about 3'0" from the ground, and connected to a powerful exhaust fan. There is a canopy under each of the two stills, and smaller canopies at the various drum filling points. Naturally, it is not always possible to continue for the equi valent of 13 batches, because the manufacturing programme may have to be changed before that. The semi-continuous working saves time and labour in tapping and recharging, and it probably permits better recovery of distillate from the bottoms. The dosage of lime, per equivalent still batch, varies with the grade of Aroclor being worked. Aroclors 1242, 1248, 1250 and 1260 take 30 lbs. per "batch", and the same amount is probably right for 1262 (not recently worked at Anniston). 4465 takes 50 lbs. and so does 5442 (rarely worked). 5460 takes 100 lbs., this high amount being found to improve the colour. If "semi-continuous working Is planned, lime is added in ratio "0 the total amount of Aroclor it is intended to work, the whole of the lime being added at the start. Thus for 13 batch equivalents of 1260, the amount would be 390 lbs. corresponding to 13 batches at 30 lbs. each. At one time it was thought best to run the stills at as good a vacuum as could be obtained with the four-stage jet, but at DSW 257163 STLCOPCB4061282 VI - 23 Process In Detail VI, PROCESS IN DETAIL, contd. Distillation, contd. Anniston it has been found better, and more economical in steam, to use only a two-stage jet for some of the Aroclors, for examples Aroclor 1260 1250 1242 1248 (probably) 1268 4465 5442 5460 m.m. Hg in the receivers recommended 50 50 50 50 3-5 3-5 3 -5 3 -5 Compare the figures reported April 1952 by Mr. Harden for Anniston 20 m. m. in the receivers for liquid Aroclors, and 10 m. m, for 5460, The temperature "spread" between the inlet and outlet cf the heating coil, of course, determines the heat input to the still, for any given rate of pumping. Under the present conditions at Anniston,the spread is about 8 to 12C., widening towards the end of a run. For the continuous working,the spread usually nans between 8 and 10C, DSW 257164 STLCOPCB4061283 VI. PROCESS IN DETAIL, contd. VI - 24 Process In Deta.i4 Distillation of Solid Aroclors. See also Lyles, Soffranko and Becker, November 1947, pages 6l-and 97*. In spite of its high melting point, when Aroclor 1268 was made, the distillation was done in the ordinary vacuum stills, as with the lower Aroclors, but with greater precautions against freezing in the pipe lines etc. iiq a \ 1169, 1170 and 1171, as formerly made, were kept hot in the gas fired chlorinator CT-0808, and drawn off in portions into retort pots R-02 and 027. The pots were placed in turn, on a rail cart, on a weighin scale, under the bottom outlet of the chlorinator, the outlet line heated with a gas flame, J>0 lbs. of lime put in the pot, and abou^500 lbs. (600 lbs. in 1947) of the hot Aroclor added, a (vented) lid clamped on with C clamps, then the pot moved to a spot under a crane for hoisting into position on one of the two furnaces. A thermocouple was inserted through the cover of the retort. Each retort pot was equipped with a channel about half-way up the Inside wall, to collect Aroclor, which distilled up on to the upper part of the wall. A pipe connection from this channel, into the pan of the flaker D-012, was made after the pot was in position. The pots were gas heated, a pre-run cut being diverted to a drum, * then the main cut taken to the flaker pan, then a finishing cut, tc the drum again (judged on colour). The tops and tails were recycled partly to the succeeding batch in the still, and partly back to the chlorinator, and the main cut was flaked, the flaking roll being warmed at first with low pressure steam, but' later as the system warmed up, the drum was cooled with water. The flaked material was moved by a conveyor and an elevator L-031 to a finished product hopper. The adjustment of the knife had to be varied as the tempera ture of the roll altered, and the flaker tray was heated by gas flames. was The end of the distillation/indicated by the evolution of a little fume caused by decomposition. The whole system was served by an exhaust fan with cyclone separators. The retorts were removed tc a concrete slab, sprayed with water to cool them, then they were cleaned for re-use. *see sketch, page VT-24a. DSW 257165 STLCOPCB4061284 VI - 24a Process Section A-A STLCOPCB4061285 \ VI. PROCESS IN DETAIL, contd. VI - 25 Process in Detail Distillation of Solid Aroclors, contd. There were spare retorts,so that the residues could be cleaned out without delaying the operation. The finished product in the hopper would be mixed by recycling it round the elevator, then sampled for the control lab. When approved, it would be run off to barrels for sale, or for trans fer to the mill ML-045, by means of an electric hoist. The mill required a steady feed of "dry-ice" to keep the product cold enough to be brittle and not sticky. A white operator, with a coloured operator to clean the pets, could distill 5 pot fulls in an 8-hour shift. Change from one Aroclor to another. See also page VI-13. In changing from 1268 to any of the other Aroclors, it is necessary to drain the still and the receivers, then to put in a 2000 lb. charge of one of the lower Aroclors, and distill it through to clear the system. The distillate is retained for chlorination to 1168, and the still is drained again to drums, inspected, and, if necessary cleaned by hand. Apart from this, at the Krummrich plant, the heel now is usually left in the still, even if a different Aroclor is to be distilled, the first two chlorinations being carried just a little further, if a heavy Aroclor Is to be charged on the bottoms from a light Aroclor, and vice versa, as set out in the following table on page VI-26. In batch working, Anniston prefer to work the still down to a very low level, and drain off the bottoms, whenever a change is to be made to a different Aroclor, and in any case, to drain the still after every 5th run of 1254 or 1260, and after 2nd run of 5460. Before a long stoppage, the still and coil are rinsed through with about 50 gallons of 1154, mainly to clean the coil. Beyond this, no rinsing of the still is ordinarily considered necessary at either plant, and there is no cleaning of the air blowing tank. DSW 257167 STLCOPCB4061286 VI. PROCESS IN DETAIL, eontd. Changing from One Aroclor to Another, eontd. VI - 26 Process in Detail AROCLOR TO BE MADE: 1142 Heel remaining from 1142 usual 1148 usual 1154 ' usual 1160 -0.001 1162 -0.005 Temperature at which Sp. Gr. is measured ] > 1 65 C. 1148 : 1154 : 1160 : 1162 Specific Gravity to be attained + 0.005 usual - 0.001 0.005 -0.005 + 0.002 + 0.001 + 0.005 + 0.001 usual usual - 0.001 usual -0.005 - 0.005 +0.005 +0.005 +0.001 usual usual 65 C. 65 c. 90C. 100C. A + sign means that the chlorination should be carried a little further than usual, and - a - sign means that the chlorination should be stopped a little short, for example + 0.005 above means that the 1162 should be finished at 1.574 to 1.576 instead of at 1.570 as given on page VI-5* below, and - 0.005 means that the 1148 should be finished at 1.406 to 1.408, instead of at 1.410 to 1.414. DSW 257168 STLCOPCB4061287 VI. PROCESS IN DETAIL, contd. VI - 27 Process in Detail Treatment of the Distilled Aroclors. Prom the still receivers at the Krummrich plant,the Aroclors up to and Including 1262 are moved by pumps P-O565 and-01037> to the blending tanks CT-0779 and 01399 Tor treatment with Attapulgus earth, mainly to remove traces of HC1. If the distillate contains moisture. It Is warmed and air-blowr to remove the moisture, before the earth is added. The Attapulgus earth is dried before use, in a vertical steam heated vessel with a cone bottom. (Sketch sent to MCL In 1947). This dryer does not carry the moisture content down to a very low level, and supplies of dried earth are sometimes drawn from Anniston, where the drying is done In an electrically heated tray dryer. The normal dosage of earth is 10 pounds for the distillate from 2 distillation batches, each of 10,000 pounds of crude Aroclor, but the amount of earth may be increased if found necessary to lower the chloride test on the distilled Aroclor. The earth is added, by hand, from a bucket or scoop. The Aroclor and the earth are agitated together for. 4 hours, the temperature being raised to 150C. at which temperature the filtering characteristics of the Aroclor are good. The steam tracing on the lines and the steam Jacket on the filter are put in action, and the batch is recycled through filter P-0238 (formerly the smaller filter F-0172) until clear, (about hour), then the stream of the filtrate is turned to one of the filtrate receivers CT-O78O and-01400, a half gallon sample of filtrate being taken in a hot dry sample Jar for the control laboratory. Filtration of a batch takes about 5 hours. A sample of the filter paper, was sent to MCL by Mr. Harden, August 1950. In May 16, 1955 it was noted that a 30" Sparkler filter, F-0238, (steam Jacketed) had been installed for use on Aroclors, and the 18" one, P-0172 moved for use on Pyranols. A small "Fulflow" filter was being installed for use on the toluene-Aroclor blends. These blends are made up in the Aroclor finished product vessels CT-O78O or CT-01400, rather than in the Pyranol mixers, see page VI-29. The Krummrich plant were depending on supplies of thoroughly dried Attapulgus Earth from the Anniston electrically heated oven. DSW 257169 STLCOPCB4061288 *> VI. PROCESS IN DETAIL, contd. VT 28 Fro =5= in Detail' Treatment of the Distilled Aroclors, contd. It does not appear necessary to empty the earth from the filters after each batch. If satisfactory on all ordinary tests, not including special G. E. approval, the filtered Aroclor may be moved to finished product containers, or to store tanks CT-O768, 0769, 01310. If G. E. approval is required, a fresh sample is taken from the bulked material in the store tank. At Anniston a Sparkler filter 20 diameter, has been installed, for the earth treatment of the Aroclors, but it has turned out to be less convenient to clean than the old plate and frame press, so the old press is mostly used. It has bronze plates and frames, 23 frames, 12" square, with open delivery to a trough which leads back to the treatment tank or forward to the filtrate tank, as required. The press'*set, under a draught hood, in a' drip tray which drains back to the treatment tank. The feed lines are steam jacketed. Lines for the finished Aroclor are mostly of galvanized steel. The filter papers are dried, (not above 85C.), before use, in an oven, and there is one compartment in the oven for storing the dipper and funnel used for sampling Aroclors, also the sample bottles. . The sample bottles are used, Just as delivered by the maker, simply rinsed out 3 times with the material being sampled, then blown out with dry air or nitrogen, then filled with the product to be sampled. Aroclor stored in sunlight in a colourless glass bottle will drop in resistivity, and will begin to smell of HC1. Amber glass bottles are better. See page VII-14. At Newport a "Steller" candle filter was provided for the earth ^ treatment of the Aroclors, and it appears to have been satis factory. There is, however, a record of leakage from the jacket, where an air pipe passes through into the interior. This suggests that steam tracing, as formerly used at the Krummrich plant, may have advantages over a jacket. The bronze dome of the Steller press was replaced by a galvanized steel one, to meet insurance requirements. DSW 257170 STLCOPCB4061289 VI - 29 Process in' Detail VI. PROCESS IN DETAIL, contd. Treatment of the Distilled Aroclors, contd. Aroclors 4465 and 5^65 are sampled from the still receivers. When the end of the distillation of these products appears to have been reached, the gas flames are cut down, and the contents of the still receiver are ''roused" by admitting air through the bottom inlet of the receiver, then the vacuum is released and a large sample of distillate drawn off into a drum. The softening point is checked, and if it is too low, the distillation is recommenced to drive over more of the heavier back ends. When the contents of the receiver show the correct softening point, the product is dropped directly into packages for sale, a sample for the control laboratory being taken during the filling off. Blending of Aroclor "1260 mix" or "1262 mix". The^ are blends of 90$ by weight of the Aroclor with 10$ by weight of toluene. The blending is done either in finished product drums or in one of the blenders CT-O78O or -01400, so for. the time that these blending operations are in hand, the use of flames etc. in the building has to be considerably restricted. Earth wires are attached to the toluene drums, and the nearer of the two still furnaces is shut down. When the blending is completed, the air of the building is tested for inflammable vapour before normal working is resumed. (See page 6, Section XI, for a note on the Davis Vapotester). The blend is sampled for a determination of specific gravity, and the com position adjusted, if necessary, as indicated by the following charts, pages VI-50 and VI-31. See also pages IX-89, 90 and 90a. The mixing tank needs to be steamed out before it can be used again for ordinary Aroclors. See also MCC report 171-4015, "Aroclor 5460 - Toluene mixture '. DSW 257171 STLCOPCB4061290 -11144 VI - 30 STLCOPCB4061291 IU l<< lhi* A-6567 VI - 31 Process In * x. STLCOPCB4061292 VI. FROCESS IN DETAIL, confcd. VI - ..'L F T 'j o e .5 3 i r Detail Blending for Pyranols. The compositions of the different Pyranols (Pyroclors, Inerteens, Askareis) are given on page 4, Section I, above. Pyrancl 1467 is the main products l48l is blended only in relatively small batches (2100 U. S. gallons). The main components are Aroclor 1254 or 1260, and trichloro benzene, or a tri-tetra chlorobenzene mixture. The Aroclors used are made by MCC, and so is most of the trichlorobenzene, but the tri-tetra mixture is bought from the Hooker Chemical Company. The "chloride scavengers", tin-tetraphenyl and glycidyi phenyl either, are purchased, but the tin-tetraphenyl may have to be puri fied by MCC, as described on page 4, Section IX, below. Before a blend is made, great care is taken that all the components are of the correct quality, especially in respect of the inorganic chlorides and corrosion tests discussed in Sections. VII and IX, below. Bulk quantities of the Aroclor and the chlorobenzene concerned are collected, sampled and put through all the routine tests set out in section- IX, below. Excess moisture may be removed, down to about 10 to 15 p.p.m., by passing dry air through these materials at about 70 to 80C. (or even through the materials after blending). The Aroclor may be treated again with Attapulgus Earth to lower the chloride test figure. ' Air-blowing after blending may disturb the composition of the blend unless the temperature is kept down, because the chlorobenzenes are more volatile than the Aroclors. When satisfactory tests have been obtained, the raw material may be sampled for submission to the customer (General Electric Company), as an additional precaution, before blending is done. When approval is complete, the Aroclor and the chlorobenzene com ponents are blended, and a sample of the blend is checked for density and refractive index, and small adjustments made if necessary in the DSW 257174 STLCOPCB4061293 Pro: ss in De a 1 VI. PROCESS IN DETAIL, corn'd. Blending for Pyranol^., contd. proportion of Aroclor to tri- or tri-cetra-chlorbenzene. Chloride scavenger is not added at this stage, but when all tests are known to be satisfactory; a portion of the blend is made up into a pilot batch., using, chloride scavenger from the batch which is to be used for the main blend, full tests are made on the pilot batch, and if everthing is correct, the main batch is treated with the scavenger, agitated 4 hours, circulated through the filter press for- 1/4 hour, and sampled for the final test, an extra sample being taken, if necessary, for submission to the customers. For blending with tintetr-aphenyl, it is usual to agitate the batch at about 50C. to make sure the FTP goes into solution. When the bulk is known to be satis factory, it is filtered info the drums, or rail tanks,for sale, a final sample being taken. In some cases the consignment is held pending the customer's acceptance of the sample. In all this work, care must be taken to exclude moist air, HC1 fumes and dirt. The filter paper used is catalog 75 and 852, size 12, for the General Electric press type FP-50. It is said to remove traces of moisture and inorganic chlorides, even without the help of Attapuigus Earth. All possible care should be taken to have the batch correct before any scavenger is added, and to check the scavenger itself, because any further treatment with Attapulgus earth, which might be necessary, after addition of the scavenger, will remove more or less of the scavenger. The presence of scavenger also complicates the"corrosion" test as discussed in Section VII, pages 12-, and Section IX, page l8l. Traces of Attapulgus earth which have carried through to the finished product amy interfere with the test for inorganic chlorides., see page IX-181. DSW 257175 STLCOPCB4061294 VI - 34 Process in Detail VI. PROCESS IN DETAIL, contd. Packing The finished Aroclcrs are run off into drums, a piece of diaper cloth being tied on the pipe outlet for the lighter Aroclors, and a piece of fine gauze for the heavier Aroclors, which have to be handled hot. This, of course, is to arrest stray bits of pipe scale etc,, but the precaution is now omitted at the Krummrich plant when materials are being filled directly from the delivery of the filter, Newport arrangements for filling and weighing drums are discussed in London Engineering Pinal Report, September 1931 * page 1D8 and 1 F3-10, also in the start-up reports, July 24, and September 27, 1951, The drums must be clean and dry, especial care being needed with electrical grades. Newport complaint NF/61, November 1951, of turbidity in 1248 was traced to the presence of water in the drums. Apparently, in presence of water, the Aroclor reacted on the galvanizing of the drum. Newport plant report, December 1951> mentions the installation of equipment for drying, the drums. Care is taken not to do ary packing if there is HC1 fume in the air. The gaskets for the bungs of the drums have to be correctly chosen. A sample of the gaskets supplied by the Melrath Supply & Gasket Co. to the Krummrich plant was sent to MCL, April 1947, See also the discussion of gaskets on page 2, Section XII, below. Mr. Pemberton, December 1950, collected samples of the labels used at the Krummrich plant; c-ne a patent list label, and the other a warning label on toxicity. The effect of exposure of Aroclors to metal contact is discussed in Section VII, comments, page 17 below. Generally speaking, the distilled Aroclors are packed in galvanized drums, the undlstilled ones in black steel drums. Flaked or milled solids were packed in barrels or Leverpac containers, bulk solid or resinous Aroclors go out in friction type lid drums, (galvanized for the distilled grades). Storage and blending of the distilled Aroclors is done in steel vessels sprayed with tin or zinc, or aluminum lined. DSW 257176 STLCOPCB4061295 VI. PROCESS IN DETAIL, contd. VI - 55 Process in Detail' Packings contd. Since the Aroclcrs are such effective solvents they damage, and are damaged by, ordinary paints, lacquers, insulating varnishes, etc. This feature is important in connection with hydraulic fluids containing Aroclors. See, for example, MCL Research Progress reports 1151, DF 54/26/7 and DF 54/277/6 and 1152 DF 4/ifc/7 and 8 July 1954, etc., also the Section III, Physical & Chemical data, above. Drums for electrical grades of Aroclors are not painted. Newport Plant Technical Committee meeting, April 14, 1955, page 2, reported some promising tests with lacquered drums for electrical grades. It was decided not to use lacquered drums for resinous Aroclors on a returnable basis, because the lacquer suffered at the high temperatures likely to be used in melting the material from the drums. Aroclors also are dispatched in rail cars. At the Krummrich plant the manhole of the car is protected by a tarpaulin tent during filling. Newport plant report for July 1954 mentions the installation of tank-filling facilities. The Krummrich plant operating instructions, August 10, 1954 mention that rail cars for Pyranols and Aroclors are insulated and have either a steam coil or a steam jacket. They are lined with Aluminium or else sprayed with tin and zinc. Only dry air is used for unloading. MCC have a "Christmas Tree" fitting, a one piece fitting carrying air valve, dip pipe, release valve and pressure gauge, for use on rail tanks. Iz is Important to drain the coil or jacket of the rail tank in cold weather. Galvanized or lacquered drums are used for Pyranols. DSW 257177 STLCOPCB4061296 VI. PROCESS IN DETAIL, eontd . VI - 36 Process in Detail Operating Records, The following pages, VT-37 to VI-46, show typical Krummrlch plant Operating Records. . Chlorination Records are given on pages VI-37 to VI-39. Examples of Dept. 246 Still Records can be seen on pages VI-40 to VI-44. Also shown in this section is a sheet giving Dept. D-218 Muriatic Acid, Acid Receiving, Treatment and Filtration Batch Data, on page VT-45, and page VI-46 is an example of a Pyranol Batch Record Sheet. See also Operating Records, pages 25b-, of the "Notes on the Plant 1B' Process", Mather, April 1947. A list of transfers! chlor-lnatcrs to air-blowing etc. etc.) also is made each day. DSW 257178 STLCOPCB4061297 CHLORINATION RECORD - Dept - 246 Arc lor Nq, 1154 223 D 1 phenyI 5600 C h -j r DH.B. Ch I or t n otor No . Operotor Sforted Boland Finished Tennyson Total Hrs Hr 25.50 |ns. to Ins. in Scrubber T i nr^e i o m : pn 8:30 7:00 V V Tank VI - 37 Process in Detail Botch No. 5-51-55 4-1-55 T,m. Cl,Css Pri ss. PSIG 10:00 26 TC 120 Cl2 Rate "Hq 3 Ch lor Back Press. PSIG 6 Chlor Peed Rate i 1 iir. 350 11:00 27 112 36 350 12 :00 1 :00 2 :00 27 27 27 112 115 115 36 36 36 300 300 300 5:00 4 :00 5 :00 6:00 7 :00 27 24 27 27 25 114 114 114 114 116 36 39 39 39 38 300 300 350 2^0 400 8:00 25 116 38 400 9 :00 Busy scrut ibers 10:00 24 120 38 400 11:00 12 :00 1:00 2:00 24 27 25 25 121 125 154 136 58 3i 8 3f 9 H9 400 450 475 475 5:00 26 135 34 9 4 :00 Bus y 5:00 27 144 3* 10 6:00 26 150 H 11 475 500 500 3p. Cr, Hold Pt. Soft Pt. C -- Acid Be 60 F ?M Unit Ac id Be 60 F H2 Unit -- -- 1.176 - 65 1210-- 65 1256 - 65 1295 - 65 1-338 - 65 1.374 - 65 1.410 - 65 L485 - 65 r emork s * De c pa: e VI- 6a. DS W257179 l1 STLCOPCB4061298 I.'. <>'>. CHLORINATION RECORD - Dept - 246 A r c 1 or . Chlormotor No. Operoior 1148 165 Chorge 5 Started Robinson Finished Edmonds - Wyatt ci2 Biphenyl 3600$ ! i H. n n. Total Hrs Gas Hrs 12,25 Ins. to Ins. in Scrubber VI - 38 Process in Detail T1 me 0 m pm 9:15 / 10:30 / ^ 0 te 5-10-55 5-11-55 Tank G G C 0- T,TM CUGos Press. P5IG 11:00 20 12 :00 16 TC 155 130 Cl2 Peed Rate "Mg 5 Ch lor Back Press. PSIG Chlor Peed Rate i 1 Hr. 9 450 8 450 1:00 2:00 3:00 4:00 5:00 B 18 20 20 22 us 126 130 138 155 y 4 4 4 4 8 8 8 8 475 475 475 475 6:00 22 155 4 8 475 7:00 B usy 8:00 20 154 4 8 475 9:00 24 140 4 8 475 10:00 24 159 4 8 475 10:30 F ini s h ( : d al ; 10:30 Sp. Cf. Hold Pt. Soft Pt. C Acid Be * 60 F SH Unit Ac id Be 60 F &2 Unit 1.176 - 90 1.240-90 1.288 - 90 1.333 - 90 1.380 - 90 1.416 - 65 r emork s Swltc hed t ;o 11^ 8. Finished at 10:30. Hole lng i `or room. us>w.'0/IOU | 1 STLCOPCB4061299 -! *rclor ' 'O. CHLORINATION RECORD - De(bt 246 CMot motor No, Operotor 1160 414 Charge Biphenyl 3600 "/ r:.. Started Robinson 5. ' Finished BolcLnd Cl2 . . Total Hrs Gas Hrs Int. to Ins. in Scrubber om pm .I r 4:50 1 /j 11:00 j/ VI - 5-J Proces .j 1 l . Detai1 E.,Ch ua. U>o* 4-26-55 4-27-55 Tank ^ pf" - t (j . C1 Go s Pre s s. P5IG TC 6:00 26 7 :00 26 124 125 8:00 27 9 : 00 27 126 120 10:00 27 11:00 25 127 157 t1 06 12:00 2:00 5:00 25 22 22 19 156 158 145 140 [ 00 4:00 B u s y 21 l4l 6:00 7:00 8:00 9:00 10:00 11:00 16 18 22 22 22 21 155 155 155 157 140 150 a2 Feed Rote "Mg 4 4 Ch lor B acU Pre ss. PSIG Chlor Feed Rate # 1 ii,. 4 4 4 1.246 - 90 4 4 1.509 - 90 4 4 1.567 - 90 4 4 4 4 4 1.505 - 90 4 4 1.558 - 90 4 Finished Sp. G,. c Hold Pt. Soft Pt. Acid 0. * 60 0F Unit Ac id B. & 60 <*> h Unit . , h e rn a r k s '1 1 DSW 257181 STLCOPCB4061300 KRUMMRICH PLANT BATCH DISTILLATION VI - 40 Process in Detail I w=K582r.v DEPT 246 STILL RECORD Ardor No. 1242 Botch No. 16 Still No. TIME DATE Started By Robinson 1:00-**?*, 4 - 17 - 55 Fini shed By Carnisl INS FROM BLOW TK STILL OUTAGE IN . 4:0 4 - 17 - 55 CHARGE TOTAL HRS STILL BOTTOMS LBS NO BTCHS aftr DRG RES LIME LBS (8) o n 46" @ oc 15.00 Tim nm Hg'a=""m Rec Still psig steam Ejector Flow Burners i 23 4 4:00 6 5 :00 / 6 :00 / 7:00 / 8:00 y 9:00 y y10:00 y11:00 y12:00 1:00 y 2 :00 y 8 175 25 5 5 5 5 y y y yyyy y y y /yyy y y y yyyy / y y yyyy y y y /yyy / y y yyyy y y / yyyy y y / yyyy y y y yyyy y y y y y y / oo oo y y y y yyyy pini s hed Temperatures C Cond* Rec Vapor Inlet Outlet Water 50 160 166 171 on y68 163 172 177 y58 165 175 180 y58 166 178 183 y58 168 180 185 y58 169 182 187 y58 171 183 188 y56 170 183 188 y55 170 184 189 y55 175 186 194 55 175 187 197 y____ . y52 180 192 207 51 184 201 237 off REMARKS i DSW 257182 STLCOPCB4061301 KRUMMRICH PLANT -- Semi-continuous Distillation VI - 41 Process in Detail I- wGKsg2rv DEPT 246 STILL RECORD Ardor Ho. 1242 Batch No. 18 Still No-___1 TIME DATE Started By Edmonds - Wyatt 3:00 omjK 4-20-55 Finished By INS FROM BLOW TK 30" @ o n mmHzv jcuum Tim# R.c Still 3:00 6 8 STILL OUTAGE IN . 8:35 zsf Pm 4-24-55 CHARGE TOTAL HRS STILL BOTTOMS LBS NO BTCHS after DRG RES LIME LBS g c 89.50 200 steam E j #ctor Flow Sheet No. I (of 4 sheets) Bumvrs T#mp#rotur#s 0 C 21 3 4 R#c Vapor In1 t Condo Outlet Wot#r REMARKS 175 30 10 6 6 5 52 167 180 187 on 6:00 7:00 8:00 9:00 10:00 11:00 12:00 1:00 2:00 3:00 4:00 5:00 6:00 7:00 8:00 9:00 10:00 11:00 12:00 1:00 2:00 3:00 4:00 5:00 6:00 7:00 / Y/ / // / // / // / // // // /'/ // // // // // / / / / / / / / / // / // / // / // / // / // / // / // / // / // ._*L_ / / y / / 61 58 y / y / / 54 53 y / y / / 52 y y / / y y / 50 / y / 50 y / / y / 50 y / / y / 50 y / / y / 50 y ( / / / 50 y / . , / / / y / 49 / y / 48 y / , / / / / y y / / 48 49 / / / y / 49 / / / y / 49 / / / y / 49 / / / / 49 / / / / / 49 / / / / / 50 / / / / 50 / / / / / 50 / / / / / 50 / / / / / 50 J-- jL JL Z- 50 165 178 185 / 165 178 185 165 178 185 / / 165 178 185 165 178 185 / I 1242 167 180 186 167 180 186 167 180 186 168 181 I87 / / y y Pumped rec.Away 168 181 I87 y 168 181 187 / 169 182 188 y 170 183 189 y 170 183 I89 y 170 182 189 y 171 183 I89 y 171 184 190 y 170 184 189 170 184 189 y y 170 184 189 y 171 184 I89 y 171 184 189 y 171 183 191 Y 171 185 191 y 171 185 191 y 171 191 -Y------- OSIV^?783 STLCOPCB4061302 VI - 42 Process in Detail I- W3K6S2r DEPT 246 STILL RECORD Ardor No.Batch No.Still No. Started By TIME am pm DATE Fini shed By INS FROM BLOW TK @ c Tim* 8:00 9:00 10:00 11:00 12:00 1:00 2:00 3:00 4:00 5:00 6:00 7:00 8:00 9:00 10:00 11:00 12:00 1:00 2:00 3:00 4:00 5:00 6:00 7:00 8:00 9:00 10:00 11:00 Vacuum Ree Still 68 // // // // // // // // // // // // // // // // // // // // // // // // // // // STILL OUTAGE IN . am pm CHARGE TOTAL HRS STILL BOTTOMS LBS NO BTCHS offer DRG RES LIME LBS e c SHEET NO. II (of 4 sheets) Bum rs Ejector Flow i 2 3 4 Rec Temperatures C Vapor Inlet Outlet WCaotenrdo REMARKS 175 30 10 6 6 5 50 171 185 190 on / / / / / y y y 49 y y y y 49 170 184 189 170 184 189 / / / / / / y y y y 49 y y y y 48 170 184 189 170 184 189 / / / / / / y y y y 47 y y y y 47 170 185 190 170 184 190 / / I 1242 / / / / y y y y 47 y y y y 47 170 184 190 170 184 190 / / Pumped rec.Away / / / / y y y y 47 y y / y 47 170 184 190 170 184 189 / / / / / / y y y y 47 y / y / 48 170 184 190 170 184 190 / / / / y y y y 48 171 I85 191 / / / y y y y 48 171 185 191 / v/ Z / / y y y y 48 y y y / 45 171 185 190 171 185 191 / / y y yv/ / / 45 171 187 192 / / / y y y y 46 171 186 191 / / / / / y y y y ^5 y y y y 48 172 187 192 172 187 193 / / / / / / y y y y 49 y y y y 50 172 187 193 172 187 193 / / y y/ / / / 49 172 187 193 / / / y y y y 49 172 187 193 / y y y/ / / y y y/ / 49 / 49 172 189 195 172 189 195 / / y y/ / z_ Z- 49 172 189 195 ____ DSW 257184 STLCOPCB4061303 VI - 4? Process In Detail I- wsk 662 rev DEPT 246 STILL RECORD Ardor No. 124-2 Batch No. Still No-____ ^ Started By TIME dm pm DATE Fini shed By INS FROM BLOW TK STILL OUTAGE IN . am pm CHARGE TOTAL HRS STILL BOTTOMS LBS NO BTCHS after DRG RES LIME LBS @ oc @ C SHEET NO. Ill (of 4 sheets) Tima Vacuum Bumors Rec Still Ejoctor Flow i 2 3 4 Roc Tomporoturos C Vapor Inlot Outlet WCootnodr REMARKS 12:00 1:00 2:00 6 / / 8 175 y y yy 3:00 / 4:00 y yy yy y5:00 6:00 / yy yy 7:00 / 8:00 / yy yy 9:00 / 10:00 / yy yy y y11:00 / ' 12:00 / y/ 1:00 / 2:00 / yy yy 3:00 / 4:00 / yy yy 5:00 y 6:00 / yy yy 7:00 y 8:00 y y y y y 9:00 / 10:00 / y y yy y11 :Q0 y12:00 yy yy 1:00 y 2:00 y yy yy 3:00 25 5 5 5 5 49 172 189 195 y y y y y 49 175 189 L95 y y y y y 49 189 189 195 y y y y y 49 172 189 195 y y y y y 50 172 189 195 y y y y y 50 172 189 195 y y y y y 51 172 189 195 y y y y y 51 172 190 196 y y y y y 51 172 190 196 y y y y y 50 172 190 196 y y y y y 49 172 190 p.96 y y y y y 49 172 190 196 y y y / y 49 172 190 196 y y y y y 49 172 190 196 y y y y y 49 172 190 196 y y y y y 48 172 191 197 y y y y y 50 172 191 197 y y y / y 50 172 192 195 y y y y y 50 172 190 195 y y y y y 48 170 190 195 y y / y y 48 170 190 195 y y y y y 48 169 189 195 y y y y y 48 169 190 196 y y y y y 48 I69 190 196 y y y y y 48 170 190 L96 y y y y y 48 171 196 196 y y y y y 48 171 191 196 _z_ y y 48 _iZL m 196 on y y Pumped rec.Away y y y y 1242 y y y y y y y y y y y y y y y y y y y y -j-- DSW 257185 STLCOPCB4061304 VI - 44 Process in Detail KK6ijiv DEPT 246 Started By STILL RECORD Ardor No. TIME am pm 1242 Botch No. 18Still No.____________ 1 DATE Finished By Boland INS FROM BLOW TK STILL OUTAGE IN . 8:35 am pm 4-24-55 CHARGE TOTAL HRS STILL BOTTOMS LBS NO BTCHS offer DRG RES LIME LBS rs> o n Tim* 4:00 5:00 6:00 7:00 8:00 8:55 Vacuum R*c Still 68 v/ // // // Pi Ejector Flow 175 25 y /y y // ni s c SHEET NO. IV (of 4 sheets) Burners Temperatures C i 2 3 4 Rec Vapor Inlet Outlet 5 5 5 5 47 172 192 197 / y // 47 172 192 198 / y y/ 52 175 200 208 / / y y 52 177 206 212 / y // 49 186 230 240 h e 'i 49 190 246 255 Cond. Water REMARKS on / / / / Pumped away at 4:30 a.m. auto, off off 1 a DSW 257186 STLCOPCB4061305 VI - 45 Process in Detail DEPT. P-S18 MURIATIC ACID ACID RECEIVING, TREATMENT AND FILTRATION CARBON BATCH NO--2 ACID BATCH NO. 318 BATCH DATA - Dates May 10. 1955 Time flow started to # 2 Receiver 8sl0 pm. Operators Mac-lin A. Hourly Readings TIME 10:00 Dm 12:00 mn 2:00 am 4:00 am 6:00 am 8:00 am 10:00 am 12:00 pm 2:00 pm 4:00 pm 6:00 pm 8:00 pm 9:00 pm INCHES 26" 35" 45" 55" 69" 69" ?? 79" 86" . 89" by stick 89" by stick 90" 93"gage 96 "gage OPERATOR Maclin Moeser Moeser Moeser Moeser Hall Hall Hall Hall Hall Hall Hall Hall TANKS WASHED BY OPER. TIME carbon added Time Start Stirring 9s00 PM JW Settling Time 9:30(5-ll-55 )PM M Time Start Filtering Qs30PM (5-12-55) Qper. Hall XM End 9s30 PM Oper. Hall xx= Time Finished 9; 30(5-12-55 )PM AM Oper-. Fin.PM Oper. ACID ANALYSIS AND ADJUSTMENT Be at 60*F. J After J Gals. Water added. Be >/ Color____ \/_ Lab. Report & Final analysis - Color J Be J_______ Color / Time Pumping to # / Time finished X Stg. AM PM PM Oper. /______ Oper.}/_ Oper. ______ X DSW 257187 STLCOPCB4061306 VI - 46 Process in Detail PYRANOL BATCH RECORD SHEET Batch No. 27 Iner PPO Lot No. R-1813TIMEDATEOPERATOR Pumoed TcB to Mix Tk.#l To 107"Out 7:45 pm May IO/55 "Mac" Prom Car No. Prom #6 Sts. B.P. 38 A.P.14" Pumped Aroclor 1260 to Mix Tk.#l ' to &Q, "out No. 5 Stg. B.P. 72" A.P. 36 11:30 om May 10/55 "Mac" 1st. Sample to Lab at 1:45 am May 10/55 Moeser Sp. Gr. Ref.2nd HaO CL 1.567 1.6160 .0010 L - 10 Added. "1260 at ' No. 6 Stg. B.P. A. P. Added 2 "TcB at 4:45 am #6 Stg. B.P. 14"A.P. 10" Mix Tk . B.P. A.P. Sample to Lab at 7:00 am Sp. Gr. Ref. 2nd NaO CL No. ' Stg. B.P. A.P. Mix Tk B.P. A.P. . Added "TcB at #6 Stg. B.P. Mix Tk. B.P. Sample to Lab at Sp. Gr. Ref.2nd. HaO A.P. A.P. CL . Added lbs.Tin Tet to Mix Tk.at lbs. from Drum No. added lbs. from Drum No. V.P.D. Mix Tk. Sampled by Lab. at 11:30 am PPO is OK Moeser ' Moeser Moeser Added 1 bucket of Att. earth 10# P.P.-Q. added 9:30 am 5-11-55 Hall 11:30 am 5-11-55 Hall DSW 257188 STLCOPCB4061307 VI. PROCESS IN DETAIL, contd. VI - 46a Process in Detail Process Records, Krummrich Plant Daily Inventory At 7:00 a.m. each working day a "Daily Inventory Report" is made covering the main items of process material, giving for example the gauge, density, batch number where applicable, in the following places: HC1 in store tanks treatment tanks rail cars Diphenyl in store tanks head tank rail cars High boilers in melt tank Aroclor in store tanks chlorinators airblowing tanks stills blending tanks rail cars Pyranol in blender rail cars Materials in drums,or bags,to the nearest whole package. Readings of the "utilities" meters, and deliveries of HC1 gas to other departments,or receipts of gas from other departments,are reported on the same form, also the past day's repairs and any? special operating difficulties, and a list of samples ready for test at 8:00 a.m. DSW 257189 STLCOPCB4061308 VI. PROCESS IN DETAIL, contd. VI - 47 Process in Detail Monthly Inventory The usual measurements of tank contents, temperatures, densities etc. are made. Prom the densities of the chlorinator batches at the time the inventory is taken, it is possible to calculate from the curves on pages III-15 and VT-48 and VI - 49, how much chlorine is still required to finish the batches, and the batches are then evaluated as if their contents of diphenyl had been carried through to crude Aroclor, with a deduction for the chlorine still needed. Other materials in process are similarly evaluated, vacuum still batches being taken at the values of the crude charges Issued to them. Examples of the inventory calculations are given on pages 55 - of Section VI, takeh from the pages 137- of the report by Lyles, Soffranko and Becker, November 1946, The Inventory is used to prepare monthly departmental returns, as described in Section X, below. ' . DSW 257190 STLCOPCB4061309 VI - 46 Process STLCOPCB4061310 10 to th * 1 i in c h , t i l l lin n : VT - i*' STLCOPCB4061311 VI. PROCESS IN DETAIL, contd. Dept. 246 Monthly Inventory Goods in Process - Arcelor 8 A.M. VI - 50 Process in Detail Shlor. Batch Diphenyl Sp. No. No. pounds Gr. Charged Temp. Equiv. C. Aroclor Finished Lbs.CI2 Aroclor required to be Finish Equiv.Lbs. of Finished Aroclor 1 Empty 2 641 5600 5 Empty 4 Empty 1.566 90 1145 (45.6 #ci) 1260 . U) 5000 (2) 7800 0.4585 95^ recovery (1) Prom curves attached, pages III-15, and VI-49. (2) Prom table attached, page X-12b. * Note: Mr. Furzey reported Dec.11/51 that the distillation yield was - about 95# at the Krummrich plant and a little higher at Anniston. Tank No. Batch Type Ins. Out U.S. No. Aroclor age Gals. Sp. Gr. Temp. C. Lbs. # Per US Recov lallon ery Blow Tank 640 1160 Old Still Empty 2Jn, 651 .1.525 at 120 12.7 95 New Still 894 1160 114 784 1.555 at 110 12.8 95 Old Blend Tank Empty New Blend Tank 895 1160 75 706 1.545 at 100 12.9 98 Total Lbs. Recovered 7854 . 9555 8925 Total Less 10# contingency Difference In Chlorinator Total goods in process 26,510 22,6,65511 25,679 7? 800 51,479 DSW 257193 STLCOPCB4061312 VI. PROCESS IN DETAIL, contd. Dept, 246 Monthly Inventory 8 A.M. Finished Goods - Aroclor VI - 51 Process in Detail Tank Type Aroclor Old F.P.Tk Empty New F.P.Tk 1260 #3 Stg. 1260 #4 Stg. 1254 Sp. Gr. 1.555 1.555 1.495' Temp. Lbs. Per. C. Gal. 90 12.96 90 12.96 70 12.46 Inches in Tank 30" outage 53 52 U.S. Lbs.Finished Gallons Aroclor 1725 6492 6587 22,356 84,136 82,073 #5 Stg. Cars Empty MONX 809 Empty (Solid Aroclors) Tank Batch Lbs. Fin. Lbs.Cl2 No. Diphenyl Hold Equiv. Aroclor Req'd.To charged Pt. Aroclor To Be Finish Lbs. Lbs. $ Fin. Crude Rec'd. Aroclor #1 Chlor. Stg.Pot Empty Empty i Still Pot - Empty Pre Runs - None Finished Goods - Aroclor North Hopper Empty Inches out - _______ Cu.Ft. x#1 Cu.Ft.# South Hopper Empty Inches out - Cu.Ft. X _______________________#1 Cu.Ft.j# Lots 0 No.Bags 50 No.Lbs.Lbs. in container DSW 257194 STLCOPCB4061313 VI. PROCESS IN DETAIL, eontd. Dept. 246 Monthly Inventory 8 A.M. Raw Materials 71 - 52 Process in Detail Aroclor Trappings Lime Attapulgus Earth Toluol 0 50 bags at 50# each = 1500# 6 bags at 50# each = 500 # 1 drum = 200# DSW 257195 STLCOPCB4061314 VI. PROCESS IN DETAIL, contd. Dept. 246 Monthly Inventory 6 A,,M. Scruboer Liquor VI - 53 Process in Detail Scrub ber No. Inches TvT 0 UQ 0 Innage Sals. Sp. Gr. Temp. r* V0 Equiv.* Aroclor 1_L 1C 172 1.20C 65 1126 U.S. #/Gal. 10.00 Lbs. Cla (l) 447 Lbs. Diphenyl (2) 1273 Lbs. Total 1720 2 10 172 1.230 65 1130 10.25 529 1234 1763 3 20 271 1.200 65 1126 10.00 706 2004 2710 4 20 271 1.250 65 1130 10.25 833 1945 2778 1A 20 271 1.230 65 1130- 10.25 833 1945 2778 Less Reserve 3348 1000 Total Reported 2348 8401 0 8401 11749 Note: (1) Lbs. total x % Cla = lb3. Cia-[2) Lbs. total - lbs. CI2 = lbs. dipnenyl * corresponding to the % chlorine from the curve on page III-I5. See also the ready reckoner on pages 10b., c and d. Section VI. DSW 257196 STLCOPCB4061315 VI. PROCESS IN DETAIL, contd. Dept. 246 Monthly Inventory 8 A,M. CRUDE AROCLOR 1142 Lot R-2 = 1 part drum 258# 1148 1154 1 T-2 = 1 II 11 T-l = 1 U ' 485 '' 492 1160 II T-l = 1 II " 530 1162 II T-l = 1 II " 597 1168 0 II69 0 1170 1171 Lot R-l - 1 part drum 170# M T-l = 1 11 " 220 4065 0 5060 0 2565 0 300 0 . 301 0 VI - 54 Frocess in Detai1 DSW 257197 STLCOPCB4061316 VI. PROCESS IN DETAIL, contd. Dept, 246 Monthly Inventory 8 A.M. 5-1-46 vi - 51 Proceii in Detail Aroclor On Hand 5-1-46 Produced Net Reed. Total To Account For 1119 1132 1142 1148 1154 1160 1162 1168 1169 1170 1171 4065 5060 2565 .. 0 0 260 285 194 530 598 0 0 170 220 0 0 0 0 .0 0 200 300 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 260 485 494 530 598 0 0 170 220 0 0 0 To -On Hand On Hand! 363 To Total 6-1-46 6-1-46 ! Net A-246 Transfer by Diff. by _ .nver.tor 00 0 0 0i 0 0 . 0 0 0; 20 rC>. 258 256 1 00 0 485 485 ; 20 2 492 \ 00 0 530 530 | 10 1 597 597 1 00 00 0 0 0 0 c-s 1! 00 0 170 170 ! 00 0 220 220 00 000 00 000 0 0. 0 0 0 1242 400 1248 415 1254 230,818 1260 307,296 1262 440 1252M 205 1268 0 1269 0 1270 116 1270S 0 1271 143 4465 0 5460 29,775 300 0 301 0 0 32,485 187,107 97,147 0 2,000 0 0 0 0 3,000 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 400 32,900 417,925 404,443 440 2,205 0 0 116 0 3,143 0 29,775 0 0 00 11,800 0 325,352 0 217,963 48,509 148 0 2,000 0 00 00 116 0 00 3,001 0 0 (1) 0 0 3,600 00 00 0 11,800 325,352 266,472 148 . 2,000 0 ,0 116 0 3,001 .0 3,600 0 0 400 -00 21,100 21.100 92,573 92,573 137,971 137,971 292 292 205 205 00 0 O' r0^\ !1 142 j 0 ^: U. ."1 26,175C11 0; 0 TOTAL 571,865 322,239 0 (l) To Dept. D-246 894,104 560,385 l\ 1 1 52,109 612,494 26l,uU| 281,5:c In process Finished 250'. 131`fr DSW 257198 STLCOPCB4061317 VI. PROCESS IN DETAIL, contd. VI - 57 Process in Detail Emergency Measures Power Failure Chlorinators 1. Shut off the chlorine feed. 2. Shut off the cooling water. 3. Shut, off the feed water and cooling water on HC1 absorbers. Stills 4. Shut, cf 3till furnaces. 5i Suck out-still coii3. 6. For a long stoppage close off, or vent, the still. Step the steam on the ejectors, then the water. 7. Drain the still if only a heel is left in it. Aroclor Filter 8. Blow the press concents to the blending tank. HCI Handling 9. Close valves below all acid tanks. 10. Replace all plugs and manlids. . General 11. Throw all motor switches to the "off" position. 12. Turn off all gas burners. 13. Leave rail cars in safe condition. Air Failure 1. Affect tank unloading, air=*blowing cf batches, air jets in the stacks of air blowing tank and acid mixing tank.2 2. Distillation will have to stop when the supplied aerated crude is exhausted. DSW 257199 STLCOPCB4061318 "\ LTV r/J VI. PROCESS IN DETAIL, cor.td. Emergency Measures, contd. Proce Detail Plant Water Failure 1. Chlorination would have to stop because of lack of coding for the HC1 absorber. 2. Ejector interstage coding cculd fail. 3. Water supply to the heat exchangers on the stills could fail. 4. Chlorinator pot gland* water cooling would fail* also the cooling of the flaker (solid Arodor plant no longer in use). 5. Water supply to various pump glands would fail. City Water Failure The following units depend on city waters 1. Chlorinator jackets. 2. HC1 absorbers (feed water). 3. Safety showers, toilets* drinking fountains* wash bowls. Natural Gas Failure* 1 Natural gas serves: 1. Chlorinator circulation line etc. 2. Chlorinator pot. 3. Still furnaces. 4. General local heating. DSW 257200 STLCOPCB4061319 VI. PROCESS IN DETAILj contd. Emergency Measures VT - 59 Process in Detail Low Pressure Steam Failure Low Pressure Steam serves s 1. Steam tracing 2. Air-blowing tank coils 5. Chlorinator Jackets 4. Scrubber liquor tank coils and jackets 5. Under-ground store tanks 6. Blending tank coils 7. Flaker drain 8. Condenser make-up water 9. Rail-car heating. High Pressure Steam Failure1 High Pressure Steam serves: 1. Tracing from No. 1 chlorinator to the still. 2. Tracing from high boiler melt-tank to the cfiiorinatc-rs 5. High boiler melt tank coil 4. Still receiver coils 5. Ejectors If gas and power are available,, but other services lacking for a short period, the circulation should be kept up through the still coils with a minimum cf furnace heat. DSW 257201 STLCOPCB4061320 VII - 1 Comments VII. COMMENTS ON THE PROCESS See also Section II, "CHEMISTRY OP THE PROCESS". See also Section XI, "Hazards". Chlorination Stage. The Iron turnings used inside the chlorinator bring about more intimate contact between gas and liquid, as well as providing the catalyst for the reaction, and probably diminishing the corrosion of the vessel itself. Coarse iron turnings are best, and before being used, they are placed in a heap on the floor, and any oil they may contain is burnt off with a gas flame, the heap being turned over with a fork, so that small pieces drop out and can be discarded. A sample of suitable turnings was sent to MCL by Mr. Harden, in August 1950. See Section VII, page 10, for a suggestion that foreign metals in the turnings may cause discolouration of the Aroclors. The turnings are slowly consumed in use, and their level in the chlorinator should be checked about once a month. High chlorine content in the off-gas is an indication that the bed of catalyst may be getting thin, or may have a hole through it, or be in some other way out of order. The presence of moisture, as from a leak in the chlorinator coll or jacket, naturally increases the rate of consumption of the iron. Normally the wastage is about 200 <r 300 pounds in 3 to 4 months for each chlorinator. Chart A 8393* page VI-48, showing the relation between density, chlo rine content, and chlorine usage in the chlorination of diphenyl, and chart A 8394, page Vll-la, connecting the rate of feed of chlo rine with the rate of increase in density, may be of use in judging the progress of chlorinations. Chart A 8394 is used also in cal culating the inventory values of unfinished chlorination batches. Chart A 8395* page VII-lb, is a calibration curve for the flow of chlo rine through the 1.1" orifice as used on the lines to the Krummrich Pit. DSW 257202 STLCOPCB4061321 i 0 In ll STLCOPCB4061322 STLCOPCB4061323 VII - 2 Cqmments VII. COMMENTS ON THE PROCESS, eontd. Chlorination Stage., contd. chlorlnatcrs. Note that the curve refers to gas at 8 psig., but the actual pressure at the orifice varies with the rate of flow cf the gas, and with the depth and density of the charge in the chlorinator, The use of low grade chlorine appears to be harmless, as mentioned on page 2, Section VI. MCC Short form report 2673, 171-790, December 10, 1951, deals with the use cf dilute chlorine, . A few points from the early experience at Newport are worth noting. If the circulation line is blocked at its upper end, samples drawn from the sample point at the bottom of the line may be misleading, and chlorination may be carried too far. The circulation lines were re-arranged for easier olearing,wlth a thermo couple in the delivery end, to guard against this at Newport. Silver relief discs 12" diameter 0.003" thick, calibrated to burst at 25 psig were used on the chlorinators, but failed by plnholing. Later, similar discs failed under pressure when the gas oatlet line became blocked. Silicone grease served well on the chlorine cocks. Chlorinated Santowax proved rather difficult to pump. The lines needed high pressure steam (or even heated Aroclor) jackets, and more power ful pumping had to be arranged. A chlorinator inlet fitting of nickel cast irc-n was installed -- said to be the same as used at Anniston. The cooling coils were lengthened in 1953, giving a 33# increase in chlorination rate. Crystallization trouble was encountered with 5^60 batches, but washing of the chlorinator with Santowax, before use, gave improve ment . A suggestion has been made at Anniston to work two chlorinators together by crossing the pump connection. This might save a little time, since twice the amount could be handled at each charging and discharging. Some thought also has been given to setting up continuous working through a cascade of chlorinators, drawing off the different grades at different points. The production rate is net yet thought to Justify this. DSW 257205 STLCOPCB4061324 VII - 3 Comments VII. COMMENTS ON THE PROCESS, eontd. Chlorination Stage, contd. In a report on a Visit to Anniston, March 31, 1952, Mr. Dalton mentions discussion of the effect of quicker chlorination. It was thought that the higher rate might disturb the isomer ratio particularly with the lower Aroclors, or might give a higher proportion of polychlorc diphenyl, leading to a higher proportion of still bottoms. Higher temperatures might have similar effects, and might Increase the rate of corrosion of the chlorination vessel. Scrubbing of the Chlorination Off-gases. At a starting temperature of 120cC. the diphenyl would have a vapour pressure of about 12 mm, so that one mole of HC1 would carry away something less than l/60th mole of diphenyl during chlorination to mono-chlor. Similarly, mono-chlor diphenyl at about 135C. would have about the same vapour pressure, so that about l/60th of a mole more would be carried away during chlori nation to dichlor, and similarly with chlorination at 150 to tri-chlor. After that, the vapour pressures drop more quickly than corresponds to the batch temperature increases,so that vapourization losses become almost negligible in the later stages, and the total vapourisation loss cannot exceed about 5# of the batch. Cooling the off-gas to something below 100C. would condense almost all of this vapour, so the Anniston cyclones, with the long outdoor gas main, and the coke towers, are probably as efficient in this respect as are the scrubbers etc. at the Krummrich plant. Reaction with unused chlorine is another matter, and the Anniston arrange ment does not include any provision for this. Havercrofr and Mather. 19^7 reported a smell of chlorine at the Anniston HC1 absorber exit, and so did Harden in 1950, but in the latter case the explanation was given that the chlorinators were running rather cold.' When the higher Aroclors are being made, there is a less depth of diphenyl etc. in the chlorinator during the early stages, than when lighter Aroclors are being made, and towards the end of the chlorination of the reaction presumably becomes quite slow, in spite of the higher temperatures used. Nevertheless, Anniston DSW 257206 STLCOPCB4061325 VII - 4 Comment s VII. COMMENTS ON THE PROCESS, ccntdo ' Scrubbing of the Chlorination Off-gases, contd. report fairly good chlorine efficiencies, (see Section X below). With the Anniston off-gas arrangements, any material volatilising from higher Aroclors can fairly easily be kept apart from any coming from lower Aroclors. Air-blowing of Crude Aroclors. It is desirable to use thoroughly dried air because it helps to remove moisture .from the product, and probably this makes the HC.1 easier to remove1?- London Engineering Dept, report,September j51 , (page 107),on the start-up of the Newport plant, reported that a dense cloud of HC1 was formed when air-blowing started, and a simple lime scrubber was installed to prevent trouble with the Alkali Acts. The amount of HC1 was about 2 lbs./batch. Resinous Aroclor required longer aeration -- up to 6 hours. Page 1F3 - 12 stated that the receiver for the air-blown batches needed an agitator. The Newport start up report of July 12, 1951 mentions a stoneware off-gas pipe carried above the roof level. A letter, Mather to Thrift, May 2, 1949, mentions a Haveg stack at the Krummrich plant, and states that there was no fume nuisance there. The moisten air -at Newport could cause the HC1 to be more noticeable. The crude, before air-blowing,on occasional tests, showed 0.5 to 1.0 mg KOH, equivalent per gram of sample, corresponding to about 2\ to 5 lbs. HC1 per chlorination batch. Anniston in 1947 were using compressed air from the plant main, not dried otherwise than by compression and cooling. Distillation. Operating difficulties may arise from poor operation of the ejectors, or from freezing of the condenser, or from plugging of the vacuum lines. The cotton wool, or the upper layers'of coke,in the scrubbers on the vacuum line,may become plugged with Aroclor, and with pipe scale, in which case the top cover of the scrubber is removed, the screen taken out, and the upper layers of coke removed. The coke in DSW 257207 STLCOPCB4061326 VII - C emu-. u VII. COMMENTS ON THE PROCESS, contd. Distillation, contd. the tower is impregnated with 50$ caustic soda solution once or twice a year. The scrubber is filled with the solution, left 2b hours, then drained through the bottom outlet. Later reports state that the caustic soda has been given up at Anniston and at the Krummrich plant. At the Krummrich plant the scrubbers are heated externally by gas flames about each 10 days, and drained to cans. The hydrated lime used in the still presumably contains some free water, and any reaction with HC1 will produce more water. Most of this water will escape during the distillation, and the remainder will be taken up by the Attapulgus earth in the subsequent treatment of the distilled Aroclor. The London Engineering Department Final Reports on the start-up of the Newport plant record the troubles encountered with the circulation pump, which' was located in a secondary, vessel belov: the main still. See also page 79* Section XII. The tube plate o: the condenser leaked at high temperature. Steam leaked into jacketed lines, and gave colour trouble. It appeared advantageous to direct the return stream from the heating coil tangentially into the still. It was easier to keep a steady vacuum at 12 mm than when working at 3 - 4 mm was attempted. There was discussion of the relative advantages of a Hagen sepa:u t inside the still, and a cyclone separator outside it on the vacua:' stream. Mr. Furzey reported, December 5* 1951, that the return lines :: the coils at Newport had been carried down below the level o: tocharges in the still. This arrangement, however, did not give srv better coloured distillate, so it was abandoned. The return section, in particular, should be arranged for easy redding, to clear it. At the Krummrich plant, Merco cocks ar- ., on the circulating line. DSW 257208 STLCOPCB4061327 VII - 6 Comments VII. COMMENTS ON THE PROCESS, contd. Distillation, contd. The stills have to be cleaned out about once a year, and any Incrust ation of lime etc. chipped out. As the pumps become less efficient by wear or corrosion, or the velocity of circulation of liquid through the heating coll becomes slower for other reasons, there is more liability for the coil to become choked with coke etc. The Anniston stills have a cyclone on the vacuum line from the receivers. Early experience at Newport broughtout the danger of leakage of water or steam from Jacketed lines, and showed the need for some means of determining the level of material In the still receivers. The temperature spread In the heating coll naturally depends on the rate of circulation of the liquid, and, therefore, is not In Itself a fully reliable warning of the end of the distillation; the delivery capacity of the pump falls as the charge In the still diminishes. Directing the return stream of liquor up through the bottom of the still appears to be bad practice, also the sucking out of the coil at the end of a run is more difficult. Aroclor 5^60 tended to block the vacuum connections from the still re ceivers. A closed feeder for the lime to the vacuum still was installed at Newport, to save losing the vacuum between batches, except when the still had to be emptied. Treatment of Distilled Aroclors Exclusion of atmospheric moisture is naturally important where high electrical resistivity is required, and, of course, the Attapulgus earth needs to be well dried. The earth treatment diminishes the "inorganic chloride" content of the Aroclor. Schwarting and others, in the Process report of October 15> 1953 > page 6, state that 10 - 20 pounds of Attapulgus earth in a batch ( of 12,000 lbs.) of Pyranol, will reduce the chloride figure from 0.5 ppm to 0.1 ppm. A larger amount of earth may be useful in some cases, but a badly contaminated batch would be returned to the air-blowing stage and then redistilled. DSW 257209 STLCOPCB4061328 v::i - 7 Comments VII. COMMENTS ON THE PROCESS, contd. Treatment of Distilled Aroclors, contd. Mr. Ellenburg, December 1949, said that finished Aroclors should not be maintained above 80C., especially In the presence of Iron. The earth treatment may be omitted If the products are not required for electrical purposes. MCL have investigated the use of alternative materials in place of Attapulgus earth, for example, activated alumina,acid-treated Puller's earth, and KN4 grade of Puller's earth, but have not found anything to equal the Attapulgus' earth either in respect of re moval of chlorides (and moisture), or in respect of speed of filtration. MCL Research Progress Reports 1151 DP 55/86/4 February 1954 DP 55/97/6 March 1954 1152 DP 55/85/7 December 1955 NR 55/103/12 July 1954 etc. deal with this question. The removal of tin-t-etraphenyl by earth treatment of Pyroclors was confirmed. ' The importance of thorough drying of the Attapulgus earth was confirmed at Newport. The steam-heated dryer installed there would bring the moisture content of the earth down only to about 2$, so electrical heating was installed to give a drying temperature of 250C. The drier earth so obtained gave shorter working cycles in the treatment of the Aroclors. Aroclor - Toluene blends. ' The curves on pages VI-30 & IX-89-show the change in densi ty to be expected from the addition of toluene, and show the range of variation which is allowable in the density of the finished blend. Blending of Pyranols. ; The necessary precautions to ensure electrical grade qualify have been set out on pages VI-52 and VI-35 above, and all that need be added here is that this has been one of the most troublesome quality questions ever met at the Krummrich plant. DSW 257210 STLCOPCB4061329 VII - 8 Comments VII. COMMENTS ON THE PROCESS, contd. Note on ''Chloride Scavengers" Mr. Stickley, September 1, 1953, quoting Dr. Jenkins, wrote: "The use of glycidyl phenyl ether as a chloride scavenger in transformer Askarels is covered by a Monsanto patent, and one of our customers, namely, Westinghouse, has been making use of this scavenger. They did this in order to avoid payment of royalty to G. E. on G. E.'s scavenger, which is tin-tetra phenyl. I understand that G. E. has either abolished royalty payments, or so lowered them, that Westinghouse is now going back to tin-tetraphenyl The only reason for using glycidyl phenyl ether, is that it is more soluble in the Askarel. It is our understanding, that in practical use it isn't quite so efficient." (There is history of actual trouble with pump blockages due to the separation of tin-tetra phenyl in the customer's plant during ccld weather, and deposits of tin-tetra phenyl have several times been seen in rail tanks returned to the Krummrich plant for refilling). Mr. Stickley adds that the glycidyl phenyl ether is supplied by Shell Petroleum Corporation, and there is difficulty in getting ''.he ether sufficiently low in chlorides. The ether is made via chlcrhydrin. A possible alternative discussed at MCL R & D meeting, October 19^9, was dibutyl diphenyl tin, but that material may be covered by the General Electric patents. See also the discussion of the action of scavengers under "Excess Inorganic Chlorides", page 12-, Section VII, below. Note on the use of tri-tetra chlorobenzene. Mr. Stickley, February 28, 1953, quoting Dr. Jenkins, wrote-. "----- the use of tri-tetra chlorobenzene was a G. E. develop ment. MCC make the blend, for G. E. licencees and use a T:itetra blend supplied by Hooker. Most of G. E.'s licencees are expected to go over to the new formulation containing 45$ Aroclor 1260 and 55$ tri-tetra chlorobenzene mixture." DSW 257211 STLCOPCB4061330 viz - 9 Comments VII. COMMENTS ON THE PROCESS, contd. Stabilizers MCC Gentral Research report 543,"Studies on Light Stability cf the Electrical Resistivity of Aroclor 1254" White and Ruehrwein, deals with this question, incidentally discussing the solubility of oxygen in Aroclors. MCL Research Progress report 1151,DF 53/86/1, September 1953, deals with the solubility, in Aroclor, of certain anthraquinone derivatives which had been proposed for use as stabilizers. About the end of 1951 MCL were asked if they had a method of estimating beta-chlor anthraquinone in Pyrands, and enquiry revealed that stabilizers are sometimes added by the 'users, to Aroclor 1252 used in capacitors (see letters Ellenburg to Mather, December 28, 1951, and Mather to Quartly, January 8, 1952). Rosella J. Ulm,of Dayton,in a letter to R. J. Good, March 12, 1951, discussed the Isolation of substituted anthraquinones by chromato graphic methods, and their identification by ultraviolet spectroscopy. Quality of the Raw Materials. , See Section IX for comments on Raw Material Quality. Quality of the Finished Products. The finished products have at times been unsatisfactory for different reasons, as set out below: --- 1. Excess Moisture air Possible causes are (a) imperfect drying of the blewi* g' (activated alumina net correctly regenerated)! (b) imperfect drying of the Atfapuigus earth; (c) entry of moisture from rain, or moist air, especially during sampling. Batches may be blown with dry air (not above 80cC-t for the lower Aroclors) to remove excess moisture. DSW 257212 STLCOPCB4061331 VII - 10 Comments VII. COMMENTS ON THE PROCESS, eontd. Quality of the Finished Products, eontd. 2. Excess Colour. Around 1950-51 the distilled Aroclors at the Krummrich plant sometimes showed yellow to green colours. In the running-in period at Newport, also, there was trouble with colour; ' the ' distillate might be brownish or pale green. The green colour was not removed by re-distillation* even in glass. The origin of the colour was never ascertained, though at Newport the occur ence of colour appeared to coincide with leakages of water into the distillation system. Details of construction, of the still *=- direction of entry of the return stream from the heating cell - use of Hagen separatoror cyclone on the vapour exit, also may play a part -= also the frequency of tapping the still bottoms. Air leak through the bottom eock on the still may be harmful. Very high vacuum may actually be disadvantageous because cf the very high linear velocity of the vapours which results. Note also that a tubular condenser, once fouled, may not quickly clear itself in use. Re-starting after a long shut-down may give colour trouble for a time. Mr. Ellenberg, December 21, 1951 * called attention to the fact that Ferric chloride has an appreciable vapour pressure at the temperature of the still and that the (dry) hydrated lime may net be efficient in "fixing" the ferric chloride. It has also been suggested that copper or nickel salts from non-ferrous metals in the turnings used in the chlc-rinators might cause colour. MCL Research Report 4l6A, 52/1/1; January 17, 1952 indicated that lime treatment would remove the green ooj our . Dr. Jenkins, January 8* 1952 mentioned that Aroclors sometimes contained traces of chlorophenols,, Possibly air in the chlorine may favour the formation of phenols. Mr. Ellenberg.. Decemosr 21, 1951; suggested that the chlorine gas may carry ether impurities. See Anniston report 2675 in the list at the end cf this section, . Diphenyl sometimes shows a yellow or pinkish colour, but colourless Arcclcr has been made from such Diphenyl, and it is not thought that the colour of the Aroclor-s is in any way related to that of the Diphenyl. . DSW 257213 STLCOPCB4061332 VII - II Comment s VII. COMMENTS ON THE PROCESS, contd. Quality of the Finished Products, contd. 5. Partial Crystallization, (possibly after admixture with solvents;. At Anniston, the trouble with crystallization In Aroclor 5^60 is attributed to the presence of diphenyl in the Santowax used. This may come about by cross-contamination in the Aroclor plant. as well as by incomplete fractionation in the diphenyl still. Attention to this point has been more effective than dropping the setting point of the Aroclor. The setting points are now in the range 98.5 to 105icC., instead of 100 to 105i-C. as formerly. There are some indi cations that Santowax from "low-conversion" runs of the diphenyl . units, will tend to give crystallization in the 5460. MCL research reports under job 1152, August - October 1953.; etc. cover work done in the blending of 1221 and 1242 to give material which would match 1252, but which would have less tendency to crystallize, also work on the blending of Aroclors with materials thought likely to diminish the tendency of the Aroclors to deposit crystals. A blend of two Aroclors to make a third may match on density etc. but still be different in other respects, as discussed in Section II above. Complaints of deposition of solid in solutions of Anniston Aroclor 5460 in white spirit were ascribed to the presence of hexachloro 1,4 -diphenyl benzene. See also MCC recerTs ?u-9?. "Formation of precipitate in organic solutions of Aroclors", May 1950, and 2272 "Solubility of Aroclors 5460 in various solvents') Wade, December 1948, (detailed in the list at mne end of this section). 1248 has also shown incipient crystal lization. An acetone solubility test was developed, to defect the tendon y to crystallize, but it was not completely satisfactory, thcug" ,t was improved by the use of the technique of seeding the test solution with a little of the insoluble product. See MCL Res^-n-.r Report 4l6 A, 52/1/4, April 11, 1952 etc. DSW 257214 STLCOPCB4061333 VII - 12 Comments VII. COMMENTS ON THE PROCESS, contd. Quality of the Finished Products, contd. 5. Partial Crystallization, contd. Refrigeration to remove the crystallizable materials has been proposed, but not put Into effect. A suggestion was made that the Insoluble matter might be tin-tetra phenyl, but though this might occur In some cases, the usual cause Is the presence of sparingly soluble chlor-diphenyls etc. as discussed above. MCL Research Progress Report 1151, NR 53/97/8, June 1954 reports determinations of solubility of TTP In 1248 and suggests that TCB Increases the solubility. Various aspects of the occurrence of this partial crystalli zation are discussed In MCL research reports under Job 4l6 A. High diphenyl content of the diphenyl highboilers appeared to be the cause of trouble In 4465 and 5460. The crystals occurred In the low and the high boiling fraction of 4465. The crystals depositing in 1252 appeared to be 4-4' dichlorodiphenyl. Processing 4465 to a lower softening point helped a little. 4. Excess Inorganic Chlorides A sample of the Aroclor being tested Is washed with hot water, the water extract clarified by centrifugation in a laboratory machine, washed with ether, then tested with acidified silver nitrate solution. Any turbidity produced. In a Tyndall beam. Is ascribed to "inorganic chlorides" in the product. The turbidity is matched by use of standard NaCl dilutions, and ex pressed as parts chloride per million on the original sample. Another portion of the Aroclor is heated with a strip of alumi num foil for 6 hours at about 210cC. under a condenser, cooled. S1V 257215 STLCOPCB4061334 VII - 13 Comments VII. COMMENTS ON THE PROCESS, eontd. Quality of the Finished Products, eontd. 4. Excess Inorganic Chlorides* eontd. and the chloride estimation repeated* care being taken to side track anything which has collected on the walls of the condenser. Details of the test methods are given in Section IX, below. These tests arise from the use of the Aroslcrs in electrical equipment. The first ohlcrlde test covers possible corrosive effects of the impurities in the Arcelor as received, and the second one is intended to cover stability of the Arcelor, and the development of corrosive materials when the Arc-clor is kept in contact with metals at temperatures liable to arise in everyday electrical use. The material collecting in the condenser in the second test is side-tracked because the General Electric Company distinguish between "volatile" and"ncn-volatile" chlorides. The volatile chlorides are supposed to go off from the transformers, etc. in which Pyranol is used* without ccrrc-ding the equipment, but the non-volatile chloride figure is supposed to represent the amount of corrosion to be expected. It would appear that in the test any reflux stream would tend to carry the "volatile" chlorides back into the test flask, confusing them witr the 'hon-volatile". See also the notes or., the test method itself. Section IX, pages 77-, and l8l-. Dr. Munch and Mr. Ashworth at St. L^uis have developed a test in which the "HCI" liberated during the heating is continuously aspirated over into silver--nitr3.ee solution., a method . whirh. would appear to give a better measure/the stability of the material. ' There is a long history of tr-cuole with tha verv stringent specification laid down by users in respects e-r the chlorides tests on Aroclors for the electrical industr-v. DSW 257216 STLCOPCB4061335 VII - 1.4 Comments VII. COMMENTS ON THE PROCESS, contd. Quality of the Finished Products, contd. 4. Excess Inorganic Chlorides, contd. In the first place, quite special precautions have to be observed in taking samples and in making the tests, especially in factory conditions where the air may contain, for example, traces of HC1. Tanks should not be opened for sampling etc. when HC1 fumes are being released nearby. Mr. Clegorn of Anniston has developed a satisfactory method of taking samples from rail cars and factory tanks. New, dry, sample bottles, not cleaned or washed in any way, are used, and plunged well below the surface of the liquid to be sampled, and washed out at least three times with the material, blown out with clean dry air or nitrogen, then filled and closed. This procedure can make the difference between acceptance, or rejection of a batch. Aroclor stored in sunlight in a colourless glass bottle will drop in resistivity, and will begin to smell of HC1. Ambercoloured glass bottles are better. Laboratory arrangements necessary for the chloride test are described in Section IX, below. The direct test, for chlorides in the sample before heating, will estimate free HC1 and metallic chlorides such as might result from corrosion, say of the still condensers. If chlo rides get through to the "clean" side of the filter, they may be very troublesome. Air-blowing of the warm material under warm conditions, will bring the HC1 down to a low limit, and reaction with tin-tetra phenyl or glycidyl phenyl ether will remove. traces of HC1. If the T.T.P. reacts to precipitate the chlorine as SnCl^, which is then removed by filtration with Attapulgus earth, then its effect is understandable, but since the tetraphenyl is used in excess, there would appear to be a chance of the formation of materials such as SnCIPha which would carry through into the finished product, and so spoil the chloride test. Gradual DSW 257217 STLCOPCB4061336 VZ1 - 15 Comments VII. COMMENTS ON THE PROCESS , contd. Quality cf the Finished Products, contd. 4. Excess Inorganic Chlorides, contd. addition of the tln-t-etra phenyl might precipitate ail the reactive chlorine as SmCl^; so preventing the formation of the hypothetical SnClFha etc. In practice, the tetra phenyl is the last ingredient to go into the blender, sc it may be that the first portion of it to enter the Pyranol picks up all the chlorides. Treatment with Attapulgus earth is the standard method of im proving batches which fail to pass the inorganic chlorides test, but sometimes quite heavy Treatment is needed. If blends such as Pyramids 1467 and i470, which are required to contain Tin-tetr-aphenyi, are heavily treated with earth- a good deal of The T.T.P. will be removed by the ear'd, and the amount so lost will have to be made up again. Possible causes of high "direct" chloride test are? 1. Contamination of the system with metal_i' chlorides already mentioned. 2. Insufficient removal of HJ1 by air-blowing. 5. Insufficient amount of lime used In the di5ti._^adon. 4. -Entrance of HC1 from the factory anrospnere. 5. Entrance cf Cads from the air breather or the tank vent. 6. Moisture (in the Arcelor cr Pyrar.ol. or in the Adapulgus Earth) will delay the removal of hll by air blowing, and will promote the formation of chic rides which will remain in tne batch. 7. High chloride content of the chloride "scavenger" usee. DSW 257218 STLCOPCB4061337 VII - 16 Comments VII. COMMENTS ON THE PROCESS, contd. Quality of. the Finished Products, contd. 4, Excess Inorganic Chlorides, contd. General Electric (1950) reported that they could improve the electric properties of Pyranol 1467 by a comparatively light treatment with heat-treated Attapulgus earth without a signi ficant change in the T.T.P. content of the material. The Krummrich plant have been -unable to duplicate this result in the plant or in the laboratory. Possibly some chlorides ere more easily removed than others. . A batch of 45,000 lbs. of Pyranol 1467 made at the Krumroricn plant early in 1951 was found to test 0.15ppm chlorides, and was, therefore, returned from the rail car to the plant for re-treatment. By this time it showed 0.8 ppm. It- wa3 treated with small amounts of Attapulgus earth, and filtered through the Sweetland press, but with little effect. The amount of earth was increased, two treatments finally being given, each with 600 lbs. of earth. The total amount of earth used was 1400 lbs. The first 600 It . treatment diminisned the chlorides to 0.2 ppm, and the second to 0.10 ppm. By this time... most of' the T.T.P. had also disappeared. Instability of the Arcclcrs, as indicated by the inorganic chlorides test after the sample has been heated in the corrosion test, presumably arises from the presence of traces of moderately stable organic chlorine compounds, rat,her than from any insta bility of the chlcr-odiphenyls themselves, since good batches show really high stability. Ring substitux-ion of chlorine for hydrogen in the diphenyl nucleus should yield stable compounds; the unstable Impurities may be ring ad:..i+ion compounds, or- they may be side-chain substitution products derived from, traces of toluene etc. in the benzene used for diphenyl. The crude diphenyl also contains traces of styrene, and no doubt other hydrocarbons, which may form unstable chlorine derivatives. Little exact Information on these points appears to be available, and it might be thought that- the unstable materials would be destroyed during the prolonged bearing of the charges in the vacuum stills, except for ary wrioh might- distill .over in the early part of the batch. DSW 257219 STLCOPCB4061338 VII - 17 Comments VII. COMMENTS ON THE PROCESS, eontd. Quality of the Finished Products, eontd. 4. Excess Inorganic Chlorides, eontd. Similar considerations apply tc tri- and tetra- chlorobenzenes. Trouble with Pyrancls In 1947 was traced to the Instability of trichlorbenzene due tc the use of too little catalyst In the manufacture of the TCB, resulting presumably In the formation of small amounts of ring addition products. Trouble also arose from the presence of "chlorides" In the purchased tin-tetra phenyl. Some deliveries contained as much as 500 ppm, and MCC found it expedient to purify the T.T.P. as discussed in Section IX, pages 4-. Trouble with Inerteen in 19.55 was as erf.bed to Instability of the glycidyl phenyl ether used. 5. Unsatisfactory Electrical Properties. Moisture and inorganic chlorides naturally are objectionable, and it has been stated that storage of Arcclors in steel con tainers will harm the electrical properties (Anniston report 2771> in the list on page VII-25 ). The choice of containers is discussed ir. Anniston report 2772. See also MCL research progress reports 1151 51/141/ 24 etc. 1$55 and 4l6A 52/1/8, October 1952 (Arcelor 1254 not dlscoloured in plain steel, 1 week at 60cC.). Packages are discussed on pages 54 and 55 of Section VI. above. Report 1151 RR 55/57/2, May 1955, shows very little deterioration in electrical properties under severe conditions of exposure to steel, and even less with aluminium. ' Mixtures containing TCB or TTC5 have a more powerful solvent effect than straight Aroclors, and this has caused trouble, lor instance, in cases where jointing materials, Glyptal "dopes" on pipe joints, etc. have been attacked ir. the customer's plant, with detriment to the electrical properties of the Pyr-ancl. DSW 257220 STLCOPCB4061339 VII - 18 Comments VII. COMMENTS ON THE PROCESS, contd. Uses for the Products; Application Work. The MCC Bulletins "Physical Properties of Aroclors" and P-115> "The Aroclors, Physical Properties and Suggested Applications", mention the following possible uses: -- Adhesives (adhere to metals) -- low vapour pressures advantageous. Electrical fluids and solids. Expansion media in instruments. Hydraulic fluids; high densities are a favourable feature. Working fluids for die casting (see the special bulletin P-137). Lubricants in high pressure work -- use in air compressors, because non-combustible (See the special bulletin P-128). Lubricants for plug cocks on chlorine lines. (MCL Res. Prog. Rpt. 291 51/92/1, April 1951). Using in cutting oils. Heat transfer media (See also the special bulletin P-130). Plasticisers in PVC, nitrocellulose, chlorinated rubber etc. -- can be used to "extend" more costly plasticisers. (Special bulletins). Water-proofing paper. Vehicle for pigments in decorations of fired glass articles. Use in paints, lacquers (flame resistance), but note possi bility of toxic vapours). Good penetration of stucco and road surfaces (traffic paints). (See Phys. & Chem. Data, Section III, above, for references to lists of compatibilities of materials with Aroclors.} DSW 257221 STLCOPCB4061340 VII - 19 Comments VII. COMMENTS ON THE PROCESS, eontd. Uses for the Products ; Application Work, contd. Extender for the costly Carnauba wax in polishes. Prevent sticking of drawers in furniture. Wood treatment (along with pentachlorophenol). For many of these uses, gaskets and packing materials, which are resistant to Aroclors are needed. On this question see Section XII, page 2, below. See also MCL research reports, 1152 DF 5k/6/7 and 8,July and August 195^ * Aroclor 2565 has been used to make non-flame roof sheeting, (Anniston visit report 19^7, page 5). Properties favouring the use of Aroclors are ; 1. The wide range of properties available. 2. Low vapour pressure. 3. Very low corrosive effect. Compatibility with numerous materials. 5. Chemical inertness and thermal stability. 6. Waterproof. 7. Non-inflammable. 8. The solid Aroclors are odourless and tasteless. 9. Good electrical properties. On the other hand, the Aroclors are not quite above question on toxicity, and they have a very high viscosity index, i. e. a large drop in viscosity with a small rise in temperature. Vis^na-^ DSW 257222 STLCOPCB4061341 VII - 20 Comments VII. COMMENTS ON THE PROCESS, contd. Uses for the Products; Application Work, contd. index improvers have been suggested, but their use may harm the products in other ways. On this point see MCL Research Progress reports, 1151, D 5V26/5, July 195^ etc. The following reports deal with electrical uses of the Aroclor group. MCC Bulletin "Askarels", July 24, 1953* use in transformers etc. MCL Research Progress Reports 1151 RR 53/58/3 June 1953, and 1151 DF 54/26/15, Feb.1955 Material for publications on application in capacitors etc. 547 52/47/1, Sept. 1952, and the corresponding Final Report, Mar.5/53 Literature survey on electrical uses Final report 347D, June 1953, Methods of testing dielectrical properties. Research Progress report 547 51/141/17, November 1952, "Electrical properties of Montars," and 1151 DF 53/86/4, February 1954 "Montars in junction boxes." Work on uses in hydraulic fluids is described in MCL Research Progress Reports. 1151 FR 52/71/3 etc. DF 53/34/4 May 1953 etc. DF 54/26/5 etc. July 1954 Testing in die casting Machines Pump tests, burn poin+s Autogenous ignition V. I. improvers See also reports under job 454 E in 1952. DSW 257223 STLCOPCB4061342 VII - 21 Comments VII. COMMENTS ON THE PROCESS, contd. Uses for the Products; Application Work, contd. Work on uses a3 plasticizers Is described In: -- MCL Research Progress Report 347 31/59/1 etc. "Aroclors In PVC". Work on uses In paints, and polishes etc. Is described In: -- 1132 DP 53/89/5 May 1954, 1242 Improves solvent polishes PR 52/90/6 Jan.1953, No gloss Imparted to silicate paints DP 54/27/1 etc. Apr. 1954 Montars in paints for pipe lines, and battery boxes. (Montars raise the softening point of asphalts). Agricultural uses: Animal repellant. See effect on vegetation; toxicity. The use with Lindane etc. was discussed in correspondence, January 26, 1955. Miscellaneous Ur s11es:* 4 Use as rust inhibitor is described in DP 54/26/11, January 1955. Use in lithographic inks has been suggested in correspondence, (May 3, 1954). Aroclors also have possibilities as chemical intermediates. See MCL Res. Prog. Rpt. 347D - 51/141/ June 1952 etc. for nitrated Aroclors. The MCL Progress Research Department report for November 1952, page 4, mentions the preparation of Aroclor derivatives for trial as insecticides. Report ll6l RR 54/77/1 > November 1954, discusses the hydrolysis of Aroclors to hydroxydiphenyl. Mr. Stark of the Krummrich plant, September 24, 1954, suggested that Montars would make a good sealing compound to cover the cast lead which holds the carbon anodes in Hooker chlorine cells. DSW 257224 STLCOPCB4061343 VII - 22 Comments VII. COMMENTS ON THE PROCESS, contd. Patent Position. Lyles, Soffranko and Becker, November 6, 19^6, page 167* states "In 1955 the Swann Chemical Company was acquired by Monsanto, which gave the latter access to the patent rights for the production of AroclDrs". MCL Research and Development Dept, report for August 19^9> page 26, states that the market for Aroclors in the electrical industry was largely dominated (in Britain) by B.T.H. patents up to about 19^6. These patents had run out, but the B.T.H. still held pro tection for the use of tln-tetraphenyl. MCL would try to come to a license arrangement with B.T.H. The September 19^9 report, page 27> stated that B.T.H. were willing to grant MCL a license,under their patents, to sell Aroclor compo sitions containing tln-tetraphenyl, for use in transformers. B.T.H. needed the British source of supply. The October report, page 50, indicated that discussions were still in progress with B.T.H. Meanwhile the Anniston alternative material, dibutyl diphenyl tin would be considered, although it probably comes under the B.T.H. patents. See also the discussion under "Stabilizers", page VII-9> above. DSW 257225 STLCOPCB4061344 VII - 23 Comments VII. COMMENTS ON THE PROCESS, contd. List of Reports relating to Aroclors and Pyranols_ PROCESS REPORTS 1. Dept. 246; Aroclor Process Lyles Soffranko and Becker November 1946 Date Copies sent to ~ MCL________ April 26, 1947 and October 24, 1950 2. Notes on No. 1 above. E. Mather April 1947 April 25, 1947 3. Notes on Anniston Aroclor Plant Havercroft and Mather September 1947. 4. Dept. A-246; Pyranol Process Lyles Soffranko and Miller March 24, 1947 5. Process Description for Aroclors, Dept. 246 Schwarting, Neff and Graves November 1955 October 7, 1947 October 15, 1947 March 26, 1954 6. Revised version of No. 5 above Schwarting and Schwartz March 15, 1955 7. Process Description for Pyranols and Inerteens Schwarting, Neff & Graves October 1955 8. Aroclors Operating Instructions Dept. 246 Alnsley and Schwartz August 10, 1954 May 17, 1955 May $3# 1955 DSW 257226 STLCOPCB4061345 VII. COMMENTS ON THE PROCESS, contd List of Reports, contd. 9 Anniston Equipment list for Aroclors , Ellenburg 10. Notes on a Visit to the Anniston Plant, Harden August 1950 11. Notes on a Visit to the Anniston Plant, Pemberton January 22/ 1951 12. Notes on a Visit to the Anniston Plant, Mather March 29, 1955 15. Anniston Process Improvement reports 14. Anniston Monthly Operation Reports 15" Anniston Plant Investigation Reports 16. Krummrich plant Monthly Operation Reports 17 Krummrich Plant Investigation Reports VII - 24 Comments Date Copies sent to MCL ,June 7 1946 March 29, 1955 routine routine routine routine routine DSW 257227 STLCOPCB4061346 VII - 25 Comments VII, COMMENTS ON THE PROCESS, contd. List of Reports, contd. MCC RESEARCH PROGRESS REPORTS Job, No. Report No. Date ~tJppies sent to MCL_________ 117-790 2675 Use of dilute chlorine December 10, 1951 January 50, 1952 117-1987 Method of determination of stability of TCB Munch and Ashworth October 16, 1950 H7-I987 part I Infra-red studies, TCB and Pyranol 1467 May 1, 1948 117-2052 Tentative Amendment to Process for TCB, Hubbard and Steahly October 16, 1950 117-4015 Aroclor 5460 toluene solutions 171-718 2771 Effect of exposure of Aroclors to steel April 27, 1955 171-719 2772 Containers for Aroclor 1242 April 27, .1953. 171-1027 A series of reports on minor inquiries from Sales April 14, 1955 171-1028 2790 A series of reports on April 14, 1953 expansion of Aroclor April 27, 1953 manufacture, increase in etc. rate of chlorination etc c DSW 257228 STLCOPCB4061347 VII - 26 Comments VII. COMMENTS ON THE PROCESS, contd. List of Reports, contd. MCC RESEARCH PROGRESS REPORTS, contd. Job No. ' Report No. Date Copies sent to MCL 171-1029 2788 Use of Aroclors with sec. butyl acetate and a series of reports on assistance to tie Aroclor Dept. April 14, 1953 April 27, 1953 etc. 171-1054 A series of reports on July 20, 1953 low-temperature dielectrics 171-1075 2887 Minor investigation for sales; examination of competitive products July 20, 1953 171-1076 Assistance to Aroclor Department July 20, 1953 171-1077 2885 Aroclor 5460 from Davis "Tarophen" July 20, 1953 171-1088 2881 Differences between Anniston and Krummrich Plants July 20, 1953 171-1089 2892 Determination of Aroclor concentration in gases June 7, 1954 171-4015 Aroclor 5460 - toluene solutions 171-4019 Customer contacts. DSW 257229 STLCOPCB4061348 VII - 27 Comments VII. COMMENTS ON THE PROCESS, contd. List of Reports, contd. MCC RESEARCH PROGRESS REPORTS, contd. Job No. Report No. 729-1573 Improve flexibility of operation of Krummrlch plant Semi continuous distillation. Will quicker chlorination give more highboilers? Date Copies sent to MCL 729-1664 Series: Maximum production rate with minor changes in equipment; Krummrich plant. April 27, 1953 etc. DSW 257230 STLCOPCB4061349 VII - 28 Comments VII. COMMENTS ON THE PROCESS, contd. List of Reports, contd. MCC CENTRAL RESEARCH REPORTS Report 543 January 1949. Studies on Light Stability of Electrical Resistivity of Aroclor 1254. White and Ruehrwein (Gives data on the solubility of oxygen In the Aroclor) Date sent to MCL MCC REPORTS 1877 Standard Process Report on Aroclor 4465 Ellenburg 2215 Anniston Aroclor Data book Pinal Report 2272 Solubility of Aroclor 5460 in various solvents. December 1948. 2492 Formation of precipitate in organic solutions of Aroclors. May 1950. 2689 Distillation of Aroclors at higher pressures. 2694 High rate of distillation of Aroclors. 2949 Compatibility of Aroclors with mineral oils. October 1953. June 7, 1946 January 5* 1951 DSW 257231 STLCOPCB4061350 VIIo COMMENTS ON THE PROCESS,contd. List of Reports, contd. PUBLICATIONS Jo Applo Chemo 3 ' October 1953, page 477 "Method of determination of thermal conductivity" Baxter, Vodden and Davies VII - 29 Comments Am, SoCo Mecho Eng. 58 (1936) p. 719 "Thermal conductivity of Aroclors" Ind. Eng. Chem. 39. (1947) p. 517 "Vapour Pressure of Trichlorobenzene" See also MCL Research Progress Report 1151* 53/58/3, 54/26/13, DF 54/27/9 and 10, December 1954, and January 1955 on preparations of material for an Aroclor booklet. See also letter, E. Mather to Dr. Newman, January 8, 1952, reviewing journal information on Aroclor toxicity. Report No. 1, project 526, February 4, 1954, W. M. Nolan, Southern Research Institute, Brimingham, Alabama, "Vapour Pressures of Aroclors below 100C." DSW 257232 STLCOPCB4061351 VII. COMMENTS ON THE PROCESS, contd. List of Reports, contd. MCC BULLETINS "Askarel" Sales bulletin - July 24, 1955 Indirect Heater for Unit Chemical Operations ----------- McArdle (re-issued as bulletin P-150) 'G Physical Properties of Aroclors P-115 Properties of Aroclors (replaced the foregoing report.) P-128 Aroclor Incombustible Lubricant P-150 Indirect Aroclor Heater for Unit Chemical Operations P-157 Die casting VII - 50 Comments Date sent to MCL September 9, 1955 January 17, 1952 Requested July 7, 195^ January 28, 195* DSW 257233 STLCOPCB4061352 VII. COMMENTS ON THE PROCESS, contd. List of Reports, contd. LONDON CENTRAL ENGINEERING REPORTS Preliminaj^y Report . March 19^9 Periodical reports on running-in the Newport Plant. July - November 1951. Pinal Report. , Aroclor Plant Performance. September 1951. Operating Instructions for Aroclors September 1951 Design Book. Newport Project 41. Chemical Engineering Design. January 1950. MCL REPORT Market Research. N. G. H. Thomas November 194-7. Tentative Process and Analytical Methods February 1951. VII - 51 Comments DSW 257234 STLCOPCB4061353 VII - 32 Comment s VII. COMMENTS ON THE PROCESS, contd. List of Reports, contd. MCL RESEARCH REPORTS Job No. 347E 50/175/2 Nov. 50 Electrical tests on TCB.Effect of insulating materials on Aroclors. 51/16/1 Jan.51 etc. Tests on TCB. Cell for dielectric tests. Equipment for high voltage break-down tests. 51/59/1 Feb.51 etc. Aroclors in PVC. Power factor curve. Resistivity. 51/129/1 Aug. 51 High voltage breakdown equipment constructed. 51/141/1 Aug. 51 Resistivities, power factors, dielectric constants Of Aroclors. Electric tests on nitrated Aroclor. Routine electrical tests.on Aroclors. Choice of containers. Competitive Aroclors. Literature survey of uses of Aroclors in the electrical industry. Properties of Montars. Nitrated Aroclors. 52/47/1 52/48/1 . Sept,52 Sept. 52 Capacitator paper. Literature survey on uses for Aroclors. Final Reports Dec. 52 Alternating current characteristics of Aroclors,. Feb. 53 Literature Survey of Uses. Jun. 53 Electrical Testing Methods. DSW 257235 STLCOPCB4061354 VII - 33 Comments VIIc COMMENTS ON THE PROCESS, contd. List of Reports, contd. MCL RESEARCH REPORTS, contd. Job. No. 355E 50/193/1 Nov.50 Examination of TCB samples 51/91/1 'Aug.51 Gasket materials. Aroclor 1248 as cooling medium, compared with mineral oil. 4l6A 52/1/1 Jan ,52 Solubility of 4465 and 5460 in white spirit. Removal of green colour. Crystal formation in 1252. Acetone solubility of resinous Aroclors. Preparation of solid Aroclors. Mild steel effect on Aroclor. Evaluation of TCB. 52/19/1 Mar.52 Evaluation of TCB. 45 4e FR52/41/3 Apr. 52 FR52/41/5 Sep.52 Aroclor as coolant for internal com bustion engines. Effect of high temperatures. Corrosion by Aroclor. FR52/71/1 Aroclors in hydraulic pumps. Corrosion very slight. 1151 52/1/12 May 53 Bakelite Co.'s (air current) method of testing stability of Aroclor, FR52/17/4 Mar.53 Aroclor as hydraulic fluid. FR52/71/3 Aroclor in die casting. FR52/90/6 Use of Aroclors in silicate paints. FR53/34/4 May 53 Aroclors in die casting fluids PR53/58/3 Jun.53 Breakdown strength after earth treatment. Capacitors. Effect of metals on Aroclors. Material for publication. ^ DSW 257236 STLCOPCB4061355 VII - 24 Comments VII. COMMENTS ON THE PROCESS, contd. List of Reports,contd. MCL RESEARCH REPORTS, contd. Job No. 1151 DF52/85/4 Nov. 52 Blowing of fuses In Aroclors. DF52/86 Sep.52 Anthraquinone derivatives as. stabilizers. Joint box compound. Storage in steel. Activated alumina in refining competitive materials. NR52/97/1 Jul.52 Stability up to 200C. Crystal deposition in 1222. (Torque con veyors ). Blending of 1221 and 1242. Topping of 1254. Fuller Earth. Alumina etc. in refining. Solubility of TTP in Aroclor. Determination of Aroclor in Air. Resinous Aroclors. DF54/16/2 Mar.54 Exposure of plastics etc. to Pyroclors. DF54/26/2 dan.54 Studies for hydraulic fluids. Metal exposure. Synthetic rubbers. Gaskets, mixtures of Aroclors with organic phosphates etc. Running tests. Rust inhibitors added. Resistant paints sought. Burn point. Auto genous ignition. V.I. improvers. Material for publication. DF54/27/1 Apr.54 Electrical tests. Montars. Paints for piping etc. Reclamation of arced Aroclors. Various applications studies. Gaskets. Test cell. Aroclor capacitors. Publications. DSW 257237 STLCOPCB4061356 VII - 35 Comments VII. COMMENTS ON THE PROCESS, cortd . List of Reports, contd. MCL RESEARCH REPORTS, contd. Job No. 1152 51/141/20 Jan.55 Technical service. Effect on Insulation of wire. Examination of arced material. Effect of Aroclor on Shellac. 55/60/1 Jua.55\ Effect on Insulation of wire. DF55/85/1 Sep.55 Technical service. Test cell. Effect on insulating materials, processed wood etc. Silicon glass coated wire. Reclamation of used Pyroclor.s DF55/89/5 May 54 Use in polishes. NR55/103/1 Jun.55 Fuller's Earth removes TTP. Other absorbents tried. Determination of TTP in Pyroclors. __ DF54/16/5 Apr. 54 Technical service. Effect of exposure of insulating materials to Aroclors. Gaskets. Test cell. Damage by arcing Customer's test method corrected. Viscosity of 2565. Resistivity of 1254 against time. Silicone glass fibre etc. ll6l NR5 4/77/1 Nov .54 Hydrolysis of Aroclors. DSW 257238 STLCOPCB4061357 VII. COMMENTS ON THE PROCESS, contd. VII - 36 Comments The early research work on Aroclors was done mainly at Anniston, from about 1929 onwards, under the Phosphate division, and the reports are feo be assimilated into the Organic Division collection of reports. Work has been done, for example, on the isolation of the individual chlor-diphenyls, and on infra-red analysis of mix tures of chlor-diphenyls, also on the investigation of numerous uses suggested for Aroclors, and on application work. Most of the basic data on Aroclors, as given in the MCC bulletins, is derived from this work. No attempt is made here at a complete survey of the early work. DSW 257239 STLCOPCB4061358 VIII. CONTROL TESTS. VIII - 1 Control Tests Determination of Sticky and Gummy Stages of Aroclors 1168, 1169, 1170, 1171 1. Shortly after a specific gravity of 1.570 at 100C. is passed, the Aroclors will pass into the sticky stage which lasts for a period of 2-4 hours. 2. Place a small amount of the Aroclor on a smooth metal surface, cool slightly and test between the thumb and forefinger, while wearing a rubber glove. If the material Is stringy it is in the sticky stage. 5. If the material-can be rolled into a ball it is in the gummy stage. The gummy stage follows the sticky stage and lasts 2-4 hours. Determination of Crystallizing or Hold Points of Aroclors 1168, ll69> 1170, 1171 . 1. After passing the gummy stage the Aroclors, when tested on a metal surface, solidify immediately into a sort of gray crystal line mass. Hold points can then be run on the chlorinator batch. 2. To run the hold point obtain a sample in a Pyrex test tube and heat, to about 200C. over a gas flame. Agitate with a 0-560C. thermometer. 5. Insert the test tube into a Dewar tube which is mounted In a large mouth bottle packed with asbestos or rags. 4. . Stopper the test tube with a cork stopper through which is in serted the thermometer. 5. Cool slowly, at the rate of 4 - 5C. every 20 seconds, until the hold point is reached. 6. The temperature will continue to drop until a period is reached where there is no change in temperature for 2-5 minutes. If the temperature increases after this period, then the highest DSW 257240 STLCOPCB4061359 VIII. CONTROL TESTS, contd. VIII-2 Control Tests Determination of Crystallizing or Hold Points of Aroclors 1168, 1169, 1170> 1171* contd. 6. contd. temperature attained will be the hold point. However* If there Is no increase In temperature, then the point where it held steady is the hold point. 7. CAUTION: Wear goggles and asbestos gloves when obtaining sample of the solid Aroclors in the; molten stage. Softening Point (SP) Determination of Aroclors 2565, 4065, 4465, 5060, 5065 ASTM Method The sample shall be melted and stirred thoroughly, to.avoid having air bubbles in the mass an4 then poured into the ring so as to leave an excess on cooling. The ring, while being cooled, should rest on a metal plate. After cooling, the excess material shall be cut off cleanly on top with a slightly heated knife. Pill the 600 c.c. beaker to a depth of 2-1/4" with glycerine at room temperature. Suspend the ring containing the sample and ball in the glycerine so that.the lower surface of the ring is exactly 1" above the bottom of the beaker and the upper surface 2" below the upper surface of the glycerine. Suspend the thermometer so that the bottom of the bulb is level with the bottom of the ring and within 1/4" but not touching the ring. Apply the heat in such a manner that the temperature of the: glycerine is raised 5C. each minute. The temperature as read on the thermometer at the instant that the melted material from the ring touches the bottom of the beaker will be the softening point. Run a standard sanple along with the chlorinator sample for comparison and make corrections as follows: Suppose the S.P. of the standard sample is 112'C. and dSjops at 110C., whieh indicates too rapid heating, then add 2C. to the S.P. ef the chlorinator sample. It is important to 'follow the setting of the ring and the thermometer as well as the rate of heating. DSW 257241 STLCOPCB4061360 VIII. ,, . CONTROL TESTS, contd. VIII-3 Control Tests Hold Point A little more detail of the "hold point" test was given by Mather, November *6, 19^8; A portion of the sample Is melted In a 5^" x 1" Pyrex test tube which is then closed with a cork carrying a thermometer, and the tube then hung in the neck of an unsllvered Pyrex vacuum vessel which in turn hangs in the neck of a wide mouthed glass bottle, forming a support. The thermometer is watched as the temperature falls, then rises as the material crystallizes again and the highest temperature reached in the "hold point". Samples of finished product are taken before filtration through the Sparkler, and most of the passing out tests .ne.-made, on them to save time in packing the O.K. material. The following sample of material in process has been sent to MCL: Distilled untreated Aroclor 125^, June 25, 19^9 DSW 257242 STLCOPCB4061361 IX. SPECIFICATIONS AND TEST METHODS IX - I Specifi cations Speclfloations_for_BIPPffiNYL ^DI PHENYL)_(XENENE^ (Raw Material) Code No. 6ll Date; -4-6-51 Chemical Formula Molecular Weight: 154.200 Supersedes Specifications of 8-6-40 Approved WGN TWD NB SMK DBH ATL PROPERTY Appearance and Color SPECIFICATION Light yellow crystal line solid METHOD NUMBER 10,252-41 Crystallizing Point 68.7C., Min. 10,298-40 Distilling Range* First Drop 100$ (First Drop to Dryness) Dry Point 252.5C., Min. 1.5C., Max. 256.5C., Max. 10,299-40 SAMPLE FOR ANALYSIS - 1 x 16 oz. W. M. Bottle Notes; Above specifications cover Monsanto Biphenyl as made at Anniston. This Raw Material will be analyzed for the Distilling Range on special request only. However, a complete analysis will be made of the material purchased from outside sources. HighJBoiLsrs^ Crude and Distilled. No specifications; used at the Krummrich plant as delivered from Anniston. DSW 257243 STLCOPCB4061362  IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 2 Specifications Specifications for TOLUENE (Raw Material) PROPERTY SPECIFICATIONS METHOD NUMBER Appearance and Colour Clear, practically colour less liquid, 10 APHA max. 11220-52 Sulphur Trace, max. 119-^0 Paraffin % 0.5 max. S-529^5 Barrett acid wash No. 2 max. 11222-52 Colour of unquenched Sulphcmchloride light brownish, but not opaque S-529-2 Distilling range C. 1st drop 97# ' dry point 110..0 min. within 0.6 111.0 max. Aliphatics % 0.10 max. 11,799-52 "Aliphatics" and "paraffins" are defined as being measured by tests 11799 and S-529-3 respectively, rather than in their usual chemical sense. DSW 257244 STLCOPCB4061363 IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for_Hydrated Lime_(Raw Material) PROPERTY SPECIFICATIONS Appearance and Colour Fine white or slightly grey powder, free from lumps or gritty material. Sulphate, as SOa # 0.50 max. Mg (0H)2 # 0.50 max. Ca COa # 9.0 max. Ca (GH)2 92.0 min. IX - 5 Specifi cations METHOD NUMBER 10,188-40 10,189-50 10,192-40 10,195-50 10,191-41 Chlorine _Gas_. No specifications. Snift gas from the chlorine cells appears to be satisfactory. Spe_ci_fi_cations_for_At_tapulgu Earth. (Raw Material) The supplier's specification is: -- Through 800 mesh screen 95# minimum Volatile matter at 950C. 15# maximum Krummrich Plant Method No. 12,504 12,505 Deliveries are not tested except that the screen test is occasion ally made. Moisture content up to, say, 250C., with a much lower allowance than 15# would appear to be more in line with the requirements of the process. Cliff Char^ No MCC specifications. DSW 257245 STLCOPCB4061364 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 4 Specifi cation Sp^ci^flocations_for_Tin-te_traghen^l_ (Raw Material) No formal Monsanto specification has yet been drawn up, but the material is being purchased on the maker's specification, as follows: M. Pt. 226 + 2C. Colour White Purity 97# based on the reactivity of the material with HC1 Condition Free from fibres, dirt and paper Inorganic Chlorides 0.000080# max.* by method 11568-52 Hot water extract Neutral to phenol phthalein Dropped to 50 ppm by agreement with Hooker. Normally only the inorganic chloride test is performed on deliveries to the Kruramrich plant. Material containing 50 ppm .of inorganic chlorides is usable, but earlier deliveries, containing perhaps ten times this amount, were purified at the Krummrich plant as follows: (D. B. Hosmer and C. Barbre, January 1950). 1. Each container of tin-tetraphenyl received from the Hooker Company is transferred to a larger Fiberpak container where it is mixed thoroughly. 2. A sample taken from (1) above is tested for its suitability for use in making Pyranol No. 1467 by adding approximately 0.130# by weight of T.T.P. to Pyranol No. 1488 which has been found to be free of chlorides by a previous test. The resulting pilot batch of Pyranol No. 1476 is tested for chloride content by the regular analytical procedure. If the pilot batch is found to contain less than 0.00001# chlo rides, the T.T.P., is approved for use. If the pilot batch contains more than 0.00001# chlorides, the T.T.P. is set aside for reprocessing.3 3. T.T.P.,which is acceptable for use,is tested again before it is added to a plant batch, by making a second pilot batch from DSW 257246 STLCOPCB4061365 IX - 5 Specifi cations IX, SPECIFICATIONS AND TEST METHODS, contd. Specifications for Tin-tetraphenyl, -contd. 3. contd. the T.T.P. to be used and a sample of Pyranol No. 1488 from the plant batch. . Our procedure for purifying T.T.P. consists of washing a monochlorbenzene solution of contaminated T.T.P. with city water followed by recovery of the T.T.P. by recrystallizatlon. (See report on Job 115-1740 Refining of T.T.P. by L. A. Hertllng. A copy of this report is to be sent to you under separate cover). This treatment diminishes the inorganic chloride content to about 5-10 ppm. A sample of suitable T.T.P. was sent from the Krummrich plant to Ruabon in January 1950. Specifications_for_Glycidyl_pheny1_ ^fether^ Phenox^ propene_ xide C. 0.0Ho. CH. 0CHo Op d d Supplier's specification (Shell) Epoxy content 98# w/w minimum Colour, Hazen Pt. Co. standard 30 max. Sp. Gr. 20/20 C. Total chlorine as Cl' 1.105 - 1.115 40 ppm max. Note; A batch showing 0.68$ total chlorine gave bad results in use. Another sample showed 0.25$, but only 0.75 ppm inorganic chloride. Another again showed 0.85$ total chlorine, but only 1.50 ppm Inorganic chlorides. DSW 257247 STLCOPCB4061366 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 6 Specifi cation Specifications_of_ Trichloro_ benzen^, (Flaw Material) (Pyranol 1478 GEC) Specification H 5228222 PROPERTY SPECIFICATIONS METHOD NUMBER Appearance and Colour Colourless mobile liquid APHA 10 max. 10,105-55 Condition Clear 10,105-55 Acid number 0.014 max. 10,087-55 Sp.Gr. 15.5/15.5C. 1.460 to 1.477 10,106-55 Inorganic chlorides 0.000010$ max. 10,195-40 Viscosity, 100F. SUS 28 - 52 10,086-40 Dielectric Strength,25C, > W O K\ 10,122-40 Refractiv index 25 C. 1.5680 to 1.5715 10,125-40 Distillation range 1st drop 5$ 50$ 9056 205.0 min. 210.0 min. 215.0 min. 215.0 max. . 10,108-42 Crystalliz.. point 10.0C. max. 10,101-55 Hs0 0.0075$ max. 10,620-41 Corrosion test 6 hours at 210C. Change in weight nil Acidity after heating 0.014 max. Inorganic chlor ides after heating 0.000010 max. Condition clear colour 200 APHA max. 10,126-55 DSW 257248 Specially processed material to make it suitable for electric grades. See also the finished product specifications for Pyranol 1478, page 55 Section IX, below. STLCOPCB4061367 v ' IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 7 Specifi- cation Specificat ions_for_Tri -Tetrachlorob_enz ene_ blend (Raw Material) Chemical Formula: Mixture Sample for Analysis: 3 x 5 pt. Amber Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests PROPERTY SPECIFICATION METHOD NUMBER Color APHA 15, max. Condition Clear Sp. Or. at 15.5/15.5#C. 1.510-1.522 Acidity (mg. KOH/g.) 0.014, max. Moisture (H2O) 75 ppm., max. Refractive Index at 25 C. 1.5775-1.5790 Free Chlorides 0.10 ppm., max. Crystallizing Point -15C., or lower Last Crystal Point 0C., max* Dielectric Strength at 25C. 30 KV, min, Distillation Range (ASTM D-85O, Modified) First Drop 210C., min. 5# by Volume 215C., min. 65# by Volume 228C., min. 90<# by Volume 255C., max. 95$ by Volume 265C., max. Dry Point 278C., max. Corrosion Test, 6 hrs.at210C. with bright aluminum foil Change in weight of A1 0.0$ Color APHA 100, max. Condition Clear Acidity (mg. KOH/g.) 0.014, max. Free Chlorides 0.10 ppm., max. Chemical Composition Trichlorobenzene 58.5$* min. 1,2,5,4 Tetrachlorobenzene 26.0-29.0$ 1,2,4,5 Tetrachlorobenzene 3.0$ max. Pentachlorobenzene 5.5$ max. . 10,105-55 10,105-55 10,114-53 10,109-55 10,620-55 10,125-55 10,118-55 12,035-55 12,035-55 11,605-54 10,108-52 10,126-55 12,036-55 General Tests (made only on request) Fire Point' None to Boiling Pt. 10,123-55 General Information Dielectric Constant 1000 cycles, 100C. Viscosity at 100F. ^, ^ 26-32 SUS DSW257249 STLCOPCB4061368 ' IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 8 Specifications Comments on Raw Materials. Diphenyl See the comments under "Excess Colour", page 10, Section VII, above. Anniston report 171-1077 2883 discusses the use of Dow's "Tarophen" as raw material. Chlorine. See the comments on the use of dilute chlorine on page 2, Section VI, above, and on possible impurities In the chlorine on page 10, Section VII. See also MCC research report 117-790, 2673, December 10, 1951> mentioned on page 25 Section VII, above. The suggested possible formation of traces of chlorphenols by air dilution is mentioned on page 10, Section VII. At one time the chlorine gas was filtered, but this seems unnecessary in view of the use of iron as a catalyst in the chlorlnator. Trichlorobenzene. The Krummrich plant laboratory, February 26, 1951, gave a limited approval of a French sample of trichlorobenzene sub mitted by MCL. Copies of the following reports, concerning the suitability of' trichlorobenzene supplies have been sent to MCL, May 7, 1948. "A Method of Determining the Stability of Trichloro benzene" II7-I987, Munch and Ashworth, April 25, 1948 "Trichlorobenzene and Pyranol 1467 (infrared Section)" 117-1987, Part I, Sherman. February 23, 1950. "Tentative Amendment to the Plant Process on TCB" 117-2032, Hubbard and Steahly, February 26, 1948. DSW 257250 STLCOPCB4061369 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 9 Specifi cations Comments on Flaw Materials, contd. Trlchlorobenzene, contd. On November 3, 1950, Dr. Jenkins,in reply to a request for information on history "of trouble with the chloride limit, stated that TCB, made at the Krummrich plant around 1948, had shown poor stability, and the cauBe had been found to be shortage of catalyst in the chlorination stage of manu facture of the TCB. MCL examination of samples of TCB is discussed in Research Progress reports 347E 355E and 4l6A 50/175/2 Nov.50 (unsatisfactory on electrical tests). 51/16/1 Jan.51 examination of research samples 50/193/1 Nov.50 examination of Prodelec Co. sample 52/19/1 Mar.52 French TTB sample failed on tests but gave passable Pyroclor. 52/1/9 etc.Nov.52 I.C.I. sample satisfactory except on chlorides. Attapulgus earth treatment did not correct it. The following samples, representing raw materials, have been sent to MCL at various times Attapulgus Earth August 23, 1949 Tin-Tetraphenyl Benzene as used for making diphenyl at Anniston January 9, 1950 (Dec.13, 1952) January 7, 1948 Diphenyl as made at Anniston January 7, 1948 Trichlorobenzene December 13, 1950 Sample G-4072 of Diphenyl G-4073 of Santowax R . (distilled highboilers) . G-4074 of bottoms of diphenyl still(crude highboilers) sent from Anniston - to Ruabon October 13, 1947 Repeated as 1-146-Dj 25, 1949 DSW 257251 STLCOPCB4061370 IX - 10 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Comments on Raw Materials, contd. Trichlorobenze, contd. . A letter from Mr. Ellenburg, July 14, 1947, discusses the use of higher grade benzene for making TCB, also the quality of bought dichlorobenzene used as raw material. A Krummrich plant report, September 23, 1947, discusses the stabilization of TCB by heating and by treatment with Attapulgus Earth. A MCC teletype message, July 13, 1954, is on file, questioning the chloride content of butyl acetate. DSW 257252 STLCOPCB4061371 IX - 11 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - Aroclor 1142 Crude, Commercial ISSUED DEC 21 STANDARDS DEPARTMENT By. G. Krummrich PI ant PRODUCT CODE NO, 2AO METHOD .IDENTITY cool5 10*0-130-0*-11-03/09 NAME AROCLOR 11*2 CRUDE> COMMERCIAL CHEMICAL FORMULA Mixture 1/6/42 SUPERSEDES SPECIFICATIONS OF VMS. (Ann itfsn) MFC. JOB. MOL. WT. 1 qt. Bottle (Anniston) 2SAMPLE FOR ANALYSIS ___ x 16 oz. W.M. Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Property Specification Appearance and Color Specific Gravity 25/l5.5C Acid Number (mg. KOH/g.) Brown to black oily liquid 1.384-1.397 0.7, max. Method Number Anniston WGK -- 10,084-53 14-49-54 14-46-54 10,114-53 10,087-53 RESTRICTED SPECIFICATIONS Acid Number of the crude, which is stored in non-lacquered metal con tainers shall be 0.2 mg. KOH/g. max. EXTERNAL SPECIFICATIONS None DSW 257253 STLCOPCB4061372 IX - 12 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - Aroclor 1148 -------------------------- -------------- __ ISSUED APR 11 1955 STANDARDS 0m"T,'r' ~ PRODUCT CODE 246 PRODUCT (Trade name) AROCLOR 1148 p roduct (Chemical name) METHOD IDENTITY SALCI CODE 104Q-l40-04/ll-03/0Q TYPE TYPE CHEMICAL FORMULA Mixture SUPERSEDES SPECS OF 11/16/40 aECI. JOB NO. SAMPLE FOR ANALYMS __ 2 X 16 oz. W. MOL WT. u Sales M. Bottles___________ UNCLASSIFIED SPECIFICATIONS Routine Tests Property Specification Method Number Appearance Color Specific Gravity at 65/15.5C Oily liquid Brown to black 1.410-1.420 WC-K 10,084 10,084 10,114 Anniston -- 14-4-52 Acid Number (mg. KOH/g.) 0.7, max. 10,087 14-42-54 RESTRICTED SPECIFICATIONS Acid Number of the crude which is Btored In non-lacquered metal con tainers shall be 0.2 mg. KOH/g., max. DSW 257254 STLCOPCB4061373 ISSUED DEC 21 1954 smm department By_ r*"nmrich Pjant IX - 15 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - Aroclor 1154 Crude, Commercial cooeUmoT 246 - **LDEES 1040-160-04/11-05/09 name AROCLOR 1154 CRUDE, COMMERCIAL CHEMICAL FORMULA WlXtUre MOl_. WT< _________ SUPERSEDES SPECIFICATIONS OF ll/lO/MU MPf. JOB. 1 qt. Bottle (Anniston) 2SAMPLE FOR ANALYSIS ___ x l6^z. W.M. Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Property Specification Appearance and Color Specific Gravity 65/l5-5C Acid Number (mg. K0H/g.) Brown to black viscous liquid 1.500-1.510 0.7, max. Method Number Anniston WGK 10,084-53 14-49-54 14-46-54 10,114-55 10,087-53 RESTRICTED SPECIFICATIONS Acid Number of the crude, which is stored in non-lacquered matal con tainers shall be 0.2 mg. K0H/g., max. EXTERNAL SPECIFICATIONS None DSW 257255 STLCOPCB4061374 IX. ISSUECDEC 21 1954 SUKEAKGS DEPAHTMEMT w e.m. Krummnch Plant By--------------------------------------------------- SPECIFICATIONS AND TEST METHODS, contd. IX - 14 Specifi cations Specifications for Finished Goods - Aroclor 1160 Crude, Commercial cooenoT. 246 -- code8 1040-.170-04/11-03/09 name AROCLOR 1160 CRUDE, COMMERCIAL CHEMICAL FORMULA Mixture 1/6/42 (Anniston) SUPERSEDES n/lO/hn SPECIFICATIONS OF **/ LO/ Tu SPECIAL MFr.. JOB 1121&9J MOL. WT. 1 pt. can (Anniston) iftliilifl2SAMPLE FOR ANALYSIS ___ x 16 oz. W.M. Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Property Specification Appearance and Color Specific Gravity 90/l5*5C Acid Number (mg. KOH/g.) Brown to black viscous sticky mass 1.558-1.572 0.7, max. Method Number Anniston WGK 10,084-53 14-49.54 14-46-54 10,114-55 10,087-53 RESTRICTED SPECIFICATIONS Acid Number of the crude, which is stored in non-lacquered metal con tainers shall be 0.2 mg. K0H/g., max. EXTERNAL SPECIFICATIONS None DSW 257256 STLCOPCB4061375 IX - 15. Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - Aroclor 1162 PRODUCT CODE 246 gMETHOI > IDENTITY 1-- product frrade name) AROCLOR 1162 p ro Du c T (Umncai name) j sales code 1 1040-180-04/11-03 TYPE TYPE ISSUED 1APR j )d55 STANDARDS OcPARTMENf Wm. e. Krummrich P|ant By. CHEMICAL FORMULA SUPERSEDES SPECS OP 11/18/48 Mixture MOL VT. ECML JO* NO. USE Sales 1 AMPLE POR AM ALYSI9 2 x 16 oz. W. M. Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Property Appearance Color Specific Gravity at 90/15.5C Acid No. (mg. KOH/g.) Specification Viscous liquid Brown to black 1.577-1.587 0.7, max. Method Number 10,084 10,084 10,114 10,087 RESTRICTED SPECIFICATIONS Acid Number of the crude which is stored In non-lacquered metal con tainers shall be 0.2 mg. KOK/g., max. DSW 257257 STLCOPCB4061376 v ' IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 16 Specifications Spe^cl^fi^cations_for_Crude_Solid_Aroclor,s^ (Finished Products) 1168 II69 2565 4065 5060 Method Number Appearance and Colour Acid number Hold Point C. ASTM Softening Point C. Gray to Grey to black black cryst. cryst. powder , powder Black brittle resin Black brittle resin Black brittle resin 10,084-40 -- 145 to 165 ---- - -- 225 to 250 ---- 0.5 --- to 1.0 ---- ---- ---- 10,870-40 ---- 10,127-40 66.0 to 72.0 66.0 to 72.0 110.0 to 115.0 10,085-40 DSW 257258 STLCOPCB4061377 IX - 17 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - Montars 3 and 4 PRODUCT CODE 246 product (Trade name) method identity MONTARS 5 AND 4 p roduct (Chemical none) CHEMICAL FORMULA sales CODE * TYPE TYPE ISSUED APR jj i955 STANDARDS DEPARiMifij Kfummrich Plant By_________ Mixture SUPERSEDES SPECS OF SPECIAL JOB NO. MOL WT. USE Sales SAMPLE FOR ANALYSIS 2 x 16 oz. W. M. Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Property Specification Method Number Appearance- Black solid *Mont;ar 3 6405-003-04-03/09 Montar 4 6405-004-04-03/09 11,321 GENERAL INFORMATION Physical Properties (typical values) Montar 3 Softening Point 120-170C Acidity . Slightly basic Chlorine Content 50-52# cao 5-10# Fe 0.3-0.6# Montar 4 140-200C Slightly basic 54-56# 5-10# 0.5-1.0# DSW 257259 STLCOPCB4061378 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 18 Specifi cations Specifications for Finished Goods - Aroclor 1242 (Pyranol 1499) 27 PRODUCT CODE NO. g-TU METHOD IDFNTITv code5 1040-240-04/11-03/09 name AROCLOR 1242 (PYRANOL 1499) CHEMICAL FORMULA Mixture SUPERSEDES 8/22/41SPECIFICATIONS OF SPECIAL MFC. JOB ___ MOL. WT, ISSUED FEB 14 1955 SUHDA80S DEPARTMENT m' ' ^ru"'nrich Plant "By. 3 xSAMPLE FOR ANALYSIS ___ 5 Pt. Amber Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Property Specification Method Number Color APHA 100, max. Condition . Clear Specific Gravity at 25/l5.5C 1.381-1.392 Acidity (mg K0H/g.) 0.010, max. Moisture (H20) 33 ppm >, max. Refractive Index at 25C 1.6245-1.6265 Free Chlorides 0.10 ppm., max. Pour Point -14C Or lower Dielectric Constant 1000 cycles, 100C 4.7-4.9 Resistivity at 100C 500 VDC and O.l" gap 500 x 10 ohm-em.. min Corrosion Test, 6 hrs. at 210C with bright aluminum foil Change in weight of A1 0.0# Color APHA 150, max. Condition Clear Acidity (mg KOH/g.) 0.010, max. Free Chlorides 0.10 ppm., max. WGK Anniston 10, 084-53 14-44-54 10, 084-53 -- 10, 114- 53 14- 49-,54 10, 087-53 14- 42-54 10, 620-53 14- 53-.54 10, 125-53 14-34-54 10, 118-53 14-48-54 10, 115-53 14- 47- 54 11, 608-54 14- 36-54 O VO 11, 54 14- 35- 54 10, 126- 53 14- 55- 54 General Tests (made only on request) Dielectric Strength at 25C Sulfates Fire Point Viscosity at 100p Distillation Range (ASTM D-20, 1056 90% 35 K.V., min. None None 82-92 SUS Corrected) 325C, min. 366C, max. 11,605-53 -- 12,169-54 -- 10,123-53 14-28-54 10,086-54 14-4-52 10,117-54 14-31-54 (over) DSW 257260 STLCOPCB4061379 IX - 19 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - Aroclor 1242 (Pyranol 1499) contd. GENERAL INFORMATION Specific Heat at 25C. Coefficient of Expansion (25 - 65C.) Fixed Chlorine 0.50 0.00068 cc/cc/C. 41.5 - 42.5 % NOTE; Mr. Harden, August 1950, reporting on his visit to the Anniston plant, gave a run of test results on Aroclor 1242 DSW 257261 STLCOPCB4061380 IX - 20 Specifi cations IX. . SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - Aroclor 1248 ISSUED SEP 9 7954 STANDARDS DEPARTMENT Wm. 0. Krummrrch PJarvt PRODUCT CODE NO. ,c METHOD c40IDENTITY cool51040-260-04/ll-7)5.................. ............ name______ Aroclor 1248 CHEMICAL FORMULA Mixture SUPERSEDES ft/oo/ln SPECIFICATIONS OF SPECIAL yrfl. JOB mol. wt. --Dielectric Grade Material - 3 x 5 pt. Amber Bottles AllSAMPLE for other uses ANALYSIS ___ W. M. Bottles 3 x 16 oz. UNCLASSIFIED SPECIFICATIONS ./ Routine Tests Property Specification Method Number Appearance and Color Colorless to light yei.- 10,084-53 green liquid; APHA 100, max. Condition Clear 10,084-53 Specific Gravity 65/15.5C 1.405-1.415 10,114-53 Acid Number (mg. KOH/gram) 0.010 mg., max. 10,087-53 Moisture (HzO) 35 ppm, max. 10,620-53 Viscosity at 54.4C (SUS) 73-80 seconds 10,086-53 The Aroclor 1248 - Dielectric Grade Material (as Pvranol 1498) shall meet the following additional specifications: Refractive Index at 25C Inorganic (free) Chlorides Pour Point Dielectric Constant at 100C 1000 cps Resistivity at 100C, ohm-cm z: 10 minimum at 500 V-DC, 0.1 "Gap" I.6285-I.6305 0.10 ppm, max. 0C, max. 4.5-4.7 500 10,125-53 10,118-53 10,115-53 11,608-54 11,607-54 Corrosion Stability Test 10,126-53 (After a sample containing one gram of aluminum foil, 0.003H thick, is heated for 6 hours at 210C with Aroclor, the aluminum must not show corrosion by change of appearance or weight and the sample shall conform to the following requirements): Corrosion of Aluminum Foil None (over) DSW 257262 10,126-53 STLCOPCB4061381 IX - 21 Specifi cs v>j. oxis IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - Aroclor 1248, contd. The Aroclor used in the corrosion test should meet the following specifications after the test: Acid Number (mg. KOH/gram) Inorganic (free) Chlorides Color Condition 0.010 mg., max. 0.10 ppm. max. APHA 150, max. Clear 10,087-55 10,118-55 10,084-53 10,084-53 General Tests (for Dielectric Grade Material only - to be run on request): Sulfates Distilling Range (corrected for stem and barometric pressure): 10# Distilled by weight 90# Distilled by weight None 345C., min. 385C., max. 12,169-54 10,117-5*1 Fire Point, C., min. Dielectric Strength at 25C. None to Boiling Point 10,123-55 35 KV, min 10,605-55 RESTRICTED SPECIFICATIONS None EXTERNAL SPECIFICATIONS None DSW 257263 STLCOPCB4061382 IX - 22 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Good3 - Aroclor 1254 (Pyranol 1476) 27 "RODUCT . CODE NO. 240 METHOD IDENTITY---------- cod!S 1040-280-04/11-03/09 NAME AROCLOR 1254 (PYRANOL 1476) CHEMICAL FORMULA MlXtUre___________________________________ SUPERSEDES 8/27/41SPECIFICATIONS OF SPECIAL MFC. JOB : ___MOL. wt. ISSUED FEB 14 1955 STANDARDS DEPARTMENT Krummrich Plant By______ ______________ Ah^ALYsi:R 3 x 5 Pt. Amber Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Property Specification Method Number WGK Anniston Color ' Condition Specific Gravity at 65/15.5C Acidity (rag KOH/g.) Moisture (H2O) Refractive Index at 25C Free Chlorides Pour Point Dielectric Constant 1000 cycles, 100C Resistivity at 100C 500 VDC and 0.1" gap Corrosion Test, 6 hrs. at 210C with bright aluminum foil Change in weight of A1 Color Condition Acidity (mg KOH/g.) Free Chlorides APHA 100, max. Clear 1.495-1-505 0.010, max. 35 ppm*, max. 1.6370-1.6390 0.10 ppm., max. 7-12C 4.15-4.35 500 x 109 ohm-cm., 0.0# APHA 150, max. Clear 0.010, max. 0.10 ppm., max. min. 10,084-53 14-44-54 10,084-53 ----10,114-53 14-49-54 10,087-53 14-42-54 10,620-53 14-53-54 10,125-53 13-34-54 10,118-53 14-48-54 10,115-53 14-47-54 11,608-54 14-36-54 11,604-54 14-35-54 10,126-53 14-55-54 General Tests (made only on request) Dielectric Strength at 25C Sulfates Fire Point Viscosity at 210F Distillation Range (ASTM D-20, 10# 50# 90# 35 K.V., min None None 44-48 SUS Corrected) 366-378C 372-33C 383-396C (------- \ 11,605-53 -- 12,169-54 -- 10,123-53 14-28-54 10,086-54 14-4-52 10,117-54 14-31-34 DSW 257264 STLCOPCB4061383 IX - 23 Specifi k cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - Aroclor 1254 (Pyranol 1476), contd. GENERAL INFORMATION Specific Heat at 25C. Coefficient of Expansion (25-65C) Fixed Chlorine 0.27 0.00066 cc/ccC. 54.5 - 55.5# EXTERNAL SPECIFICATIONS Comell-Dubilier Resistivity at 100C. (500 VDC and 0.1" gap) 9 1500 x 10 ohm - cm 11,604-54 14--55-54 Paint Customers Specific Gravity at 65/15.5C. 1.495-1.505 10,114-53 14--49-54 Acidity (mg KOH/g.) Color 0.010, max. APHA 100, max. 10,087-55 14--42-54 10,084-53 14--44-54 Moisture (H2O) 35 ppm., max. 10,620-53 14--55-54 Viscosity at 210F. 44-48 SUS 10,086-54 14--4-52 Flash Point None 10,123-55 14--28-54 NOTE: Mr. Harden, August 1950, reporting on his visit to the Anniston plant, gave a run of test results on Aroclor 1254. DSW 257265 STLCOPCB4061384 IX - 24 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - Aroclor 1260 (Pyranol 1482) 27 PRODUCT 0i. METHOD CODE NO. _______________ IDENTITY code 1040-290-04/11-03/09 name AROCLOR 1260 (PYRANOL 1482) CHEMICAL FORMULA MlxtUTC______________________________ SUPERSEDES 8/27/41SPECIFICATIONS OF MSFPCE.CJIAOLB ISSUED FEB 14 1955 mol. rr.------ STANDARDS DEPARTMENT Wm. <5. Krummrich Plant By------------------------------------- analysisw 3*5 Pt. Amber Bottles UNCLASSIFIED SPECIFICATIONS Routine Test3 Property Specification Method Number WGK Anniston Color Condition Specific Gravity at 90/l5.5c Acidity (mg K0H/g.) Moisture (H2O) Viscosity at 210F APHA 150, max. Clear 1.555-1-566 0.014, max. 35 ppm., max. 72-78 SUS 10,084-53 14-44-54 10,084-53 -- 10,114-53 14-49-54 10,087-53 14-42-54 10,620-53 14-53-54 10,086-54 14-4-52 The Aroclor 1260 Dielectric Grade Material (as Pyranol 1482) shall meet the following additional specifications: Refractive Index at 25C Free Chlorides Pour Point Distillation Range (ASTM D-20, 10# by weight 50# by weight 90# by weight Corrosion Test, 6 hrs. at 210` with bright aluminum foil Change in weight of A1 Color Condition Acidity (mg KOH/g.) Free Chlorides 1.6455-1.6470 0.10 ppm., max. 25-34C Corrected) 385-398C 390-404C 400-420C 0.0# APHA 150, max. Clear 0.014, max. 0.10 ppm., max. 10,125-53 14-34-54 10,118-53 14-48-54 10,115-53 14-47-54 10,117-54 14-31-54 10,126-53 14-55-54 DSW 257266 (over) STLCOPCB4061385 IX - 25 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - Aroclor 1260 (Pyranol 1482) contd. General Tests (made only on request) Dielectric Strength at 50C Resistivity at 100C. 500 VDC and 0.1" gap Fire Point ` Fixed Chlorine 50 K.V.,pmin. 11,605-53 -- 500 x 10y ohm-cm.,min. 11*607-53 14-55-54 550C., min. 59.5 - 60.5# 10,125-53 14-28-54 10,088-53 14-15-54 GENERAL INFORMATION . Dielectric Constant 1000 cycles, 100C. Evaporation Loss after 6 hours at 100C. Stability test - after 50 days at 100C. in glass sealed in air. 5.6 - 5.8 0.2#, max. No liberation of chlorine or chlorides 11,608-54 14-56-54 10,116-55 14-52-54 DSW 257267 STLCOPCB4061386 IX - 26 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - Aroclor 1262 PRODUCT CODE METHOD IDENTITY ISSUED APR j j ld55 STANDARDS department G.Win. Krummrich PJ*nt SALES CODE product (Trade name) AROCLOR product (Chemcal name) 1262 CHEMICAL FORMULA TYPE TYPE Mixture MOL WT. SUPERSEDES SPECS OF 8/22/41 VEQAL JOB HO. SAMPLE FOR ANALYSIS __ 2 x 16 oz. W, USE Sales M. Bottles__________________________ UNCLASSIFIED SPECIFICATIONS Routine Tests Property Appearance Color Specific Gravity at 90/15.50C Specification Viscous liquid APHA 150, max. 1.577-1.587 Method Number 10,084 10,084 10,114 Acid No. (mg. KOH/g.) Viscosity at 210Pl 0.014, max. 86-100 sus 10,087 10,086 General Information Pour Point (ASTM) Distilling Range Total Chlorine Specific Gravity t coeff 185-1J0oc) 35-38C 390-425C 61.5-62.50 0.00l/C DSW 257268 STLCOPCB4061387 IX - 27 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - Aroclor 1260 - 10# Toluol PRODUCT CODE 246 METHOD IDENTITY ----- . AROCLOR 1260 - 10# TOLUOL cp no du T (frermcol name) CHEMICAL FORMULA ALES CODE 1040-295-04/11-03 TYPE ISSUED APR 21 1955 TYPE stakmws DEPARTMENT Vm. <5. Krummrich Plant SUPERSEDES SPECS OF H/l8/40 Mixture FECIAL JOB NO. -- MOL WT. USE SAMPLE FOR ANALYSIS Sales 2 x 16 oz. W. M. Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Property Appearance Color Composition: Aroclor 1260 Toluol Specification Syrupy liquid Amber 90.5-89.5# 9.5-10.5# Method Number 10,084 10,084 10,194 GENERAL INFORMATION Physical Properties - Aroclor 1260 Specific Gravity at 90/l5.5c Specific Gravity t coeff. (75-130c) Physical Properties - Toluol Specific Gravity at 15.5/l5.5C Specific Gravity t coeff. (15-30c) Physical Properties - 1260 Toluol Mix Specific Gravity at 40/15.5c 1.555-1.566 0.00l/c 0.870 0.00089/C 1.475-1.495 DSW 257269 STLCOPCB4061388 ISSUED APR jj -,u55 SUUims DEPAKTfotrti- By Kru"''nrich Plant IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 28 Specifi cations Specifications for Finished Goods - Aroclor 1262 - 10# Toluol PRODUCT CODE 246 product (Trade name) METHOD identity -- " type AROCLOR 1262 - 10# TOLUOL___________________ product (Chemical name) type 1] SALES CODE 1 1040-510-04/11-03 1 1 CHEMICAL FORMULA Mixture SUPERSEDES SPECS OF 7/7/40 9EQAL JOE NO. MOL VT. USE Sales SAMPLE FOR ANALYMS 2 x 16 oz. W. M. Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Property Specification Method Number Appearance Syrupy liquid 10,084 Color Amber 10,084 Composition: 10,194 Aroclor 1262 90.5-89.5# Toluol 9.5-10.5# GENERAL INFORMATION Physical Properties - Aroclor 1262 Specific Gravity at 90/15.5C Specific Gravity t coeff. (85-130c) Physical Properties - Toluol Specific Gravity at 15.5/15.5C Specific Gravity t coeff. Physical Properties - 1262 Toluol Mix Specific Grayity at 40/15.5*0 1.577-1.587 0.001/C 0.870 0.00089/C 1.497-1.516 DSW 257270 STLCOPCB4061389 IX - 29 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - Aroclor 1254 - 10# Secondary Butyl Acetate MAR 20 1955 PRODUCT CODE 246 PRODUCT (trade METHOD IDENTITY By - ` Krw^^ ALU CODE : ~ 1040-285-04/11-05 TYPE product (theimeal none) TYPE AROCLOR 1254 - 10# SECONDARY BUTYL ACETATE CHEMICAL FORMUL A Mixture MOL WT. SUPERSEDES SPECS OF New 9EOAL JOB NO. USE SAMPLE POR ANALYSIS Sales 2 x 16 oz. . M. Bottles UNCLASSIFIED SPECIFICATIONS AND INFORMATION Routine Tests . ! \ j t I Property Color Composition: Aroclor 1254 Secondary Butyl Acetate Specification APHA 200, max. 90.0-91.0# 9.0-10.0# Method Number 12,215-34 12,208-54 General Information Specific Gravity of Aroclor 1254 at 65/15.5c Specific Gravity of Secondary Butyl Acetate at 25/l5.5C 1.495-1.505 (changes 0.00095/^0 0.866 Specific Gravity Range of Mixture at 29/l5.5C 1.423-1.449 DSW 257271 STLCOPCB4061390 M e th o d N o . 1 0 ,0 8 4 -4 0 1 0 ,1 2 7 -4 0 1 0 ,5 7 8 -4 1 1 0 ,0 8 6 -4 0 DSW 257272 OP fO^-1 c 4> P XHWa cOo Kto P C o T3 GOC 73 CD 73 4-5 Pco c oQ o CO o o o C3 T3E-* CO Q> co QH c P Dh b O 4-1 E-t O< m Go ft* o 0) eo P CO Cm O 4> XQ er X O rH X rH flj a> e > C'-' P o p bO u in n < ri 0) 0* . r-' S5 ft P CO P a> p o rH p O CM o rH ^ rH 0> C K r* P CO CD S SEW IT. bO rH 4) VO 4* PP p Q- 44- k P X co P P-t LT\ rH O rH zo* rH rH -=f .=}- 1 1t On f CD e' O en in O o' o rH rH rH tn a o in on o o 4> P rH , > H P J>> 3 ,, rH rH Ph f- rH Cm Q) CM rH CO o OP* n O p bOft OP <0 cd a 0) c rH .o 0) rH (4 o P rH 4> on O C- CVJ P CO 'O g-s S o p P &a in o CD CM U fct O X73 XO xo a U0) rH H 4) u c X rH O rH ON P P rH VO CM iH C0 4> UP P rH 05 o in in OJ o p in CM CM X o rH rH 4) CO 4) C . XrH tn VO rH 4> . CM rH OH-O P CO * PO 4) to a p ?> H Ph o * o VO H o p in on rH Ph 3 o p o o 73 C 3 b 0 4> p OC CP C0 O U Q-4 cd 4) T3 a rH aO <X O < in -=r o Oo on CD < O CO in o o X CO e w oo X CO X 73 H C bC <E 4) G 4) s rH O P C~ PK C0 >* B in'-- pT 3 O rH O o i >* ua> 3 P a H o z: c P e w- * p c o a, to ,C p p P 4) Oo Jj- 11 o CO rH CO in o O in 00 o cT o' o rH p p in 3 VD in ao co o p a VD o o Op pP o O o ON o in p in o b 47 Co op X in On VO i* 4) GG 3P O P4 T3 o O rH cO tO: pP 4U> 3 P oO ft- E-* p G P o a w c p c 4) P Cm O CO JO* 1 On CO O O P O P CM o O om pp o vo p o VO Tn oP c o 4-> H CO CO P H> co r3coHo SM hO CH O<M C <0 oOmN cb>dO 3~3~r) i--iadi p p o co CO -P co > p pn CO 'O OC oo CO o P 4) > CO > P C p p P CO p m & o ucod STLCOPCB4061391 IX - 31 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - 60# Aroclor 1260 - 40$ Trlchlorobenzene (Pyranol 1467) ISSUED JAN 28 1955 PRODUCT , CODE NO. A-24P METHOD IDENTITY STANDARDS DEPA"T`!ENT SALES Wm. G. Yr :,'i . CODE 1050-100-11^03 name 60# AROCLOR 1260 - 40# TRICHLOROBENZENE (PYRANOL 1467) Chemical Formula - Mixture Mol. Wt. Supersedes Specification of 8-27-541 Special Mfg. Job ------- Samples for Analysis ? x 5 pt, amber bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Property Specification Method Number Color Condition Specific Gravity at APHA 150, max. Clear I.560-I.568 10,084-53 10,084-53 10,114-53 15*5/15*5 C Acidity (mg KOH/g.) Moisture (H2o) Refractive Index at 25C Free Chlorides Dielectric Strength 0.014, max. 30 ppm., max. 1.6137-1.6147 0.10 ppm., max. 35 KV, min. 10,087-55 10,620-53 10,125-55 10,118-55 11,605-53 Resistivity at 100C 500 VDC and 0.1 gap 100 x 10 ohm-cm., min. 10.604-34 Viscosity at 100F Pour Point Tin Tetraphenyl Distillation Range: First Drop Below 270bC 90# by wt. 52-56 SUS -32C, max. 0.115-0.135# by wt. (ASTM D-20 , Corrected} 200C, max. 40$, max. 595-415*0 10,086-54 10,115-55 11,553-55 lO.HT-i21 Corrosion Test, 6 hrs. at 210 C 10.126-33 with bright aluminum foil Change in weight of A1 0.0# Color Condition Acidity (mg KOH/g.) Free Chlorides APHA 200, max. Clear 0.014, max. 5.0 ppm., max. . DSW 257273 STLCOPCB4061392 IX - 32 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - 60# Aroclor 1260 - 40# Trlchlorobenzene (Pyranol l467)/contd~] GENERAL TESTS (made only on request) Dielectric Constant 1000 cycles, 100C. Fixed Chlorine Fire Point 3.7-4.0 59.1# min. None to Boiling Point 10,608-54 10,088-53 10,123-53 Arc Formed Combustible Gases 1.0#, max. Electrical Stability (Aged 96 hours at 100C.covered jar, 15# air). Decrease in resistivity 10# max. 10,71110,121-54 Analysis of each 10 ml. fraction of a fractional distillation Chlorine/Hydrogen Ratio^ Arc Formed Combustlble'l XL, min. Gases J^-?1.5# max. GENERAL INFORMATION Dielectric Constant 1000 cycles, 25eC. 4.0 - 4.3 Inerteen PPO-TCB has the same specification as Pyranol 1467, but it contains 0.20# of glycidyl phenyl ether Instead of 0.125# of tlntetraphenyl. The fire point is reported every time for Inerteen PPO-TCB. DSW 257274 STLCOPCB4061393 IX - 33 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - 45# Aroclor 1260 55# Tri-Tetrachlorobenzene Blend (Pyranol 1470) ISSUED JAN 1355 PRODUCT .- CODE NO. A-246 METHOD IDENTITY STANDARDS DEPARTMENT . Wm. G. Krummrich Plant SALES ,, 1050-110-11-03-------------------------------- CODE _ ~ name 45# AROCLOR 1260 - 55# TRI-TETRACHLORQBEKZENE BLEND (PYRANOL 1470) CHEMICAL FORMULA MlXtUTe_________________________________________ MOL> WT, _________ NewSUPERSEDES SPECIFICATIONS OF SPECIAL MFC. JOB 3 x 5 PtSAMPLE FOR ANALYSIS ___ Amber Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Property Specification Color APHA 150, max. Condition Clear Specific Gravity at 1.563-1.571 15*5/15 r5C . Acidity (mg KOH/g.) 0.014, max. Moisture (H2O) 30 ppm., max. Refractive Index at 25C 1.6075-1.6085 Free Chlorides 0.10 ppm., max. Dielectric Strength at 25C 35 K.V., min. Resistivity at 100C, 500 100 x 10 ohm-cm., min. VDC and 0.1 gap Viscosity at 100 F 41-45 SUS Pour Point -44C, max. Tin Tetraphenyl . O.II5-O.135# by wt. Distillation Range: (ASTM D- 20, Corrected) First Drop 210C, min. 35# by volume 240-256C 55# by volume 290-330oC 65# by volume 385-400oC 90# by volume 395-4l5C Corrosion Test, 6 hrs. at 210 C with bright aluminum foil Change in weight of A1 0.0# Color APHA 200, max. Condition Clear Acidity (mg KOH/g.) 0.014, max. Free Chlorides 5.0 ppm., max. Method Number 10,084-53 10,084-53 10,114-53 10,087-53 10,620-53 10,125-53 10,118-53 11,605-53 10,604-54 10,086-54 10,115-53 11,533-53 10,117-54 10,126-53 (over) DSW 257275 STLCOPCB4061394 IX - 34 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - 4-5$ Aroclor 1260 55# Trl-Tetrachlorobenzene Blend (Pyranol 1470), contd. GENERAL TESTS (made only on request) CVJ CO K-\ Dielectric Constant 1000 cycles, 100C. 10,608-54 Fixed Chlorine 60.0 - 61.0 10,088-53 Fire Point None to Boiling Point 10,123-53 Arc Formed Combustible Gases 1.0# max. 10,711- Electrical Stability (Aged 96 hours at 100C. covered jar. 15# air) 10,121-54 Decrease :in Resistivity 10#, max. GENERAL INFORMATION Dielectric Constant 1000 cycles, 25C. 4.5 - 4.9 Inerteen PPO - TTCB has the same specification as Pyranol 1470, but it contains 0.20# of glycidyl phenyl ether instead of 0.125# of tintetraphenyl. DSW 257276 STLCOPCB4061395 IX - 55 Specifi cations IX, SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - Trlchlorobenzene (Pyranol 1478) PRODUCT CODE NO. NAME _____ JP-?33 METHOD IDENTITY TRICHLOROBENZENE cool* 8510-000-05-03 (PYRANOL 1478) ISSUED JAN 23 1355 STANDARDS DEPARTMENT CHEMICAL FORMULA Mixture* MOL. WT. Win. G. Krummrich Plant By--------------------------------------- SUPERSEDES q /1,. SPECIFICATIONS OF O/ C l /`ll SPECIAL MFC. JOB an'alysiow 3 x 5 pt Amber Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Property Specification Method Number Color APHA 15, max. Condition Clear Specific Gravity at 1.460-1.477 15*5/15.5C . . Acidity (mg KOH/g.) 0.014, max. Moisture (H20) 75 ppm., max. Refractive Index at 25C 1.5680-1.5715 Free Chlorides 0.10 ppm., max. Crystallizing Point 10C, max. Dielectric Strength at 25C 30 K.V., min. Distillation Range: (ASTM D85O, Modified) (Corrected for Stem and Barometric Pressure) First Drop 205 C, min. 556 by volume 210C, min. 50# by volume 213C, min. 90^ by volume 215C, min. Corrosion Test, 6 hrs. at 210c with bright aluminum foil Change in weight of A1 0.0 Color APHA 200, max. Condition Clear Acidity (mg KOH/g.) 0.014, max. Free Chlorides 0.10 ppm., max. 10,105-53 10,105-53 10,114-53 10,109-52 10,620-53 10,125-53 10,118-53 10,107-53 11,605-54 10,126-53 GENERAL TESTS (made only on request) Fire Point Fixed Chlorine GENERAL INFORMATION Dielectric Constant 1000 cycles, 100C. None to Boiling Point 58.556, min. 10,123-53 10,088-53 3.8 - 4.3 DSW 257277 Viscosity at 100C. 28 - 32 SUS Of,,theKvarious isomers of Trichlorobenzene plus STLCOPCB4061396 ISSUED JAN 28 1955 STANDARDS DEPARTMENT Wm. 0. Krummrich Plant By._______________ IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 56 Specifi cations Specifications for Finished Goods - 75/6 Aroclor 1254 25% Trichlorobenzene (Pyranol 1481) PRODUCT , CODE HO. A-24P METHOD IDENTITY looV 1050-120-11-03 name 75$ AROCLOR 1254 - 25# TRICHLOROBENZENE (PYRANOL l48l) CHEMICAL FORMULA MlXtUTe MOL. WT. ~~ SUPERSEDES SPECIFICATIONS OF NeW SPECIAL MFC. JOB lXvlsw 3 x 5 Pt. Amber Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Property Specification Method Number Color Condition Specific Gravity at 15.5/15.5C .. Acidity (mg KOH/g.) Moisture (H2O) Refractive Index at 25C Free Chlorides Dielectric Constant 1000 cycles, 100C Resistivity at 100C, 500 VDC and 0.1 gap Viscosity at 100 F Pour Point Corrosion Test, 6 hrs. at 210 C with bright aluminum foil Change In weight Color Condition Acidity (mg KOH/g.) Free Chlorides APHA 150, max. Clear 1.525-1.535 10,084-55 10,084-53 10,114-53 0.010, max. 55 ppm., max. 1.6205-1.6215 0.10 ppm., max. 4.1-4.6 100 x lOe ohm-cm., min. 10,087-53 10,620-53 10,125-53 10,118-53 10,608-54 10,604-54 70-82 SUS -15C or lower 10,086-54 10,115-53 10,126-53 0.0J6 APHA 200, max. Clear 0.010, max. 0.10 ppm., max. GENERAL TESTS (made only on request) Fire Point Distillation Range: 1st Drop Below 270C 90% None to Boiling Point (ASTM D-20, Corrected) 205 C, min. 25max. 380-595C 10,123-53 10,117-54 GENERAL INFORMATION DSW 257278 Fixed Chlorine 55-5$, rain. STLCOPCB4061397 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 37 Specifi cations ISSUED JUN 6 195tj Specifications for Finished Goods - 60$ Aroclor 12^ft m' ' *fu'nmrich Pianl 40$ Trlchlorobenzene ~ PRODUCT (Trade name) type PYRAN0L 1488 p roduct (Ckenical name) type 60$ AROCLOR 1260 - 40$ TRICHLOROBENZENE CHEMICAL FORMULA Mixture PRODUCT CODE A-246 method identity SALES CODE. 1050-130-11-03 MOL WT. SUPERSEDES SPECS OF 8/27/41 FECIAL JOE NO. ----- UE Sales SAMPLE FOR ANALYSIS 3 x 5 Pt. Amber Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Property Specification Method Number Color - APHA 150, max. Condition . Clear Specific Gravity at I.56O-I.568 15.5/15?5"C Acidity (m& KOH/g. 0.014, max. Moisture (H2O) 35 ppm., max. Refractive Index at 25C 1.6137-1.6147 Free Chlorides 0.10 ppm., max. Dielectric Strength at 25C 35 KV, min. Resistivity at 100C 100 x 109 ohm-cm., 500 VDC and 0.1" gap Viscosity at 100 F 52-56 SUS Pour Point -32C, max. Distillation Range (ASTM D-20, corrected) First Drop 200C, min. Below 270C 40$, max. 90$ by wt. 395-4l5C Corrosion Test, 6 hrs. at 210 C with bright aluminum foil Change in weight of A1 0.0$ Color APHA 200, max. Condition Clear Acidity (mg. K0H/g.) 0.014, max. Free Chlorides 0.1 ppm., max. min. 10,084-53 10,084-53 10,114-53 10,087-53 10,620-53 10,125-53 10,118-53 11,605-53 10,604-54 10,086-54 10,115-53 10,117-54 10,126-53 DSW 257279 General Tests (Made only on request) Dielectric Constant 1000 cycles, 100C Fire Point Fixed Chlorine Arc Formed Combustible Gases 3.7-4.0 None to boiling point 59*1#, min. 1.0$, max. 10,608-54 10,123-53 10,088-53 10.711- STLCOPCB4061398 IX - 38 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Goods - 60# Aroclor 1260 40# Trlchlorobenzene, contd. Electrical Stability (aged 96 hours at 100C., covered Jar, 13# air) Decrease in Resistivity 10#, max. 10,121 EXTERNAL SPECIFICATIONS Wagner Electric Company Power Factor (60 at 100C.) 2#, max. Resistivity at 100C. 500 VDC and 0.1" gap . 3000 x 10^ ohm-cm min. 11,608 11,607 General Information Dielectric Constant 1000 Cycles, 23C. 4.0 - 4.3 DSW 257280 STLCOPCB4061399 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 39 Specifi cations Finished Products Spe_ca_fiLcati1ons_fo_r_Muriat_ic Acid 20 B<^. (American) Commercial. PROPERTY SPECIFICATION Method No. Appearance and Colour Turbidity Sulphates as h2so4* AS203 % Assay (HCl) % (max.) (max.) (min.) Colourless to light yellow liquid 1.5 NPA max. Practically clear 10,070-40 10,071-40 0.01 0.0001 51.45 10,073-40 10,074-40 10,072-40 - - - - - * -- --- DSW 257281 STLCOPCB4061400 _ IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 40 Specif!cations and Test Methods . Finished Product Specifications and Test Methods. Close cooperation with the General Electric Company has cleared up certain misunderstandings about the specifications and test methods for electrical grade materials, and there is now very little trouble in meeting G. E.'s requirements. Sometimes, for example, in the past, the acidity figures had been set in terms of mg. NaOH per gram of sample, and sometimes in terms of mg. KOH, and the numerical value of the specification limit had not always been changed to suit, and such points have now been corrected. There had also been confusion between "corrected" and "uncorrected" temperatures in the distillation range test. G. E.'s main plant blend their own Pyranols from MCC Aroclor, and purchased chlorobenzenes, but MCC do the blending for G. E.'s Canadian and West Coast plants, and for G. E.'s licencees. G. E. still receive advance samples of components intended for their use, and samples of finished blends before despatch, though they are coming to rely more on MCC control test work. For example, the "advance" samples of com ponents may be sent along with the sample of the finished blend. A set of the specifications and test methods,as finally established about a year ago between MCC and the customers,is being obtained for MCL. Both G. E. and Westlnghouse give the blends a light treatment with earth to improve the electrical properties? the resistivity, in particular, falls during packing, and during transit of the goods from MCC to the customer. . It will be noted that a mixture of tri-tetrachlorobenzene is largely replacing the trichlorobenzene. This is a change originated by G.E. mainly on grounds of cost. Recently a blend of Aroclor with secondary butyl acetate has come into use (not for electrical purposes). While the butylacetate is being handled, the same fire precautions are observed as with toluene. The butyl acetate mixtures are made in the finished Aroclor vessels CT-0780 and CT-01400. . DSW 257282 STLCOPCB4061401 _* IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 41 Test Methods 10,006-54 Dates 8-9-54 Bys SMKsHOH Materials General Method Tests Distilling Range Method No. 10,006-54 WGK G.M. No. 1 The distillation test method as used by WGK Plant in testing its various products and raw materials is an adaptation of the method as outlined by the Barrett Company for the "Distillation of Nitration and Industrial Pure Benzol. A. Flasks s - The flask shall be the Standard Barrett Benzol Flask of 200-ml. capacity. For testing materials boiling above 100C. the flask will be covered with a layer of' asbestos paper, cutting into the latter a circular hole 1^ inches in diameter, with the center of the hole coincident with the bottom of the flask, and leaving the glass completely bare. The sidearm is not covered. Two rectangular slits are also cut in the asbestos covering the neck of the flask, one on each side of the neck, and the center of each located 90 from a vertical plane bisecting the sidearm of the flask. The rectangular slits shall be 3/8" wide, and 2-i" long. The top and the bottom of each slit shall be 7/8" from the top and bottom of the flask neck. These serve to determine the thermometer bulb position, and the pro gress of the refluxing procedure. Two circular holes are cut in the asbestos covering the bulb of the flask, one on each side, each 1-1/2" in diameter, and the center of each located in the center of the side of the flask bulb. These enable observation of the dry point to be made. For testing materials boiling below, or including, 100cC., uncovered Standard Barrett Benzol Flasks of 200 ml. capacity are used. B. Corks ? - Select a new, sound #10 cork, free from holes of grooves which might cause escape of vapor. Choose a'sharp cork borer of slighly smaller diameter than the thermometer to be used, and employing a slicing action rather than excessive pressure, bore the cork about half through from the bottom, then complete the hole from the top of the cork. The hole must be exactly centered when viewed at each end. Gently DSW 257283 STLCOPCB4061402 IX. SPECIFICATIONS AND TEST METHODS, eontd. IX - 42 . Test Methods 10,006-54 General Method, Distilling Range, Method No. 10,006-54, eontd. Increase the hole-size with a rat-tail file, to fit the thermometer snugly. Discard corks which have split, even partly. Using a similar procedure, bore a hole in a #5 cork to fit the sldearm of the flask snugly. C. Condensers - The distillate is condensed in a straight glass tube 0.5 inch I.D. and 24" long set at an angle of 75 to the vertical. For materials boiling below, or including, 100C., the tube will be cooled in a trough filled with ice-water mixture having a temperature of less than 5C. (measured) throughout the distillation. The trough will be filled so that the entire length of glass in the trough is covered. For materials boiling 100-200C., the trough will be filled to the same extent, but with water only. Distillates which crystallize in the tube must be kept fluid by the use of sufficiently hot water. For materials boiling above 200C., the condenser tube will be air-cooled only. Any crystals must be kept from forming in the tube by playing a flame over its length as needed. D. Receivers s - The receiver shall be either a standard 100-ml. graduated Pyrex cylinder, or one of the formed type distillation receivers. These are made up specially and are graduated from 0-10 ml. and 90-100 ml. in 0.5 ml. divisions along a relatively narrow glass tube, and 10-90 ml. in 10-ml. divisions along the bulb. The overall height is about 11 Inches. The formed receivers are used for materials normally liquid at room, temperatures. The standard 100 ml. Pyrex cylinders are used for materials which crystallize at room temperatures or above. E. . Heat Source; - Only the Bunsen type burner may be used, the entire flame being blue. The Meker types must not be used. A burner shield about 6" in diameter and sufficiently high to fully protect the flame shall be used. DSW 257284 STLCOPCB4061403 v -' IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 43 Test Methods 10,006-54 General Method, Distilling Range, Method No. 10,006-54, contd. F. Thermometers; - The thermometer shall be an Instrument of suitable range for the material being tested. If an accurate thermometer is used. It shall be checked against a U.S. Bureau of Standards Standardized thermometer and the proper corrections applied to the readings. Normally the accurate thermometers used have a range of 35> are graduated in 0.1C. and are capable of being read to 0.05C. Select, if possible, a thermometer which will indicate the anticipated range desired in its upper two-thirds of graduation, so as to prevent the cork or flask from interferring with readings. The usual accurate thermometer will be scaled for three inch immersion so no stem correction need be applied. If, however, a full immersion type thermometer is used, the stem correction is -calculated and applied: The calculation is: -- Correctlon = (No. of degree graduations exposed)(Temp.diff.in)(O.OOI58) 4 The exposed graduations are read from the top of the cork. The temperature difference is the reading of the thermometer minus the temperature of the stem midway of the exposed mercury column as taken by an auxiliary thermometer. The correction shall be added. G. Transite Boards: - The transite board used should be ca. 6" square, 3/16" thick and shall have a hole with a diameter corresponding to the following: Materials boiling below 100C. 100-150C. 150-200C. 200-250C. 250-300c. above 300C. ~ 111 2 diameter hole - 1" diameter hole - 1 i2" diameter hole - 2' -J diameter hole " *0-21 II diameter hole ~ O1 H ^2 diameter hole DSW 257285 STLCOPCB4061404 IX, SPECIFICATIONS AND TEST METHODS, contd. IX-44 Test Methods 10,006-54 General Method, Distilling Range, Method No. 10,006-54, contd. The flasks shall not be set directly on the transite boards during distillations, but shall be set upon a sheet of asbestos paper having a hole whose diameter is slightly smaller than the hole of the transite board. This provides a better seal, to prevent the flame from touching the sides of the flask and super heating the vapours. H. Manipulation s - Swab out the condenser with a piece of dry cloth and a wooden ramrod. 1. Measure 100 ml. of the liquid sample in the receiver and transfer to the flask, being careful not to get any sample into the sidearm. 2. Seat the cork and thermometer, which is at room temperature, in the neck of the flask, adjusting the thermometer so that the top of the expansion bulb, or the top of the upperexpansion bulb, if there are two, is level with the bottom of the sidearm of the flask. Be sure the thermometer is in the center of the neck of the flask, and not inclined to the side. 3. Clamp the flask in place on the asbestos sheet, which rests on a transite board having the proper hole-size previously designated. 4. Connect the flask to the condenser in such a manner that the sidearm extends 2" into the condenser. The neck of the flask and the thermometer shall be in a truly vertical position. 5. Place the receiver in position at the lower end of the con denser tube without further draining or drying. 6. Place water, ice-and*water, or hot water in the trough, as indicated previously, if any is required. 7. The flask is then gently heated until the liquid begins to boil. Use only a Bunsen burner and an all blue flame. Center the flame, while heating, in the middle of the exposed glass at the bottom of the flask. DSW 257286 STLCOPCB4061405 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 45 Test Methods 10,006-54 General Method, Distilling Range, Method No. 10,006-54, contd. 8. As the vapours rise In the neck of the flask, a ring of condensed liquid forms. When this ring of condensed liquid envelopes the bulb of the thermometer and approaches the sidearm outlet, tilt the burner back until the ring subsides back into the flask, and the mercury in the thermo meter recedes. 9. Restore the burner to position and repeat this "refluxing" procedure, which allows the thermometer time to reach the proper temperature. 10. Repeat once more, and when this is accomplished, restore the burner to position and quickly adjust the flame height to that which experience dictates will conduct the distill ation at a rate of 2 drops per second unless otherwise specifically noted. 11. Thermometer readings are taken and recorded at the following intervals? 1st drop - the instant the 1st drop of distillate falls from the end of the condenser tube into the receiver; 1 ml, 3 ml., 5, 10, 20, 50, 40, 56, 60, 79, 80, 90, and then in 1 ml. intervals on up to the dry point. The dry point temperature is read at the instant the last drop of liquid material is vapourized from the bottom q the flask. At this same time, the burner is turned off. Any distillation showing less than 96 ml. recovered must be re-run. 12. The temperatures are all recorded at first .s uncorrected. The barometer is read during the distillation procedure. The net correction incorporating the barometric correction, thermometer correction and stem correction (if required) is calculated and applied to the readings to obtain the corrected readings which are reported. DSW 257287 STLCOPCB4061406 -v ' IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 46 Test Methods 10,006-54 General Method, Distilling Range, Method No. 10,006-54, contd. Corrections for deviation of the barometric pressure from the normal are applied using the following formula: y\Tp = (0.00012 Tfi) C^p) In which ^^T = Change in boiling point B TB = Normal boiling point in degrees absolute P = Change in pressure in mm. Hg (MacDougall "Thermodynamics and Chemistry", p.153.) This correction is added if the Barometer is below 760 mm. and subtracted if the Barometer is above 760 mm. For your con venience, these corrections are already tabulated in a chartat the front entrance to the Laboratory. NOTES; After the completion of a distillation test, the flask shall be disconnected from the condenser, and the condenser tube Immediately wiped dry by means of a cotton patch and a wooden ramrod. The, thermometer is allowed to remain in the flask until the mercury has contracted into the thermometer's expansion chamber, if there is one. Never cool a hot thermometer suddenly. The flasks and receivers are cleaned with the proper reagents and finally rinsed With distilled water and then alcohol. They are then placed in an oven at 110-150C. to dry. Before,, using, the flasks and receivers are blown with filtered air for several minutes. See specific method for details. DSW 257288 STLCOPCB4061407 . - IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 5/25-55 Material: General Method By: SMK,NPA:SMK Test: Color - APHA (Hazen) IX - 47 ' Test Methods 10,007-55 Method NO. 10,007-55 WGK G.M. No. 2 Introduction: The colour of WGK Plant products for which the tints (hues) are not very pronounced are estimated by comparison with standards in 50-nil. tall form Nessler tubes. The standards are made up in accordance with the directions as given in the APHA Standard Methods of WaterAnalysis 7th Ed. 1955# PP* 9# as worked out by A. Hazsn. Preparation of the APHA Stock Solution: 1. Weigh accurately on an analytical balance 1.24-5 gms. potassium chloroplatinate (KgPtClg), containing 0.5 gm. Platinum, and 1.000 g. cobaltous chloride (CoC12.6H2Q) containing about 0.25 g. Cobalt.. 2. Add both components to one liter flask with 100 ml. C.P. HC1 and distilled water. 5. Make up to one liter with distilled water and mix well. This is the APHA stock solution. It has a colour APHA - 500. 4. Keep the stock solution in a black painted bottle. NOTE: In the absence of a reliable supply of potassium chlorcplatinate, chloroplatinic acid may be substituted as follows: Dissolve 0.5 g. metallic platinum in aqua regia; remove nitric acid by repeated evaporation to dryness after adding an excess of hydrochloric acid. Dissolve this product together with 1 gram of cobalt/as above directed, chloride DSW 257289 STLCOPCB4061408 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - -48 Test Methods 10,007-55 General Method, Colour APHA (Hazen), Method No. 10,007-55, contd. Preparation of the APHA Standards: 1_. To prepare standards, add the proper volume of the stock . solution according to the following chart, to a set of matched tail-form, 50-ml. Nessler tubes. APHA std. ml- Stqqft Sol'n. APHA Std. ml. Stock Sol'n. 5 0.5 50 5.0 5 0,5 40 4.0 8 0.8 50 5.0 10 1.0 60 6.0 15 1.5 80 8.0 20 2.0 100 10.0 25 2.5 200 20.0 NOTE; For every unit of APHA, 0.1 ml. of the stock solution used. 2_,, Dilute with distilled water contents of each Nessler tube to the mark. IMPORTANT; The prepared standards should be kept in the closed boxes provided for them to prevent excess evaporation and contamination. Procedure for Colour Determination: 1. Fill a standard 50-ml. tail-form Nessler tube to the mark (to a height equal to that in the APHA Std. tubes) with the material to be examined. 2,, Compare the tube with standards. The intensity of light passing through the samjSLe shall be observed and compared with that of the standard. DSW 257290 STLCOPCB4061409 ._ v - IX, SPECIFICATIONS AND TEST METHODS, contd. IX - 49 Test Methods 10,007-53 General Method, Colour APHA (Hazen), Method No. 10,007-53, contd,, Procedure for Colour Determination, contd. 5. Make the observation by looking vertically downward through the tubes upon a white surface placed in such a position that non-glaring daylight is reflected through the column of liquid,, the regular -daylight lamps can be used for night work. IMPORTANT: Since our products vary in hue, the property sought is light intensity, rather than color (hue, tint). This method is good only up to a color intensity of about 100. The APHA suggests dilution to read the higher values, but we have found that not all materials can be treated in this manner. The results are reported as so many units of Colour APHA ~ "A.PoH.A. 25", or in some cases as "Colour - Hazen 25". Report the result to the nearest APHA standard, or by interpolation between standards. Remarks: The standard Nessler tube (refer to Sargent Catalog #S - 21055) is approximately 12" long with 5/4" O.D0, graduated at 50-ml. mark. DSW 257291 STLCOPCB4061410 IX. SPECIFICATIONS AND TEST METHODS, contd. Date; 8-19-53 Material: General Method By; DKL:SMK Test: Melting Point IX - 50 Test Methods 10,052-51 Method No. 10,052-51 WGK G.Mo No. 3 Apparatus: The melting point apparatus used is the modified Thi%L type described in Drawing No. D-779 by Dept. 116 of Monsanto Chemical Company, J. P. Queeny Plant. The bath liquid is Dow-Coming ' #D.C-550,, and sufficient is used in the apparatus so that the liquid level is coincident with the top inside of the crossarm when the liquid is at the temperature of the test and the thermometer and stirrer are inserted. The bath is heated electrically by means of Nichrome ribbon heating elements. The temperature is controlled with a variable transformer or other suitable voltage controlling device. A lighted magnifier is placed before the bath wiridow to facilitate observation. The melting point tubes are unwashed Pyrex glass capillary tubes, sealed at one end 1.20 + 0.15 mm O.D. and Q.,75 + 0-.15 mm . I.D. and ca. 125 mm long. These tubes are to be stored in clean, and screw capped bottles to protect them from dust. The thermometers, unless otherwise specified are standardized instru ments of 35C. range, graduated in 0.2C. increments and capable of being read to 0.05C. and of the 3-inch or 75 mm Immersion types. Manipulation: 1. Punch enough of the well mixed powdered sample (ca. 200 mesh; into the open end of the capillary tube so that when the tube is righted and tapped and/or gently rubbed with a file, the sample falls to the sealed end to a depth of ca. 0,75 inch. 2. Attach the capillary tube(s) (no more than four) to the proper range thermometer by means of small rubber bands positioned above the liquid level so that the sample(s) lie adjacent to the bulb (reserve! r) of the thermometer. 3 Place the thermometer and sample(s) in the center of the (sample side) arm of the melting point bath at such a depth DSW 257292 STLCOPCB4061411 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 51 Test Methods 10,052-51 General Method, Melting Point, Method No. 10,052-51, contd. 5. contd. that the thermometer will be properly immersed at the test temperature and the sample is clearly visible when viewed through the window with the lighted magnifier. 4. Start the motor-driven stirrer. 5. Adjust the voltage control for the heating element so that the temperature rises rapidly until it is within 10-20C. below the anticipated melting point, and then adjust the rate of heating to 0.1C. per minute (+ 10 seconds) (unless otherwise directed) until the melting point is reached. The rate of heating is very Important. Tests run at other rates must be repeated. The following points may be read: Softening Point: The point at which the material seems to pull away from the side of the tube and becomes mushy. Melting Point: (First Meniscus): The point at which there is first seen a portion of liquid that is perfectly clear extending from wall to wall in the capillary. Complete Melting Point: The point at which the last traces of solid disappears into the liquid melt. ' Report the points required to the nearest 0.1C. after applying bfre necessary thermometer corrections. DSW 257293 STLCOPCB4061412 IX. SPECIFICATIONS AND TEST METHODS, contd IX - 52 Test Methods 10,056-54 Date: 8-12-54 By: SMK, DKL, NPA GWM:WJG Material: General Method Method No. 10,056-44 Test: Total Chlorine in WGK G.M. No. 4 Organics - Parr Sodium Peroxide Bomb Method The chlorine content of. chlorinated organic materials may be determined by means of the Parr Sodium Peroxide Bomb method which converts the organic chlorine to NaCl that is determined by means of a Volhard titration. 1. Scrub a Parr steel (50 Ni) Na202 Bomb thoroughly with a test tube brush in hot water. Do not use acid. Rinse thoroughly with distilled water and dry on a hot plate or in an oven at 110C. Cool to room temperature.. IMPORTANT: Discard any bomb that is badly etched or shows other obvious mechanical defect. 2. A sample, of suitable size to give chlorine equivalent to approximately 40 ml. of 0.1 N AgNOs (0.14 g. Cl) is used. If the material being tested is a solid, the sample must be ground to pass a 60 mesh sieve. If the material to be tested is a liquid, it is weighed onto 2.0 g. of sodium carbonate A.R. contained in the fusion cup. In some Instances it is neces- . sary to add some powdered sugar to give sufficient heat for a good fusion. CAUTION: In no case should more than 1.00 g. total organics be fused in this manner, unless experience has shown it to be safe. PUT 0 N SAFETY GLASSES l 5. Add one scoop (ca. 14 g.) Nae0a to the bomb. 4. Stir the mixture in the bomb with a clean dry stirring rod (1/8-in x 6-in.) until thoroughly mixed. Push any lumps of material below the surface of the materi&l. CAUTION: Goggles must be worn during this operation, inas much as premature ignition of the charge may take place, especially when the humidity is high. It is imperative to DSW 257294 STLCOPCB4061413 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 53 Test Methods 10,056-54 General Method, Total Chlorine In Organics^, - Parr Sodium Peroxide Bomb Method, Method No. 10,056. contd. CAUTION: contd. ' hold the bomb away from the operator and not to hold the head directly above the cup in order to see into it. 5. Wipe the stirring rod thoroughly with a small piece (1/2" x 1") of ashless filter paper. Drop the paper into the bomb and press lightly into the fusion mixture. 6. Cap the bomb. Put it into the jacket and tighten with wrenches provided. 7. Tap the bomb several times on the bench top to compact the fusion mass. DO NOT MIX BY SHAKING. CAUTION; Prior to lighting the fusion burner, always blow a stream of air around and through the shield to remove any gas which may have accumulated in the area. 8. Ignite the mixture for exactly two minutes within the shield provided for the purpose with the burner set so that the apex of the inner core is just below the bottom of the bomb. 9. Allow the bomb to cool in the air for one minute' . 10. Place the bomb in the water bath and allow it to cool to room temperature (ca. 5 min.). 11. Remove the jacket and rinse the outside cf the bomb with distilled water. 12. Remove the cap from the bomb and place the bomb on its side in a clean 800 ml. beaker. 13. Wash the cap with distilled water, catching the washings in the beaker. 14. Cover the beaker with a watch glass and add enough distilled water rapidly (between the watch glass and the beaker) to cover the bomb. 15. Heat slowly to boiling. SW 257295 STLCOPCB4061414 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 54 Test Methods 10,056-54 General Method, Total Chlorine In Organics, - Parr Sodium Peroxide Bomb Method, Method No. 10,056, contd. CAUTION; Be careful that the solution does not proceed so vigorously that mist is carried out of the beaker. The addition of a few carbo rundum chips will prevent excessive bumping. 16. When the fusion mass has dissolved, remove the bomb with a clean pair of stainless steel tongs, and wash the bomb and tongs thoroughly, .receiving the washings in the beaker. Inspect the bomb carefully for presence of undissolved fusion mass. If any remains, boil further until dissolved completely. 17. Put a stirring rod with a rough end in the beaker to aid in boiling later. Cool to room temperature in the water bath. 18. Neutralize the solution with cone. HNOs to litmus paper (ca. 50 ml.). Add 5 ml. excess. 19. Heat the solution to boiling. 20. Add 50.00 ml. standard 0.1 N AgNOa solution with stirring. 21. Boil gently until the AgCl has coagulated and the supernatant liquid is clear (ca. 15 min.). 22. Cool to room temperature in the water- bath. 25. Add one ml. ferric alum indicator and back titrate with standard 0.1 N NH^CNS to first appearance of faint pink colouration. When the titration is within ca. 0.5 ml. of the end point, stir gently and only within 1 inch of the bottom of the beaker sc that the coagulated AgCl is not carried up into the body of the solution, obscuring the end point. 24. Make a blank determination in duplicate each time new reagents are used. Carry out the blank determination except omit the sample using 0.800 g. of sugar in its place and only 10.00 ml. DSW 257296 STLCOPCB4061415 IX - 55 Test Methods 10,056-54 IX. SPECIFICATIONS AND TEST METHODS, canta. General Method, Total Chlorine in Organics, - Parr Sodium Peroxide Bomb Method. Method No. 10.056-54, coirtd. 24. contd. standard 0.1 N AgNOs (Step 20). If the duplicates do not check within 0.005 milliequivalents, re-run the blank determination. If the blank is greater than 0.025 milliequivalents, use fresh reagents. Calculations s (1) Blank Milliequivalents = mi. 0.1 N AgNOs x N - ml. 0.1 N NHk CNS x N (2) $ Cl = (ml.0.1 N AgNos x N}-(0.1 N NH4CNS x N) - Blk x 0.055457 x 100 Sample Weight The method is precise to + 0.05$. Report the results to the nearest 0.1$. DSW 257297 STLCOPCB4061416 IX. SPECIFICATIONS AND TEST METHODS, eontd. Date: 8-12-5^ Material: General Method By. LG, WJG:SMK Test: Odour IX - 56 Test Methods 10,060-5^ Method No. 10,060-5^ WGK G.M. No. 5 The odour of* Monsanto Products Is quite frequently listed under the specifications for the products. The odour is generally tested in the sample bottle by the sense of smell. The intensity of foreign odour, if any, is estimated by the analyst and a supervisor or- shift leader. If necessary, the opinion of a third person should be asked. As a guide for the estimation of the intensity, the terminology given by the American Public Health Association as applicable to water analysis is used, in part, with some slight modifications. We use only 5 Intensities as indicated below. Term Definition None Nc foreign odour perceptible. Very Paint An odour that would not be detected ordinarily by the average consumer', but that could be detected In the laboratory by an experienced observer. Paint An odour that the consumer might detect if his attention were called to It, but that would not attract attention otherwise. Distinct An odour that would be detected readily and might cause the material (water) to be regarded with disfavor. Strong An odour of such intensity that the material (water) would be absolutely unfit to use (drink). A term used only in extreme cases. The Interpretation of these terms must necessarily be left to the indi vidual analyst; however, it has been found that fair agreement may be reached. In all cases, any detectable foreign odour should be characterized as to some familiar type of odour. DSW 257298 STLCOPCB4061417 IX, SPECIFICATIONS AND TEST METHODS, contd. IX - 57 ' Test Methods 10,084-55 Dates 2-11-55 Bys HOH,NPAsSMK Materials Aroelors, Pyranols Method No,10,084-55 Inerteens, and Tri- WGK Dept, No, 246 Tetrachlorobenaene Blend Tests Appearance, Colour and Condition (Turbidity and Residue) I, APPEARANCE (Crude or distilled liquid or solid material) s 1, Examine the material in the sample bottle and describe its appearance. Report as colourless, light yellow, yellow, tan, light Drown, brown or- black mobile liquid, viscous liquid, sticky solid mass, brittle resinous mass, or otherwise if appropriate. II. COLOR (Distilled liquid material)s a. If the colour of the sample is APHA 250 cr less proceed as followss 1. Pill a 50-ml. tail-form Nessler tube to the mark, NOTEs If the material is of high viscosity, warm up the material carefully until it flows readily. 2, Determine the colour of the sample in terms of APHA units by comparing with the APHA standards in similar tubes. Follow General Method No. 2 (Method No. 10,007). 5. Report the colour to the nearest 5 units. b. If the colour of the product is APHA 200 to 500, proceed as follows: 1. Pour a 50-ml sample into a 250-ml. Erlenmeyer flask and compare with the APHA standards in similar flasks. c. If the colour of the material is greater than. APHA 500, use the following procedure t DSW 257299 STLCOPCB4061418 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 58 Test- Methods 10,084-53 Test on Appearance, Colour and Conditions of Aroelors, Pyranols, Inerteens, and Tri-Tetrachlorobenzene Blend, Method No. 10,084-54,contd. e. contd. 1. Fill 1-7/16" x 5" NPA tube half full of sample. 2. Place the tube in the ASTM Union Colorimeter and turn on the light at the back of the instrument. 3. Determine colour of the sample according to General Method No. 11 (Method No. 11,732) by matching the sample and standard coloured glasses through the observation hole. 4. Match the sample to the nearest half increment of colour. The method is precise to + 1/2 colour increment on all three sets of standards. Report the result to the nearest 1/2 NPA unit. . III. CONDITION (Turbidity and residue); 1. Observe the sample in the sample bottle. Report the condition (both turbidity and residue) as clear, very slight, slight, moderate, or considerable. . 2. Indicate the presence (if any) and describe the character of any foreign matter present, e.g., black specks, white lint, rust, etc. DSW 257300 STLCOPCB4061419 .v IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 59 Test Methods 10,085-53 Dates 2-26-53 Bys AEB,NPA;SMK Material: Aroclors (Solid) and Montars Test: Softening Point Method No. 10,085-53 WGK Dept. No. 246 Introduction: The softening point of solid Aroclors or Montars (Monsanto Pitch) is determined according to the "Ring-and Ball method (ASTM Desig nation: D36 ~ 26, reapprcved in 1949) for Softening Point of Bituminous Materials" as described in 1949 Book of ASTM Standard, Part 5, p. lOfcl. The apparatus is essentially the same as that illustrated in the ASTM procedure with the exception tnat two rings and bails are in our assembly instead of one. Procedure s1 1. To prepare the sample melt the material under test- and stir it thoroughly. CAUTIONs While stirring the material, avoid overheating or incorporating air bubbles in the mass. 2. Place a ring on a square of tinned sheet metal and pour molten material into the ring so as to leave an excess on cooling. 3. After the sample has cooled, cut off the excess material and trim the edges of the ring with a heated knife,, 4. Prepare another ring in the same Tanner (Step 1 to 3) using a Standard Aroclor which has been provided for this purpose. NOTE t For Montars prepare another ring of the material under test. There is no standard Montar. 5. Fill a 600 ml. beaker to a depth of 3.25 inches with freshly boiled distilled water-. DSW 257301 STLCOPCB4061420 IX. SPECIFICATION AND TEST METHODS, ccntd. IX - 60 Test Methods 10,085-5? Test for Softening Point- of Aroclc-rs (Solid) and Montars, Method No. 10,085-5?, contd. 6. Place the rings in the support and suspend them 1 inch above the bottom of the beaker. ' 7. Insert a -2 to 80C. r-ange, ASTM Softening Point thermometer into a support and adjust it sc that the bottom of the mercury bulb is level with the rings and within 1/4 inch of both of them. 8. Place the balls on the bottom of the beaker and maintain the temperature of water at 5 (+ 0.5 )cC. for 15 minutes. 9. Place the balls in the center of the upper surface cf each ring, thus completing the assembly. NOTE; Use a suitable forceps for- this operation. 10. Apply heat in such a manner that the temperature of the water is raised at a rate of 5C. per minute. NOTE; This rate of rise should be uniform within 0.5aC. after first ? minutes of heating, otherwise the test shall be rejected. 11. Continue heating until both samples have softened to such a degree that the Aroclor (Montar) touches the bottom of the beaker. Record the temperature at this instant. 12. Correct the temperature reading (Step ii) by applying to it the difference between the observed softening point of the standard Aroclor and the known softening point which is or: the label, thus allowing for the variations in the technique. NOTE; No temperature corrections are made on Montar "Softening Point" determinations. : DSW 257302 STLCOPCB4061421 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 6l Test Methods 10,085-55 Test for Softening Point of Aroclors (Solid) and Montars, Method No. 10,085-55, contd. 15. Report corrected temperature as the "Softening Point" of the Aroclors. NOTE; For Montar report the observed temperature. The method is precise to + 0.5C. Report the results as follows: For Aroclors to the nearest 0.5eC. For Montars to the nearest 1.0C. NOTE; For Aroclors (Montars) with the Softening Point above 80C. use a sllghly modified technique. The modifications are as follows; a. Use Dow Coming Fluid Instead of water in a bath.. b. Suspend the ring apparatus off the center of the con tainer and place the burner midway between the center and the edge of the beaker away from the rings. Co Use an ASTM High Softening Point Thermometer of a 0 - 360 C. range. DSW 257303 STLCOPCB4061422 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 61 a ' Test Methods 10,086-54 Date: 9-15-54 By: SE,DKL,NPA, WWK: WJG Material: Aroclor, Pyranol, Method No. 10,086-54 Inerteen, Tri-Tetra Chlorobenzene Test: Viscosity WGK Dept. 246 1. Determine the viscosity according to General Method No, 25 (Method No. 11,455) Part B - Kinematic Viscosity. For the products listed below use the following temperatures and series number of Ostwald Viscosimeter tubes: Tube Series Product Temperature Number 1242 Aroclor (Distilled) 100F. (37.8#C.) 200 1248 Aroclor 150F. (54.4c.) 200 1254 Aroclor (G.E. 1476)(Distilled) 210F. (98.9C.) 100 1260 Aroclor (G.E. 1482)(Distilled) 210F. (98.9ec.) 200 1262 Aroclor (Distilled) 210F. (98.9C.) 200 1467 and i4861 Pyranol and Inerteen PPO 100F. (57.8C.) 100 1470 Pyranol 100F. (37.8C.) 100 1478 Pyranol (TCB) 100F. (37.8C.) 50 or 1481 Pyranol 100F. (37.8C.) 200 Calculation: V = ct Where V = Viscosity in centistok.es at TF. C = Tube constant (accompar&rbng each tube) at t = efflux time in seconds at TP. TC'F., and Determine V to the nearest 0.05 cent!stokes. Convert to Saybolt Universal Seconds using Chart No. B-7781 Report to the nearest. C.l S.U.S. DSW 257304 STLCOPCB4061423 IX - bib T est Methods 10,578-52 y U C C M T 'Y n 6 AYBOLT U N IV E R S A L S t u iw r: STLCOPCB4061424 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 62 Test Methods 10,087-53 Dates 5-11-53 By : DEL, 'NPA: SMK Material: Distilled Aroclors, Method No. 10,087-55 Pyranols, Inerteens and Trl-Tetrachlorobenzene Blend Test: Acid Number' (G.E.Acidity) WGK Dept. No.255/246 (For the products "as received" and after the "Corrosion Test"). Procedure: 1. Place 100 ml. of benzene, 100 ml. of Methanol (Measure both by a graduate), and 0.5 ml. (by pipette) of Phenol Bed indicator into one of two clean, dry 500-ml. Erlenmeyer flasks. 2. Neutralize carefully with the 0.01 N. KOH (to the first definite pink colour). 5. Pour the mixture back and forth between the two flasks several times. If the solution is still neutral, divide it equally between the two flasks, if not,repeat Steps 2 and 5. 4. Weigh on a beam balance into one of the flasks a 75 (+5.0) g. sample of the material under test. . 5. Titrate with 0.01 N. KOH until the sample matches the blank (second 500-ml. flask). ft NOTEs For Aroclors 1270 and 1271, toluene is used as the solvent and 500 to 400 ml. is required in order to dissolve the sample. Also, the sample shall be reduced to 10 (+ 0.05) grams. Calculation: Acid Number (Acidity of G. E. Specifications) = mg. KOH/gram sample = ml. 0.01 N KOH x O.56 Sample Weight LDSW 257306 STLCOPCB4061425 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 63 Test Methods 10,087-53 Test for Acid Number (G.E.Acidity) on Distilled Aroclors, Fyranols, Inerteens, and Trl-Tetrachlorobenzene Blend,Method 10, 087-53 . contd. Calculation, contd. To convert mg. KOH/gram to mg. NaOH/gram (on request only) mg. NaOH/gram - (mg. KOH/gram) x 0.7-15 The method is precise to + 0.002 for acid numbers below 0.01 and to + 0.01 In the range of 0.1 to 0.01. Report the results to the nearest 0.001 If they are below 0.1, otherwise to the nearest 0.01. Reagents: 1. Benzene - Nitration Grade: This may be secured from reserve samples of benzene which have been analyzed for Depts. 223 and 233. 2. Methanol - Anhydrous. 3. Phenol Red: A saturated solution of phenol sulfonphthalein (Phenol Red) in methanol (approx. 0.1$). 4. A 0.01 N KOH solution in methanol: This solution is prepared by the Service Section (see "Procedure Manual for the Service Section", Part 2, page 6). DSW 257307 STLCOPCB4061426 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 64 Test Methods 10,088-55 Date: 5-11-55 By: AEB, DKL, NPA:SMK Material: Aroclors, Pyranols, Method No. 10,088-55 Inerteens WGK Dept. No. 246 Test: Total Chlorine (Fixed Chlorine) 1. Determine the total chlorine cdhtent of Aroclors, Pyranols, and Inerteens by the Parr Sodium Peroxide Bomb fusion method according to General Method No. 4 (Method No. 10,056) with the following modifications. 2. Use the quantities of sample under test and reagents to be used as listed in the following table: Required Chlorine Content Sample Weight Sugar Required ** Ml.0.1 N AgNOa Expectancy in a Sample (Use analytical balance) (Use analytical balance) (By burette) 0-50# 50 - 45# 45 - 5856 58 - 66% 66 - 76% . 0.5 (+0.0100)g. 0.4 (+0.0100)g; 0.5 (+0.0100)g. 0.25(+0.0100)g. 0.22(+0.0100)g. 0.5(40.01)g. 0.4(+C.01)g. 0.5(40.01)g. 0.6(40.01)g. 0.6(40.01)g. 50.00 ml. 50.00 ml. 50.00 ml. 50.00 ml. 50.00 ml. 5. If the sample is liquid, in addition to the above reagents use 2 (+ 0.05) g. Na2C03 (weigh accurately on a beam balance), to be placed in the bomb before weighing the sample. Calculation: % Total (Fixed) Chlorine (as % Cl) = Rmi. AgNOs x Normality - ml. NELCNS x Normality) - Blank*"}* ._____________ ______________ 0.055457 x 100 Sample Weight * Blank milliequivalents = (ml. AgNOa x Normality)-(ml.NH^CNS x N) The method is precise to + 0.2%. Report the result to the nearest 0. 1*. DSW 257308 STLCOPCB4061427 IX. SPECIFICATIONS AND TEST METHODS, contd IX - 65 ' Test Methods 10,100-5^ Date: 9-5-54 Material: General Method Method No. 10,100-54 by:DKL,NPA:WJG Test: Water - Traces WGK G.M. No. 7 Introduction:* 1 Water may be determined In most organic and many inorganic compounds by means of a titration with Karl Fischer (K. F.) Reagent, using either the "Dead Stop" or visual poin. A._ _^DEAD STOP^ Method 1. Place 100 to 500 ml. of dry methanol in the titration flask (see note at the end of method). IMPORTANT: The stopper, which closes the charging opening of the titration flask, must be firmly in place before any attempt is made to proceed with the teat. This applies, of course, to both the "blank" and the sanfple. 2. Start the stirring motor and adjust its speed so that effective agitation is achieved without splashing. 5. Snap the toggle switch on the front of the electron-ray indicator panel to the "ON" position and allow the instru ment to warm up for 5-4 minutes. 4. Turn the "SOLVENT SELECTOR SWITCH" knob to the position corresponding to the type of solvent (or mixture) used as a solubilizing medium. NOTE: The switch positions are: "NONE" (when no other sol vent but methanol is used); BENZENE (for benzene-methanol mixtures); TOLUENE (for methanol-toluene mixtures); and ACETIC ACID (for methanol-acetic acid mixtures). 5. Slowly add the K, F. reagent to the titration flask. Observe that the shadows on the indicator tube open momentarily and then close, the length of the "open" time increasing as more DSW 257309 STLCOPCB4061428 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 66 Test Methods 10,100-54 General Method, Water - Traces, Method No. 10,100-54, contd. 5. contd. ' K. F. reagent is added. The solvent is "blanked" when the tube shadows remain fully open (ca. 100c each) for 50 seconds. Refill the burette with the K. F. reagent. 6. Weigh accurately (to three significant figures), by difference, a sample containing 0.05 to 0.06 grams of water, but not more than ca. 200 grams. Transfer quickly to the titration flask. NOTE; Use a powder funnel if the sample is a powdered solid. 7. Allow the material in the flask to be agitated until all the sample is in solution. 8. Titrate the solution with K. F. reagent to the end point des cribed in Step 5. Record the volume of K. F. reagent used. Calculation: % H20 = ml, K.F. Reagent x HgO factor x 100 Sample Weight The method is precise to + 5$ of the water present. Report the result to the nearest 5 in the third significant figure. B. VISUAL METHOD 1. Place 100 - 500 ml. of dry methanol (see note) in a dry 500 ml. g.g.s. Erlenmeyer flask. 2. Titrate the solvent with K. F. reagent to the visual end point, i. e. the first change from the yellow to reddish orange that persists for 50 seconds. Refill the burette. DSW 257310 STLCOPCB4061429 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 67 Test Methods 10,100-54 General Method, Water - Traces, Method No. 10,100-54, contd. B. VISUAL METHOD, contd. 5. Weigh accurately (to three significant figures), by differ ence, a sample containing 0.05 - 0.06 grams HgO into the flask. 4. Stopper and shake until the sample is in solution. 5. Titrate the solution with K. P. reagent to the end point described in Step.2. Record the volume of K. F. reagent Used. CALCULATION: # HgO = ml. K. P. Reagent x HgO factor x 100 Sample Weight The method is precise to + 5$ of the water present. Report to the nearest 5 in the third significant figure. NOTE: Dry benzene or other suitable dry solvents may be used together with methanol in order to render some samples soluble. Dry glacial acetic acid must be added in excess when amines are present in the sample to prevent interference in the water determination. References: Mitchell, J. and Smith, D. M. Chemical Analysis, Vol. 5> Aquametry, Interscience Publishers Inc., N. Y. (1948). Prederickson1s Report to Hehner, May 25, 1950. DSW 257311 STLCOPCB4061430 k ' IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 68 Test Methods 10,105-55 Date: 5-25-55 Material: Trlchlorobenzene Method No. 10,105-55 By: AEB,NPA:SMK Test: Appearance, Colour and WGK Dept. No. 235 Turbidity Trlchlorobenzene (TCB) Is usually a clear, colourless to light yellow liquid. Appearance: 1. Examine the sample and describe its appearance noting any unusual characteristics. Report as a clear, colourless liquid, or otherwise, if appropriate. 2. Observe the sample for residue (visible foreign bodies), such as rust, dark specks, lint, etc. Report as none, very slight, slight, moderate, or considerable. Describe appearance of impurities briefly. Colour: 1. Determine the colour of this product in terms of APHA units by comparing 50 ml. of the sample to the APHA Standards. Follow General Method No. 2 (Method No. 10,007). Report the colour to the nearest 5 units. Turbidity:1 1. For information of the manufacturing supervision, determine the turbidity of TCB. Apply General Method No. 15, (Method No. 11,788). Report the result to the nearest General Turbidity Standard Number. DSW 257312 STLCOPCB4061431 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 5-26-55 Material! Trichlorobenzene By: CCS, NPA: SMK Test: Specific Gravity 15.5/15.5C. IX - 69 Test Methods 10,106-55 Method No. 10,106-55 WGK Dept. No. 255 1. Determine the specific gravity of Trichlorobenzene (TCB) by means of the hydrometer. Apply General Method No. 15 (Method No. 10,497), with the following modifications: 2. Use a 1.400 - 1.600 range hydrometer. 5. Use a 0 - 110C. range paper scale thermometer. 4. Read the hydrometer scale at a point .directly in line with the lower meniscus. 5. Use the temperature correction of 0.0011 perC. 6. Add this correction to any reading obtained above 15.5C. and subtract it from readings obtained below 15.5C. 7. Then make the hydrometer correction, if one is necessary. The method is precise to 0.001 unit. Report the Specific Gravity 15.5/15.5C. to the nearest 0.001 unit. DSW 257313 STLCOPCB4061432 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 2-15-52 By: DKL:SMK Material: Trichlorobenzene (Pyranol 1478) Test: Distilling Range1 IX - 70 Test Methods 10,108-52 Method No.10,108-52 WGK Dept. No.255-246 Determine the distilling range of the sample according to General Method No. 1 (Method No. 10,006-50) using a 190 - 250C. thermometer and a translte board with an opening 2" in diameter. Report the following for 1,2,4 TCB: First Drop 1 - 96 ml. 100$ Dry Point (95$ range) (First Drop to Dry Point) The method is precise to + 0.1C., however, if appreciable quantities of low or high boiling material are present, the precision is of the order of + 0.5C. Report the results to the nearest 0.1C. Report the following for Technical TCB or Pyranol 1478: First Drop 5$ 50$ 90$ Dry Point The method is precise to + 0.1C., however, if appreciable quantities of low or high boiling material are present, the precision is of the order of + 0.5C. Report the results to the nearest 0.1C. DSW 257314 STLCOPCB4061433 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 71 Test Methods 10,114-55 Date: 2-11-55 By: RWS,RAC,SE NPArSMK Material: Aroclors, Pyranols Method No. 10,114-55 Inerteen, and Tri-Tetra- chlorobenzne Blends Test: Specific Gravity (by WKG Dept. No. 246 Hydrometer)1 1. Determine the specific gravity of Aroclors, Pyranols, Inerteen.;:, and Tri-Tetrachlorobenzene Blend according to procedure des cribed in General Method No. 15 (Method No. 10,497) with the following modifications: NOTE: The temperaturesat which the specific gravities of the named products are taken vary with the viscosity of the indi vidual material. 2. Find in the table, attached at the end of this method, the temperature at which the gravity is to be taken for the par ticular product under test and heat the sample to 10C. above that temperature. 5. Pour the hot sample into the steam-jacketed hydrometer jar provided for this test. 4. Immerse the bulb of a hydrometer of a suitable range in the liquid and stir well with a paper scale thermometer. 5. Adjust the temperature to the desired point by controlling the steam feed to the jacket. Continue stirring until the tempera ture remains constant for half a minute. 6. Note the temperature, quickly withdraw the thermometer and allow the hydrometer to sink into the liquid at the center of the cylinder. 7. Read the hydrometer scale at the point of the lower meniscus and record with the temperature. NOTE: Due to the opaque nature of crude Aroclors, it is necessary to estimate this reading. Usually it is one scale division below the highest visible part of the scale. DSW 257315 STLCOPCB4061434 v -v ' IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 72 Test Methods 10,114-55 Specific Gravity Test (by Hydrometer) for Aroclors, Pyranols, Inerteen, and Trl-tetrachlorobenzene Blend, Method No. 10,114-55, contd. 8. Correct the specific gravity reading from the observed tempera ture to a temperature required by the specification for the product under test. Use the following table Material Sp. Gr. Correction Temperature Range Aroclor 1142-1242 o..00090/C. 50 - 105c. Aroclor 1148-1248 o.00090/c. 50 - 100c. Aroclor 1154-1254 0.00095/c. 55 - 105C. Aroclor 1160-1260 0.00100/C. 75 - 130C. Aroclor 1162-1262 0.00100/C. 85 - 130C. Pyranol 1478-1470 0.00110/C. 11 - 50C. Pyranol 1488-1467 0.00110/C. 11 - 30c. Pyranol l48l 0.00110/C. 11 - 30C. Pyranol 1495 0.00100/C. -- Inerteen P.O.P.O. 0.00110/fc. 11 - 30c. Tri-Tetrachlorobenzene Blend 0.00110/C. 11 - 30 c. Toluene Mixtures 0.00100/c. Taken at 40C. The determination is precise to + 0.001 unit (1/2 scale division). Reportthe Specific Gravity to the nearest 0.001 unit. DSW 257316 STLCOPCB4061435 IX. SPECIFICATIONS AND TEST METHODS, contcL Date: 2-26-53 By: AEB,NPA:SMK Material: Aroclors, Pyranols and Inerteens Test: Loss on Heating at 100C. IX - 73 Test Methods 10,116-53 Method No. 10,n-55 WGK Dept. No. 246 Introduction: This test Is a modification of the test ASTM Designation D6-39T described in 1949 Book of ASTM Standard, part III, p. 1075-1077. Procedure: 1. Weigh accurately on an analytical balance a 40 (+ 0.00005) g. sample of Aroclor (Pyranol, Inerteen) Into a tared (on the same balance) 3 ounce Gill style, flat bottom, seamless ointment box (jar). NOTE: If It is necessary to sample the material hot, upon sampling, cool the box and its contents to room temperature in a desiccator before making the weight determination. 2. Place the box with the sample in an oven maintained at 100C. 3. Keep the sample in the oven at the same temperature for 6 hours. 4. Then cool the sample in a desiccator and reweigh on an analytical balance. Record weight. Calculation: $ Loss on Heating (Loss due to volatilization) = /sample wt. (Step l) - Sample wt. (Step 4)J x 100 Sample voejght (Step l) Report the loss on heating to the nearest 0.01$. DSW 257317 STLCOPCB4061436 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 2-4-54 By: AEB, LJW NPA,WWK:SMK Material: Aroclors, Pyranols, and Inerteens Test: Distilling Range IX - 74 Test Methods 10,117-5^ Method No. 10,117-54 WGKDept. No. 246 Introduction: Distillation tests on Aroclors, Pyranols, and Inerteens are made essentially in accordance with the ASTM procedure D20-50 for the "Distillation of Tar Products Suitable for Road Treatment". Apparatus: Standard ASTM apparatus is used throughout with the following modifi cations : Thermometer: Use a calibrated, 5-inch immersion. Palmer 0-400C. range thermometer. If a full immersion thermometer is used, correction must be made for emergent stem. Condenser: Electrically heated condenser controlled by a variac to an internal temperature of 125 + 10C. The variac settings, necessary for the desired temperature, for all available condensers are attached to the respective condensers. These settings were established using a variac that delivered 100 volts at a setting of 100. When variacs are changed, the voltage out-put at a setting of 100 must be checked with an A. C. voltmeter. If the voltmeter reading is not within 2 volts of 100, make the necessary setting correction for the stated variac settings. The voltage correction is assumed to be linear over the entire range of the variac. Heat Source: Electrical-rheostat control. Material: Point at which condenser heat should be applied: Aroclor 1254 Aroclor 1260. Pyranol 1467 Inerteen PP0_ Pyranol 1470* Pyranol l48l At beginning At beginning When a pot temperature of 250C. is reached When the distillate volume is 40 ml. When a pot temperature of 250C. is reached. DSW 257318 STLCOPCB4061437 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 75 Test Methods 10,117-54 Distilling Range of Aroclors, Pyranols, and Inerteens, Method No. 10,117-54, contd. Procedure:1 1. Weigh and transfer a 100 (+ 0.05) g. sample of the product under test to the distilling flask. Take 100 + 0.5 ml. for Pyranol 1470, Assemble the apparatus as described under ASTM D20-50. NOTE; The electrical condenser will be a permanent set-up so that no connection will be necessary. 2. Insert a 5-inch immersion thermometer into a cork so that the three inch (or 76 mm) line is at the bottom of the cork. Place thermometer and cork in the flask making sure the thermometer is in a vertical position. 5. Turn on the heat source of the flask and the condenser heat when indicated above. 4. Turn the rheostat control,for the heat source to the flask, to ca. 120. Leave in this position until exposed mercury column is within 20C. of the approximate range of distillation. 5. When the distillation starts, reduce the rheostat (on the stillpot) reading until the rate of distillation averages 50-70 drops/ minute. 6. Collect the distillate into a tared flask set on a beam balance. NOTE; Use a graduated cylinder to collect distillate for Pyranol 1470. 7. Record the temperature at the weight percentages indicated in the individual specifications for all Aroclors, Pyranols, and Inerteens with the exception of Pyranol 1470. 8. Collect distillate of Pyranol 1470 "by volume percent" instead of "Percent by weight". For this Pyranol, record the tempera tures as follows; DSW 257319 STLCOPCB4061438 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 76 Test Methods 10,117-54 Distilling Range of Aroclors, Pyranols, and Inerteens, Method No. 10,117-54, contd. 8. contd. First Drop 35# by volume 55# " " 65# " " 90# " " 9. Make the following thermometer corrections (to be added algebraically to observed temperatures): A. Barometric Pressure: C = 0.00012 (76O-P) (273 + T c ) Where P = observed pressure in mm. T = observed temperature in C. B. Emergent Stem Correction: If 3 Inch Immersion thermometer is used there is no emergent stem correction needed. If a full immersion thermometer is used then the positive emergent stem correction is: Ce = L (Te - To ) 0.000154 Where L = ?C. on emergent stem. T - observed temperature in C. Tq= temperature of emergent stem at mid-point in C. NOTE: The use of a full-imftiersion thermometer -is not recommended because of the difficulties involved in obtaining an accurate measure ment of To . Report the temperatures (corrected) to the nearest 1C. DSW 257320 STLCOPCB4061439 ,* -* IX - 77 Test Methods 10,118-55 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 5-6-55 Bys RAC, NPA:SMK Material: Aroclors, Pyranols, Method No. 10,118-55 Inerteens, and Tri-Tetrachloro- benzene Blend WGK Dept. No. 246 Test: Inorganic(G.E.Free)Chlorides (For the products "As received" and after the "Corrosion Test"). 1. Thoroughly rinse two separatory funnels with chloride-free water three or four times. Then take an aliquot from each funnel in a test tube which has.been rinsed with chloride-free water. Test these aliquots for Tyndall beams by adding 5-5 drops of AgNOs and allowing 45 seconds for full beam to evolve. Absolutely no dust or chloride beam should be present. Note: If beam is present rinse all equipment with dilute HNO3 (1:1) and repeat Step 1. 2. When funnel are beam-free, drain out all the water except 50-ml. in one and 25-ml. in the other. Heat the water in both funnels to boiling. NOTE: Hold stopper while heating as steam may cause stopper to fail. 5. Transfer 50-ml. of the sample from the sample bottle at a tempera ture of 95-100C. into the separatory funnel containing the 50-ml. of boiling distilled water. NOTE: As a precautionary measure pour some of the sample from the sample bottle into a waste beaker before adding the 50-ml. to the funnel. 4. Stopper the funnel and shake-vigorously for at least 1 minute, venting frequently through the stopcock. CAUTION5 Care must be exercised at all times to touch neither the lower part of the funnel stem nor the ground part of the stopcock. _ DSW 257321 STLCOPCB4061440 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 78 Test Methods 10,118-55 Test for Inorganic (G.E.Free)Chlorides In Aroclors, Pyranols, Inerteens, and Tri-Tetrachlorobenzene Blend, contd. 5. Allow the layers to separate and drain off the sample Into the second funnel containing the 25 ml. of boiling, distilled, water. It may be necessary to heat the sample when transferring the sample to the second funnel; e. g. Aroclor 1260. NOTE: As previously (in Step 5, Note), drain off a few ml. of the sample into a waste beaker before draining the sample into the second separatory funnel. 6. Repeat Step 4 and allow the layers to separate. Then drain off the sample into a waste beaker. 7. Combine both water extracts in one funnel and shake thoroughly. 8. Take approximately a 10 ml. aliquot of the water extract out through the bottom of the funnel into a 5/4" x 6" test tube. Again first allow a few ml. to drain out before taking the aliquot. NOTE: The test tube used should be rinsed with distilled, chloride-free water several times prior to using. 9 Add an equal (approx.) portion of chloride-free ether. CAUTION: Test ether for chlorides before using in the following way. a. Shake a portion of the ether with chloride-free distilled water. b. Separate water layer and test it for Tyndall beam at the end of 45 seconds. c. If the beam is present, wash ether (as in a and b) several times with chloride-free water until washings dhow no beam after adding 5-5 drops AgN03. DSW 257322 STLCOPCB4061441 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 79 Test Methods 10,118-55 Test for Inorganic (G.E.Free)Chlorldes In Aroclors, Pyranols, Inerteen, : and Tri-Tetrachlorobenzene-Blend, Method No. 10,118-55,contd. 10. Shake the ether-water mixture until the emulsion in the sample disappears and the water layer is completely beam free before adding AgN03. If emulsion is difficult to break, add sample dropwise through the ether and then shake. 11. Add 5-5 drops of 10$ AgNOs solution and test for chloride beam for 45 seconds exactly. If no beam is present at the end of 45 seconds, report a <0.1 ppm. The very faintest of beams is con sidered 0.1 ppm. If beam Is stronger it will be necessary to compare with standards of 0.15, 0.20 up to 1.0 ppm, adding the 5-5 drops of AgN03 and comparing at the end of 45 seconds. The method Is precise to the nearest 0.1 ppm. Report results to the nearest 0.1 ppm. Reagents, Solutions and Accessories: The following standards are prepared by the Service Section of the W.G.K. plant laboratory: Standard Chloride Solution: (See "Procedure Manual for the Service Section Dated 2/27/52, Part 5, page 59). The following standards are made up: A primary standard of 100.0 ppm by weighing 0.1648 g. C.P. NaCl into a chloride-free 1-liter volumetric flask. Dilute to the mark with chloride-free distilled water and mix thoroughly. DSW 257323 STLCOPCB4061442 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 80 ' Test Methods 10,118-53 Test for Inorganic (G.E.Free)Chlorides in Aroclors, Pyranols, Inerteens, and Trl-Tetrachlorobenzene Blend, Method No.10,118-53,contd,, A 10.0 ppm Standard; Dilute 100 ml. of the primary standard to 1-liter and mix well. 0.1 ppm. 0,2 ppm etc. Standards; For every 0.1 ppm of a standard, dilute 10 ml. of the 10.0 ppm Standard to one liter and mix well. NOTE: A 0.1 ppm beam is considered the very faintest beam perceptible to t& eye between 15 to 45 seconds after the addition of the AgNOs solution. If the beam intensity Is not visible at all, or if it is easily visible (too strong) discard the solutions and make new standards. 10$ Silver Nitrate Solution: Weigh on a beam balance 20 ( + 0.05) g. C. P. AgN03 into a chloridefree darlc bottle. Add 20 ml. C. P. HNO3 (chloride free). Dilute to 200 ml. with water. NOTE: All solutions should be freshly prepared every two weeks and stored in glass-stoppered Pyrex bottles. Source of light s Use the 2-battery Penlite flashlight, having a 3-4 mm light and aperture. New batteries (use "Eveready" No. 915) size AA; "Burgess" No. Z, chrome protected; or comparable batteries)must be used fre quently in order to perceive beams properly. SW 257324 STLCOPCB4061443 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 7-25-54 By: AEB, NPA, GWMtWJG Material: Aroclors, Pyranols and Inerteens Test: Electrical Stability (or Aging Test) IX - 81 Test Methods 10,121-54 Method No. 10,121-54 WGK Dept. No. 246 Introduction: Electrical stability is determined by measuring the resistivity of Aroclors, Pyranols, or Inerteens at 100C. before and after exposing the same sample to air at 100C. for 96 hours. PROCEDURE: 1. Allow the Electrode assembly (Method No. 11,607) containing the product under test, from the Initial resistivity determination to remain in the oven at 100C. for 96 hours. NOTE: For this test It is permissible, when convenient, to use either the same oven where the resistivity test has been conducted or any other suitable oven regulated at 100C. However, care should be taken to see that material under test Is not contaminated in any way during the aging process. 2. At the end of the 96 hour period merely attach the leads from the megohm bridge to the electrodes (top lead) (+) on the bridge to inner electrode and other lead to outer electrode) and measure the resistiyity again. Follow the procedure described in Method No. 11,607. Report the resistivity at the end of 96 hours and indicate the change, if any, from the initial resistivity. DSW 257325 STLCOPCB4061444 IX. SPECIFICATIONS AND TEST METHODS, eontd. IX - 82 Test Methods 10,125-53 Date: 5-10-53 By:AEB,NPA:SMK MaterialsAroclors,Pyranols, Iner-- Method No.10,123-53 teens, and Tri-Tetrachloro- benzene Blends WGK Dept. No.246/253 Test: Plash and Fire (Burn)Point Introduction: The flash and fire (burn) point of Aroclors, Pyranols, Inerteens, and Tri-Tetrachlorobenzene Blend shall be determined in the Cleveland Open Cup Tester, following the procedure (ASTM Designation D92-46) described in 1949 Book of ASTM Standards, part 5* p. 716-718. Pcrr our purposes, however, it is not usually necessary to make the complete test (Complete Procedure) as given below (A). On routine sample of Pyranols 1476 and 1482 merely use the abbreviated test (Abbreviated Procedure) for Pire (Burn) Point described under (B) at the end of the method. A. Complete Procedure: 1. Pill the cup to about 5/8"from the top with the sample. 2. Insert a 20-760P. range ASTM Open Plash (l inch immersion) thermometer so that the bulb is 1/4" off the bottom and midway between the center and the back edge. 3. Adjust the flame so that the rise of the sample's temperature will be at the rate of 9 - 11CF. per minute. 4. Adjust the testing flame so that if will be produced through a blow-pipe with an opening 1/32". This flame should be only a bead 3/32" in diameter. CAUTION s The test should be carried out under a hood where there are no drafts. This is very important, as is the rate of tempera ture rise. SW 257326 STLCOPCB4061445 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 85 Test Methods 10,125-55 Flash and Fire (Burn) Point Test for- Aroolors, Pyranols, Inerteens, and Tri-Tetrachlorobenzene Blends, Method No. 10,125-55, contd. A. Complete Procedure, contd. 5. When visible vapors start to rise from the product under the test carry across the surface of material the small bead flame (Step 4). The test flame should never be allowed to get any lower than a height of the top rim of the cup. 6. Carry the flame directly across the product, as in Step 5, every five degrees Fahrenheit until the rising vapors flash back to the material under the test. 7. Record the temperature at this time as the Flash Point. 8. Continue to pass the flame bead across the sample (Step 5) ever five degrees Fahrenheit until the vapors flash down to the material and continue to bum for at least 5 seconds. 9. Record this temperature as the Fire (Burn) Point. NOTE: Always read the temperature before testing as the flash tends to increase the temperature. 10. Convert the reading to centigrade units. Report the Flash and Fire (Burn) Points tc the nearest 1C. B. Abbreviated Procedure: 1. Fill the cup with the sample, to within 5/8" of the top and heat to boiling under a well ventilated hood. 2. As the material comes to a boil pass a test flame (see Step 4,Com plete Procedure), across the top of the cup (Step 5 .-Complete Proce dure). 5. Note if the sample burns for five seconds or more, 4. If the material does not burn for 5 seconds, report the Fire (Bum) Point as^B.P. (above boiling point). 5. If a positive result (the sample burns for 5 seconds or more) was obtained, a test for Flash and Fire (Burn) Point should be run on the same material using the procedure described above under "Complete Procedure". DSW 257327 STLCOPCB4061446 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 84 Test Methods 10,124-55 Date: 2-26-53 By: AEB,NPA:SMK .Material: Aroclors, Pyrands, Method No. 10,124-55 Inerteens, and Tri-Tetrachloro- benzene Blends WGK Dept.No.253/246 Test: Iron (as Fe) Iron is determined in Aroclors, Pyranols, Inerteens, and Tri-Tetrachlorobenzene Blend on occasional samples only. 1. Weigh on a beam balance a 50 (+0.05) g. sample In a casserole. 2. Add 20 ml. C. P. H2S0^ and digest the mixture on the hot plate. 3. Ignite the carbonaceous mass in the muffle at 800C. for 1 hour, burning off the carbon residue. 4. Add to the residue 1-3 ml. HaSO^ and warm to dissolve the iron. 5. Heat up the sample until S0a fumes will appear, to insure com plete solution of Iron in the ignited sample. 6. Cool the sample and dilute it to 100 ml. 7. Transfer an aliquot to a 100-ml. low form Nessler tube. 8. Add 3 drops H20a, 10 ml. N NH^SCN, dilute with distilled water to 100 ml. and mix thoroughly. 9. Compare the intensity of the color with that of a standard con taining the ;same- quantities of HgSO^, Hg02 and NH^SCN. Follow the procedure described in General Method No. 8 (Method No. 10,199). Add easttgh Standard Fe solution to match the color of the sample-. Calculation: % Iron (Fe) (ml. Std. Fe solution x 0.000025) x 100 Weight of Sample (Step 1) x Aliquot 100 Report the results to the nearest 0.0001$ DSW 257328 STLCOPCB4061447 IX. SPECIFICATIONS AND TEST METHODS, cont-d. IX - 84a' Test Methods 10,125-53 Date: 2/26/53 By: AEB, NPA SMK Material: Aroclors, Pyranols Method No. 10,125-55 Inerteens, and Tri- Tetrachlorobenzene Blends Test: Refractive Index WGK Dept. No. 233/246 1. Determine refractive index of Aroclors, Pyranols, Inerteens, and Trl-Tetrachlorobenzene Blend according to General Method No. 28 (Method No. 11,784) with the following modifications: 2. Take refractive index at 25C. 3. Clean the Abbe prisms by flushing with Trichlorobenzene. Then follow with benzene and "Mersol" washes. NOTE: DO NOT TOUCH THE POLISHED SURFACES OF THE ABBE PRISMS! Report Refractive Index to the nearest 0.0001 unit. DSW 257329 STLCOPCB4061448 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 3-9-53 Material: Aroclors, Pyranols Inerteens, Tri-Tetrachlorobenzene Blend By: SE,NPA:SMK Test: Corrosion and Chemical Stability IX - 85 Test Methods 10', 126-53 Method No. 10,126-53 WGK Dept. No. 233/246 Procedure;1 1. Roll a rectangular (2" x 4") piece of aluminum foil so that it will pass through a E 24/40 joint of the corrosion test flask. CAUTION: Be careful that after rolling the specimen does not touch itself at any point. 2. Wash the aluminum foil (Step l) scrupulously with acetone, distilled water, acetone, benzene, and chloride-free ether. 3. Then place the foil on a clean watch-glass and dry in an oven at 110C. for 30 minutes. After cleaning handle the specimen with tongs or forceps only. 4. Weigh accurately on an analytical balance the specimen (Step 3) at room temperature. 5. Drop the weighed aluminum foil into the chloride-free corrosion flask of the "G. E. Corrosion Apparatus". Rinse out flask with sample and rinse end of condenser with sample. . 6. Add 200 ml. of the product under test to the aluminum foil (Step 4 and 5). 7. Set the corrosion flask in the corrosion test apparatus. 8. 'Attach a 12-inch straight-tube air-cooled condenser, the outside of which is painted with aluminum. 9. Cover the exposed part of the flask with aluminum foil. 10. Heat the flask for 6 (+0.1) hours at 210 (+ 5)C. DSW 257330 STLCOPCB4061449 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 86 Test Methods 10,126-55 Test for Corrosion and Chemical Stability on Aroclors, Pyranols, Inerteens, Tri-Tetrachlorobenzene Blends, Method No. 10,126-53, contd. 11. At the end of the heating period, detach condenser from the flask before removing it from the hot plate. 12. Remove the flask from the hot plate and cover all of the flask with aluminum foil (when the flask is not on the hot plate). 13. Without removing the aluminum foil covering of the flask, ana lyze the product (Step 6) remaining in the corrosion apparatus for; a. Appearance, Color, and Condition - Use Method No. 10,084 b. Inorganic (Free) Chlorides - Apply Method No. 10,118 c. Acidity (Acid Number) - Follow Method No. 10,087 14. With a pair of clean, straight nichrome tongs remove the alumi num foil specimen (Step 5)> wash thoroughly, dry and weigh accurately on an analytical balance in the same manner as before (Steps 2, 5, and 4). ' Report the corrosion as loss or gain in weight to the nearest 0.0001 g. and the Chemical Stability as indicated by the analysis of the ' products "After Corrosion Test", in the same way as reported for the original (as received) material. Apparatus t G. E. Corrosion Apparatus consists of the following; a) A Corrosion Flask - It is a 300-ml. Pyrex flask with a ffi g.g. 24/40 joint equipped with a 12-inch straight tube as an air cooled condenser. The air-condenser is painted on the out side with aluminum. b) The Corrosion Apparatus; A transite box 32" long x 8" wide x 5" deep. The top -of the box represents a split transite board with holes cut to fit the flasks. The box is heated by / ** two 500-watt, 15 volt G.E. Strip heaters with off-set terminal 1 at one end (23.5" overall length). The heating length of the heating element is covered by a copper strip 19-1/2 ' long x 4" wide x 1/4" thick. The temperature is controlled by an automatic thermostat with tempera ture setting indicator. DSW 257331 STLCOPCB4061450 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 87 Test Methods 10,127-55 Date: 2-26-55 Material: Aroclors(Crystalline) Method No. 10,127-55 By:EAB,NPA:SMK Test: Hold(Crystallizing)Point WGK Dept. No. 246 Introduction: The cyrstallizing point of the crystalline Aroclors is defined as the highest temperature noted after crystallization begins when the sample is cooled slowly in an insulated container. This is alafr ref-erred to as the "Hold Point". Procedure: 1. Pill a 1" x 8" test tube to within 2 Inches of the top with molten Aroclor and heat sufficiently to insure complete fluidity. 2. Insert an 0-560eC. range, 5-inch immersion, thermometer through a cork and place in position in the center of the tube with the lowest part of the mercury bulb about 1" from the bottom of the test tube. 5. Place the test tube in a suitable Dewar flask (tube form-evacuated). 4. Allow the sample to cool to about 5C. below the expected crystal lizing point without stirring. After the temperature is 5 to 5C. below the expected crystallzing point (material supercooled 5-5C.) start to stir the Aroclor carefully with the thermometer and note the highest temperature rise of the Aroclor. This point is taken as the Hold (Crystallizing)PoiTit.. NOTE: If a material of unknown quality is to be tested and the approximate cyratallizing point is not known, a preliminary test is made in order to determine at what temperature the stirring of material should start. CAUTION: The material must not be supercooled more.than 5 - 5cC. below the expected crystallizing point. Duplicate tests should check within 1C. Report the Crystallizing (Hold) point to the nearest 1C. DSW 257332 STLCOPCB4061451 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 88 Test Methods 10,194-55 Date: 4-5-55 by: WWK:WJG Material; Aroclor-Toluene Mixtures Test: Composition Method No. 10,194-55 WGK Dept. No. 246 Introduction: Certain customers require a mixture of 90$ by weight of Aroclor (1254, 1260, or 1262) with 10# Toluene. A rapid method of determining whether or not the required amount of Toluene is present in the sample of the mixture has been devised and is described below. Procedure:1 1. Examine the sample bottle label to ascertain whether the mix is a 1254, 1260, or 1262 - Toluene mix, and the Lot number of the Aroclor used. 2. From the supervisor's file obtain the specific gravity of the Aroclor used in the mix. 5. Warm the sample to about 50C. by placing it next to a hot plate. 4. Pour the sample into a clean, dry hydrometer jar and determine the specific gravity at 40/15.5C. according to General Method No. 15 (Method No. 10,497). NOTE: The gravity must be taken at exactly 40C. since no gravity-temperature coefficients are available for these mixes. 5. Use a 1.400 - 1.600 hydrometer. 6. The gravity of the mix is the abscissa and the gravity of the Aroclor used in the mix the ordinate on the following graphs on pages IX-89, IX-90, and lX-90a. 7. Using the appropriate chart (TS-A-139 for 1254, A-11144 for 1260, or A-6567 for 1262) determine the point where the ab scissa and ordinate Intersect on the graph. If this point falls within the shaded portion of the chart, the mixture contains 9.5 - 10.5# Toluene and is acceptable. If the point falls outside this area, the sample is rejected. Report only the specific gravity of the mix at 40/15.5*0. and whether or not the material passes the specification limits. Report the gravity to the nearest 0.001 unit. DSW 257333 STLCOPCB4061452 STLCOPCB4061453 ix -so STLCOPCB4061454 DSW 257336 STLCOPCB4061455 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 91 - Test Methods 10,199-54 Date: 8-25-54 Material: General Method Method No. 10,199-54 By: AEB,NPA:WJG Test: Iron (Pe) Traces (Colorimetric) WGK G.M. No. 8 Introduction: Quite frequently iron is present in Monsanto products as an impurity to an extent of from 0.0001 to approximately 0.02$. In these in stances it is advisable to test for iron cplorlmetrically if inter fering ions are absent. This method determines only ferric iron. It is based on the fact that ferric iron and ammonium thiocyanate in an acid solution give a red color, the intensity of which is propertional to the quantity of iron present. Important: Silver, copper, cobalt and mercuric chloride interfere with iron determination. Nitric Acid also gives a color that may be mistaken for iron. Procedure: . Carry out preparation of the sample in a clean 100 ml. low-form Nessler tube which has previously been rinsed with C.P. HC1. If the material to be tested is a solid:* 1 1. Weigh accurately on an analytical balance a 1 to 10 grams (more for extremely low Pe content). 2. Dissolve the sample in dilute HgSO^. 5. Oxidize the iron by adding 5-4 drops of 5$ EaOs solution. If the material to be tested is a liquid: 1. Acidify the sample with C.P. HaSO^ or C. P. HC1. 2. Oxidize the iron by adding 5-4 drops of 5$ H2O2 solution. The procedure is continued for solid and liquid material in the following way: -- DSW 257337 STLCOPCB4061456 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 92 Test Methods 10,199 General Method, Iron (Fe) Traces (Colorimetric), Method No. 10,199-5^> contd. A. Add to the prepared sample (Step .5 - solid material: Step 2 liquid product) 10 ml. N NK^SCN solution and make up the 100-ml. mark. B. Prepare "blank" in a second Nessler tube of the same type. Use the same quantities of acid and reagents as used in the sample. C. Add to the "blank" standard Fe solution until the tints of the two tubes match. Record the number ml. of Standard Fe solution re quired to make the match. Calculations; # Iron (as Fe) = ml.Std.Fe Sol'n.x 0.000025 x 100 Weight of Sample The test will easily detect 0.00001# Fe. Important: In the event that a sample contains sufficient iron to require a titration of more than 10 ml. Standard Iron (Fe) solution, the prepared sample should be diluted to a larger volume (500 or 1000 ml.) and the iron (Fe) should be determined on a suitable aliquot. Reagents Used: N NH^SCN Solution: Dissolve 76.1 g. NH^SCN in distilled water and dilute to one liter. 5# HgOg Solution: - U.S.P. Iron Stock Solution: Add to 0.2500 gm. pure iron wire* 10 ml. C. P. HC1, 25 ml. distilled water, and 2 drops Bromine water. Cover and place on steam bath to effect solution. When iron is completely dis solved, dilute to one liter. This solution contains 0.00025 g.Fe/ml. Standard Iron (Fe) Solution; Pipet 100 ml. of Iron Stock Solution into a liter volumetric flask and dilute to the mark with distilled water. Mix well. This solution contains 0.000025 g. Fe/ml. * Clean wire with emery cloth to remove any oxide and wipe clean before weighing. DSW 257338 STLCOPCB4061457 _- IX. SPECIFICATIONS AND TEST METHODS, contd. Date; 7-25-52 Material; Biphenyl (Diphenyl) By; AEB,NPA:SMK Test: Appearance and Colour IX - 95 Test Methods 10,252-52 Method No. 10,252-52 WGK Dept. No. 246* 1 Biphenyl (Diphenyl: Xenene) is a light yellow crystalline solid. The melt of this material is a straw coloured liquid. It should be clear and free of residue. NOTE: Biphenyl is not manufactured at WGK Plant'*but it is purchased from Anniston or outside suppliers for use in production of various biphenyl derivatives. 1. Examine the sample and describe its appearance and colour noting any 'unusual characteristics. Report as light yellow crystalline solid, or otherwise if appropriate. 2. Examine the sample in molten and solid state for residue (visible foreign bodies) such as rust, foreign particles, etc. Report observations as none, very slight, slight, moderate, or considerable. Describe appearance of impurities briefly. NOTE: Any off colour dirty gray or deep brown material or material which contains more than a slight amount of residue in the melt is to be rejected. '. DSW 257339 STLCOPCB4061458 ._ / IX - 94 Test Methods 10,298-52 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 7-25-52 Material: Biphenyl (Diphenyl) Method No. 10,298-52 By: AEB, NPA SMK1 Test: Crystallizing Point `WGK Dept. No. 246 1. Melt completely the sample. Avoid overheating. 2. Pill a 1" x 8" test tube to within one inch of the top with the molten material. 5. Place the test tube in a Dewar vacuum jacketed tube. 4. Insert a 55 - 90C. range, 5" immersion thermometer and a plungertype metal stirrer. 5. Cool the material with constant'stirring to crystallization. After slight supercooling of the molten sample, the temperature will rise sharply and remain at equilibrium for a few minutes. 6. Record the highest point of the temperature rise as the crystal lizing point of the material. The method is precise to + 0.1C. Report the results to the nearest 0.1C. The crystallizing point of this material is approximately 68 - 69 C.' DSW 257340 STLCOPCB4061459 IX ~ 95 Test Methods 10,299-52 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 7-24-52 Material: Biphenyl (Diphenyl) Method No. 10,299-52 By: AEB,NPA: SMK Test: Distilling Range: WGK Dept. No. 246 1. Determine distilling range of Biphenyl in the manner described in General Method No. 1 (Method No. 10,006) with the following changes s 2. Measure 100 ml. of the molten sample into an asbestos covered benzene distilling flask. 5. Use a 2500 - 265C. 5" immersion thermometer and set up the distillation apparatus using a transite board having a two inch opening. 4. Use an air cooled condenser. Be sure to warm up. the con denser before the first drop to prevent crystallization of the distillate. Report the following results along with the complete distillation to the nearest 0.1C. First Drop Dry Point 100$ Range (First Drop to Dry Point) The results are precise to + 0.1C. DSW 257341 STLCOPCB4061460 v -' IX - 96 Test Methods 10,497-53 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 11-17-53 Material: General Method Method No. 10,497-55 By:LG,DKL,NPA:SMK Test: Specific Gravity by Hydrometer1 WGK G.M. No. 15 1. Rinse each piece of equipment with a portion of the sample. 2. Fill a hydrometer jar with the well~mixed liquid or molten sample near the specified temperature to a height sufficient to float a specific gravity hydrometer of appropriate range. IMPORTANT: Pouf the sample into the cylinder (jar) without splashing, so as to avoid formation of air bubles. Remove any air bubbles adhering to the surface by touching them with a glass stirring rod. Select a location for the test that is free from air currents. Place the jar on a level surface. 5. Insert a 0 to 110C. range thermometer and a hydrometer of suitable range. 4. Holding the thermometer and hydrometer together in the hand, stir the contents of the cylinder (Jar), being careful to avoid formation of air bubbles. Stir until a uniform tempera ture is reached throughout the liquid. Use a vertical stroke which will prevent thermal stratification. 5. If the Specific Gravity coefficient is known, record this temperature (Step 4) and withdraw the thermometer. If this coefficient is not known heat or cool the liquid under the test to the specified temperature. In either case, wipe the stem of the hydrometer, allow it to settle back gently into the liquid and to come to rest floating freely away from the walls of the cylinder. 6. Read the Specific Gravity as the point at which the surface of the sample apparently cdts the hydrometer scale. Record the reading after applying the hydrometer correction (if any). DsW 257342 STLCOPCB4061461 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 97 Test Methods 10,497-55 General Method, Specific Gravity by Hydrometer, Method No.10,497-55 contd. IMPORTANT; Make this observation by placing the eye slightly below the level of the liquid and slowly raise the eye until the surface of the sample first seen as a distorted ellipse seems to become a straight line (lower meniscus) cutting the hydrometer scale. The reading should not be taken until the liquid and hydrometer are free from air bubbles and are at rest. 7. If the specific gravity coefficient is not known, record the value obtained in Step 6. If the specific gravity coefficient is known take the numerical difference between the specified and the observed temperature. Calculations: ACTION: These calculations apply only to those hydrometers whose specific gravity scales are numerically higher at the bottom of the scale than at the top of the scale. Specific Gravity temperature correction = (Difference between the specified and the observed temperature) x Specific Gravity Coefficient Apply the specific gravity correction as follows: a. If the observed temperature is above the specified temperature: Sp.Gr. at specified temperature = Sp.Gr. at observed temp.+ Sp. Gr. temp, correction. b. If the observed temperature Is below the specified temperature: Sp.Gr. at specified temperature = Sp.Gr. at observed temperature - Sp.Gr.temperature correction Report the specific gravity at the specified temperature to the nearest 0.001 units. SW 257343 STLCOPCB4061462 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 98 Test Methods 10,497-53 General Method, Specific Gravity by Hydrometer, General Method 10,497-53 contd. The method Is precise to ca. + 0.001 units. ' Material specifications often specify different temperatures at which specific gravity shall be measured. For example: Specific Gravity 15*5/15*5#C. Specific Gravity 25/15*5G. Specific Gravity 60/60F. Specific Gravity 20/4C. The meaning of the expression given in this example can be easily seen from the following definition of specific gravity and of density: A Specific Gravity is the ratio of the weight (in air) of a given volume of the material at a stated temperature to the weight (in air) of an equal volume of gas-free distilled water taken as a standard at a stated temperature. Density: The weight of any substance per unit volume at any definite temperature. . Then in the expression "Specific Gravity 25/15*5C. the upper tempera ture is referred to the material under the test and the lower one to the distilled water of corresponding density. It should be noted that the specific gravities at x/xC. and at x/yC. are inversly proportional to the absolute densities of water at xC. and yC. NOTE: Absolutedensities of water at different temperatures are tabulated in Lang's Handbook of Chemistry; page 1221, 8th Edition, 1952. If it is desirable, therefore, to report the specific gravity at x/yC. instead of x/xC., the following calculation is sufficient: Specific Gravity x/ycC.=(Sp.Gr. x/xC.) x density of HaO at xC. density of HeO at yC. DSW 257344 STLCOPCB4061463 .v -' IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 99 Test Methods 10,510-54 Date; 6-7-54 By; AEB, NPA: WKG Material; Aroclor 1270 Test; Foreign Odour Method No. 10,510-54 W.G.K. Dept. No. 246 1. Place approximately 2 or 5 grams of the material in a large metal spoon. 2. Apply heat to the bottom of the spoon for about 5 seconds with a Bunsen flame. 5- Upon removing the spoon from the flame dense white fumes are given off. The fumes should have the odour of burnt rubber and should be free of sharp, penetrating odour of the lower chlorin ated A*scclors. 4. Material showing sharp odours will be rejected. Report the Foreign Odour according to the General Method No. 5 (Method No. 10,060) definitions of odours (none, very faint, faint, distinct, or strong). DSW 257345 STLCOPCB4061464 v ' IX. SPECIFICATIONS AND TEST METHODS, ccntd. IX - 100 Test Methods 10,511-54 Date: 6-7-54 By: AEB, NPA WJG Material: Aroclors 1270 and 1271 Method No.10,511-54 Test: Colour of 5# Toluene Sol'n. WGK Dept. No. 246 1. Weigh accurately on an analytical balance a 2.5 (+ 0.0100) g. sample of Aroclor. 2. Transfer to a 250-ml. beaker containing 50 ml. of filtered toluene. 5. Place on a hotplate and stir until all the ArGclor has dis solved. Do not overheat the solution. 4. Transfer the hot solution to a warm 50-ml. tall form Nessler tube. 5. Determine colour of the material according to General Method No. 2 (Method No. 10,007). The method is precise to + 5 units. Report the AFHA Colour to the nearest 5 units. DSW 257346 STLCOPCB4061465 -v ' IX, SPECIFICATIONS AND TEST METHODS, contd. IX - 101 Test Methods 10,576-5^ Dates 6-18-54 By: AEB, NPA WJG Material: Arcelor 1271 Method No. 10,576-54 Test: Appealance and Colour WGK Dept. No. 246* 1 Aroclor 1271 (Decachlorodiphenyl) is usually a fine, practically white, fluffy powder. Normally the material is pure white, but on standing in the presence of small amount of moisture if may take on a very pale blue cast. The material is a redistilled product, and the best material is that which is free of jagged crystals when examined under a microscope. 1. Examine the sample and describe its appearance noting any unusual characteristics. Report as fine, white, fluffy powder or otherwise if appropriate. 2. Observe the sample for visible foreign bodies (residue), such as rust, wood, lint, black specks etc. Report observations as none, very slight, slight, moderate, or considerable. Describe appearance of impurities briefly. DSW 257347 STLCOPCB4061466 ' IXo SPECIFICATIONS AND TEST METHODS,, contd. IX - 102 ' Test Methods 10>577-54 Dates 6-1.8-54 By: AEB, NPAs WJG Materials Aroclor 1271 Tests ^Moisture (Haft) Method No. 10,577-54 WGK Dept. No. 246 1. Tare accurately on an analytical balance a wide mouth drying bcttle. Record tare. 2. Weigh accurately on the same balance a 10(+ 0.0005') g. sample into the tared bottle. Record weight of the sample. 5. Place the bottle in an oven at 120C. for 24 hours. 4. Cool the sample in a desiccator. 5. Reweigh the bottle. Record loss in weight of the sample. Cal culate percent moisture. Calculation s $ Moisture (HgO) = Loss in weight (Step 5) x 100 wt. of Sample (Step 2) The method is precise to + 0.01$ Report the resui+ the nearest. 0.01$. DSW 257348 STLCOPCB4061467 ' IX. SPECIFICATIONS AND TEST METHODS, ccntd. IX - 105 Test Methods 10,578-52 Date: 5-26-52 Material: Aroclcr 1271 Method No. 10,578-52 By: RK,WJG:SMK Test: Melting Point WGK Dept. No. 246 1. Fill a 400 ml. tail-form beaker with Dow Corning Fluid. 2. Fill one capillary melting point tube to a height of 5/4l! with sample and another with the standard Aroelor 1271. Attach both capillary tubes to a 500-555C. immersion thermometer with two short lengths of thin wire, adjusting the lower end of the tubes level with the mercury bulb. 5. Immerse the assembly in the bath and clamp the thermometer stem in position 5/4" from the side of the beaker. (A desk lamp placed near the bath will facilitate observations). Adjust the initial bath temperature to 250-60C. 4. After the apparatus is in position, neat at such a rate that the bath temperature will increase 0.5 + O.iVirdn. The rate of rise in temperature is important and strict observance of the above limits is necessary. 5. Record the temperature at which the first meniscus appears and the temperature of complete melting of both the sample tested and the do. Pont standard. The first meniscus is taken as the temperature at which the first liquid meniscus in the tube is observed. The complete melt is taken as the temperature ~'r which all crystals have disappeared. The method is precise to + 0.2C. Report the meJting point (M.P.) (first menis us) and the complete melt. (G.M.) on tot-; "nc standard and sample ested to the nearest 0.10.C. DSW 257349 STLCOPCB4061468 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 105a Test Methods 10,579-41 and 10,580-52 Date: 5-4-41 Material: Arcelor 1271 Method No. 10,579-41 By: AEB,MJW Test: 5$ Toluol Solution Color WGK Dept. No. 246 Weigh 2.50 grams of sample and transfer to a 250 ml. beaker containing 50 ml. of filtered toluol. Place on a hot plate and stir until all the Aroclor has dissolved. New transfer the hot solution to a warm 50 ml.tall form Nessler tube and compare the colour with APHA Stan dards contained in similar tubes, employing the procedure described in General Method 2 (10,007). Report the APHA Colour to the nearest 5 units. The method is accurate to + 5 units. Date: 6-24-52 Material: Aroclor 1271 BysAEB,WJG:SMK Test: Crystal Structure Method No. 10-580-52 WGK Dept. No. 246 1. Spread a small amount of the sample on a glass slide and pla.ee it on the stage of a microscope which magnifies from 75 to 500 diameters. 2. When the sample has been brought into the field and is ir. focus, slowly move the slide from, side to side and observe the kinds of crystals present and the proportion of each. 5, Estimate roughly the percent of jagged crystals. Report the amount of sharp edged crystal the nearest; ?%. Two analysts observ g the Ssie material will usually agree within 10%. DSW 257350 STLCOPCB4061469 IX - 104 Test Methods 10,620-53 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 3-9-53 By:SE,NPA:SMK Material: Aroclors, Pyranols Method No. 10,620-53 Inerteens, Tri-Tetra- chlorbenzene blends WGK Dept.No.233/246 Test: Moisture (H2O Water Content) Introduction: Because of the varying solubility of Aroclors, Pyranols,Inerteens, and Tri-tetrachlorobenzene Blend, different proportions of a mixed solvent are required. However, the analysis itself is the same for all listed products. Procedure: 1. Determine moisture (water content) in Aroclors, Pyranols, Inerteens, and Tri-tetrachlorobenzene Blend using Karl Fischer (K. F.) reagent. Apply the "Dead Stop" method described in General Method No. 7, (Method No. 10,100) with the following modifications: 2. Place the solvents, in the proportions indicated below, into the titration flask: Material Anhydrous Benzene Anhydrous Methanol Pyranol 1478 Pyranol 1488 Pyranol 1467 Pyranol 1470 Pyranol l48l Pyranol 1495 Inerteen P.O.P.O. Tri-Tetrachlorobenzene blend All Aroclors 0 ml. 100 mi. 100 ml. 100 ml. 100 mi. 100 ml. 100 ml. 100 ml. 110 ml. 300 ml. 200 ml. 200 ml. 200 ml. 200 ml. 20 0 ml. 200 ml. 200 ml. 190 ml. Titrate the solvent wit h the K. F. reagent until it is "blanked". DSW 257351 STLCOPCB4061470 IX. SPECIFICATIONS AND TEST METHODS, conid. IX - 105 ,Test Methods 10 620-53 Test for Moisture (HgO Water Content) for Amclors, Fyrs.no!s. Inerteens, Trl-Tetrachlorobenaene Blends, Method No. 10,620-53, ecr.fd 0 NOTE; The solvent Is "blanked" when the tube shadow remains fully open (ea. 100) for 30 seconds. 4. Refill the burette with K. F. reagent to the aero mark. 5 - Weigh on a beam balance a ICO 0.05} g. sample by difference, into the "blanked" solvent and allow the material in the flask to mix well. Titrate the solution, with K. P. reagent to the end-point described in Step 5. Record the volume of K. F. reagent used. Calculation s $ Moisture (Hz0)* - ml K. F. Reagent x llss!J factor x 1C'! . Sample Weight The method is precise to + 5# of the water present. Report the result to the nearest 0.0003$ or equivalent p.p.m, NOTE; 1 ppm is equivalent- to 0.0001$. 4*. If required by a speuificat-i or.-., report P.p.m. equivalent to per-"--nt moisture. Content DSW 257352 STLCOPCB4061471 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 106 Test Methods 10,670-53 Date: 4-13-53 By: DBH,NPA:SMK Material: Pyrancls 1488 and 1495 Test: Trichlorobenzene (TCB) Method No. 10,670-53 WGK Dept. No. 246 Introduction: Arcelor 1260 (G.E. Compound No. 1482) and Trichlorobenzene (TCB) (G. E. Pyranol No. 1478) are blended together to make transformer Pyranols for the General Electric Company. Two blends are made: Pyranol 1488 (60$ Arcelor - 40$ TCB) and Pyranol 1495 (90$ Aroclcr 10$ TCB). Sixteen ounce samples of the Aroclor 1260 and the TCB used for blending in the department are brought to the laboratory for the analysis. Procedure: 1. Tare accurately on an analytical balance two conical ground glass stoppered weighing bottles. 2. Add 10 (+ 0.0005) g of warm (60 - JOcC.) Aroclor 1260 to each bottle. ~ 3. Cool and reweigh on the same balance. 4. Add TCB to each weighing bottle from an eyedropper until the desired composition is obtained. NOTEs The following proportions are used: Pyranol No. TCB Added Sample No . 1 Sample No. 2 1488 39$ 41$ 1495 9$ 11$ 5. Reweigh the material accurately on the same balance. DSW 257353 STLCOPCB4061472 IX - 106a Test Methods 10,670-53 IX. SPECIFICATIONS AND TEST METHODS, contd. Test for Trichlorobenzene (TCB) in Pyranols 1488 and 1.495# Method No. 10,670-53# contd. 6. Put the stoppers in the weighing bottles and place them on a covered steam bath. Swirl the materials occasionally to facilitate thorough mixing. 7. After the blends are thoroughly mixed, determine the refractive index at 25C. with an Abbe Refractometer according to Method No. 10,125. 8. Plot ND25 versus $ TGB on coordinate paper and connect the two points obtained with a straight line. 9. Determine the refractive index at 25C. of the sample under test according to Method No. 10,125. 10. Determine the percent T.C.B. present from the graph (step 8). Report T.C.B. to the nearest 0.1$. DSW 257354 STLCOPCB4061473 ' IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 106b Test Methods 10,723-51 Date: 5/16/51 By: HOH,DKL:SMK Material: General Method Operation of Fisher Test: Electrophotometer Method No. 10,723-51 WGK G.M. No.18 PRECAUTIONS: a. Remember that this is a precision instrument, and that for best results it must be handled with care. Certain adjustments have been made for optimum operation of the instrument. If in doubt as to proper adjustment of functioning of the Instrument consult your supervisor. b. Be certain that the proper filter is in the instrument before depressing the lamp button and that the filter is clean. c. Always adjust the galvanometer needle at the beginning of a series of measurements. d. See that the intensity control is in the proper position. e. Use only absorption cells in the instrument. The matched pairs will be engraved with the same number by the Service Section. Be sure the cells are clean and free from fingerprints. f. In filling the absorption cells, always add sufficient solution to bring the meniscus safely above the path of the light beam when in the operating position. g. Always fill the cells before placing them in the adapter; never fill them while they are in the Instrument. h. Always be sure to have the label of the cells facing front (towards the operator) when placed in the adaptor. i. Always close the compartment when making measurements or setting the initial null. j . In changing the position of the sliding platform, push the platform gently but firmly against the proper stop. Do not slam the platform against the stop. DSW 257355 STLCOPCB4061474 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 106c Test Methods 10,725-51 General Method, Operation of Fisher Electrophotometer, Method No. 10,723-51, contd. ' PRECAUTIONS: contd . k. Do not release the lamp button during the interval required to move the platform, exchanging in the light path the reference cell and the cell containing the unknown material. l. Do not keep the lamp button depressed longer than necessary. 1. Place the proper filter in position. 2. Set the intensity control (lower left switch) to "ADJ. GAL" and turn the "ADJUST ZERO" knob (above the galvanometer) so that the galvanometer needle coincides exactly with the index line. 5. Set the intensity control to that position designated by the letter engraved on the handle of the filter holder. b. Place one of the matched pair of carefully cleaned 25 mm Fisher cylindrical absorption cells containing the reference solution in the rear position in the adapter platform in such a manner that the label faces front (towards the operator) and place the other cell of the pair, containing the unknown solution in the front position in the adapter holder with its label also facing front. . 5. Close the cell compartment door. 6. Pull the platform knob forward until the catch is in firm contact with the front stop in order to bring the rear absorption cell containing the reference solution into the light path. DSW 257356 STLCOPCB4061475 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 107 Test Methods 10,725-51 General Method, Operation of Fisher Electrophotometer, Method No. 10,725-51, contd. 7. Adjust the dial control to zero on Scale A. Depress the lamp button (in the center of the dial control) and after ten seconds adjust the "INITIAL NULL" knob to bring the galvanometer needle back to the index line. 8. Without releasing the lamp button, push the platform knob until the platform is firmly in contact with the rear stop to place the absorption cell' with the unknown solution in the light path. 9. Still holding down the lamp button, bring the galvanometer needle back to the index line by turning the dial control. 10. Record the A-Scale or B-Scale reading as indicated in the specific method. 11. Without releasing the lamp button, recheck the initial null adjustment as before (Steps 6 and 7). If not in adjustment, repeat steps 6 thru 11 until there is no change in null adjustment. 12. Empty the cells, rinse thoroughly, fill with distilled water, and return them to the adapter. /-------------------- / DSW 257357 STLCOPCB4061476 ` IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 107a Test Methods 10,753-53 Date: 5/21/53 Material: Boiler Water Method No. 10,752-55 By: H0H,NPA:SMK Test: Chloride WGK Dept. No. 550 1. Filter, using Whatman No. 42 filter paper, about 125 ml. of the sample. 2. Place 100 ml. of filtered sample into a 250-ml. Erlenmeyer flask. Then add 10 ml. of 5^ H2O2 solution and mix well. 5. Add 5 drops phenolphthalein, then follow with 0.5 N H2S0^ until pink color just disappears. NOTE: If the sample Is acid to phenolphthalein, add 0.5 N NaOH until pink, then 0,5 N H2S0^ dropwise until the color just disappears. 4. Add 1 ml. Chromate indicator (Na2C20i.) and titrate with standard Silver Nitrate solution (0.0005 g. Cl/ml) to the first appearance of a permanent red coloration. Record ml. AgN03 used. 5. Prepare and make a blank determination as follows: a. Place 100 ml. distilled water Into a 250 ml. Erlenmeyer flask, add 10 ml. 5# H202 solution and mix well, b. Add 5 drops phenolphthalein and 0.5 N NaOH until pink. c. Add carefully 0.5 N H2S0^ until the color just disappears. d. Add 1 ml. Chromate indicator and titrate with standard Silver Nitrate solution to the same end-point as for the sample. Record ml. AgN03 used. Calculation: Chloride (as ppm Cl) = ml. AgN03 for sample (Step 4) - ml. AgN03 for blank (Step 5i) x 5 The method is precise to + 5 ppm. Report the chloride to the nearest 1 ppm. DSW 257358 STLCOPCB4061477 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 108 Test Methods 11,147-53 Date: 2-27-55 By: SE,NPA:SMK Material:Aroclors, Pyranols Inerteens, TCB,and Tri-Tetrachloro- benzene Blends Test: Sampling Procedure Method No.11,147-55 WGK Dept. No.255/ ' 246 Samples of the listed products are taken in the following way: A. Batch Samples (taken by men in Dept.) Three l6-oz. wide-mouth, screw cap bottles for each batch. B. Storage Tank (S.T.) Lot, Car and Drum-Lot (D-Lot) are sampled by the Laboratory personnel according to the following: For S.T. Lot, Car, and D-Lot samples use only 5-pt. narrow-mouth (narrow-neck), amber coloured, Bakelite-screw-cap, bottles. Samples to be taken as per table below: Material Reserve Sample Pyranol 1467 S.T. Lot - 5 X 5-pt. Bottle Pyranol 1470 Car D. Lot S.T.Lot Car - 2 X 5-pt. - 2 X 5-pt. - 5 X 5-pt. - 2 X 5-pt. If M 1! 11 D. Lot - 2 X 5-pt. II G.E.Compound No.1476 S.T.Lot - 5 X 5-pt. (Aroclor 1254) ' Car - 2 X 5-pt. D. Lot - 2 X 5-pt. Pyranol No. 1478 (Trichiorobenzene) S.T. Lot - 5 X 5-pt. Car - 5 X 5-pt. G.E. Cc.mpound No . 1482 S.T.Lot - X 5-pt. (Aroclor 1260) Car - 2 X 5-pt.. D. Lot - 2 X 5-pt. Pyranol No. 1488 S.T.Lot - 5 X 5-pt. (60$ Aroclor - 40$TCB Car - 2 X 5-pt. II It H V M M M U M 11 Tri-Tetrachlorobeuffine Blend Car(only)- 5 X 5-pt. II Inert-eens S.T.Loo - 5 X 5-pt. M n\sCr-., I D. Lot -- 2 X 5-pt. - 2 X 5 pt. n ^ Advance samples to be sent on request or Advance Sample i X 5-pt. Bottle l X 5-Pt. ! i X 5-Pt. It l X 5-Pt. l X 5-pt. II II JTL X 5-pt. n l X 5-pt. l X 5-pt. n M DSW 257359 STLCOPCB4061478 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 109 Test Methods 11,147-55 Sampling Procedure for Aroclors, Pyranols, Inerteens, TCB, and TriTetrachlorobenzene Blends, Method No. 11,147-55, contd. General Information: 1. As soon as the amber (brown) 5-pt. bottles (see "Caution" on the last page of the method) are received, the carton is opened, each bottle Is capped, and the bottles are returned to the carton until needed. 2. When ready to sample, remove a bottle from the carton and wipe off with a clean, dry towel (see Note 1 at the end of method). Procedure for Car Sampling:1 1. Attach bottle to the clean stainless steel sampling rod (see Note 2 at the end of method). NOTE: The bottle is attached firmly so that it can not swing, to one end of the rod, with the neck toward the handle of the rod. 2. After the department man has opened the car dome, remove the cap from the bottle and immediately plunge the bottle, neck up, at least 12 to 18 inches beneath the surface of the material in the dome. Allow the bottle to fill completely. 5. Withdraw the bottle and empty the contents into a bucket. NOTE: The bucket content is later thrown away . 4. Repeat the filling of the bottle from the car and emptying into the bucket three times (Step 2 and 5). 5. Plunge the bottle again into the car, fill it. completely with the material, remove from the car, pour out few milliliters of its contents to rinse the inside of the bottle cap, allowing the drip pings to fall into the bufcket. 6. Cap the bottle'with the rinsed cap and remove from the rod, wipe clean and label. SW 257360 STLCOPCB4061479 ` IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 110 Test Methods 11,147-53 Sampling Procedure for Arcclors, Pyranols, Inerteens, TCB, and TriTetrachlorobenzene Blends, Method No. 11,14-7-55, contd. Procedure for Storage Tank (S.T.) Lot Sampling; 1. Use the same procedure as described for car sampling with the following modifications: 2. Substitute by a specially designed sample holder the sampling rod used for car sampling. 3. Ascertain that a sampling line of the storage tank has been drained ana thoroughly flushed with the material to be sampled. Procedure for Drum-Lot (D-Lot) Sampling: 1. Sample directly from drums designated by the department. Take a composite sample of the lot. 2. Use for transfer of the material a syphon with a rubber bulb as an aspirator. 3. Cap the sample bottle with the rinsed cap, clean and label. CAUTION: USE NO SUBSTITUTE BOTTLES for the standard 5-pint, narrowneck, amber sample bottle fitted with the factory metal-lined screw cap. NOTE: 1: In Dr. R. L. Jenkins' memo to Mr. D. L. Eynon, 9/26/47, in which Clegorn's method of sampling is included, "diaper cloth" is used. Mr. J. F. Stickiey has approved the method as here modified. NOTE: 2: In Dr. R. L. Jenkins' memo to Mr. D. L. Eynon, 0/26/47, in which Clegorn's method of sampling is included, "a clean hardwood stick about 1" x 1" x 4'"is used. Mr. J. F. Stickiey has approved the method as here modified. DSW 257361 STLCOPCB4061480 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 111 Test Methods 11,321-54 and 11,323-54 Date: 2-25-54 Mate.ua.': Montars Method No. 11,321-54 By:SE,NPA:SMK Test: Appearance WGK Dept. No. 246 Montar is usually brown to black lumps or chunks. 1. Examine the contents of the sample bottle and describe Its appearance. Report as black chunks or otherwise if appropriate. 2. Observe the sample for visible foreign bodies, such as rust, wood, lint, etc. Report as none, very slight, slight, moderate, or considerable. Describe appearance of impurities briefly. Date: 2-25-54 Material: Montars Method No. 11,323-54 By:SE,NPA:SMK Test: Non-Volatile Residue at 800c. WGK Dept. No. 246 1. Weigh accurately on an analytical balance a 5(+0.0100)g. sample in a large porcelain crucible which previously has been cleaned and heated in the muffle at 800C., cooled in a desiccator'and weighed on an analytical balance. Record weight of the sample and the tare of the crucible. ' 2. Smolder the sample over a burner until volatile matter is no longer given off. 3. Place the crucible in the muffle and heat at SCOcC.for 45 minutes. 4. Cool the sample in a desiccator and reweigh accurately on an ana lytical balance. Record weight of the crucible. Calculation : % Non-Volatile Residue at 800C = Weight of Crucible (Step 4) - Tare (Step 1) x 100 Weight of Sample (Step 1) rterort the suit to tne nearest 0.01$. DSW 257362 STLCOPCB4061481 IX. SPECIFICATIONS AND TEST METHODS, contd. Date; 9-21-54 Material: General Melted By: WMK, LJW, WJG WWK:WJG Test; . Viscosity IX - 1.12 Test Methods 11,453-54 Method No. 11,433-54 WGK G.M. No. 25* 1 Part A: Saybolt Universal Viscosity by Saybolt Viscosimeter. 1. Take a scrupulously clean, dry 60-ml. viscosity receiving flask from the oven and allow it to cool to room temperature while the viscosimeter is being cleaned. (Use only receiving flasks which have been standardized and found to be within + 0.05 ml. of 60.00 ml.) tube 2. Clean the visoosimeter/as follows: A. Insert the cork, which should be clean and in good condition, in place in the bottom of the tube. B. Carefully pour enough benzene into the tube so that the latter is filled and the liquid overflows into the gallery. Do not allow any benzene to spill down into the oil bath, as the vapours will affect later viscosities. CAUTION: While using benzene for cleaning the viscosimeter, be sure all circuits of the instrument are turned off. C. Using a thermometer fitted with a holder to prevent it touching the bottom of the tube, stir the mixture well so that any ad hering material is dissolved. Be sure the entire inner surface of the tube and gallery is wet. Pull the cork to drain the tube. With a clean withdrawal tube draw the excess liquid from the gallery and discharge it directly into a beaker -- not into the viscosity tube. D. Repeat- Steps A tnrough C inclusive. E. Permit the viscosimeter tube to drain and dry. ABSOLUTELY DO NOT INTRODUCE A CLOTH OR KLEENEX INTO THE TUBE OR GALLERY FOR BLOTTING UP RESIDUAL LIQUID. DSW 257363 STLCOPCB4061482 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 113 Test Methods 11,433-5^ General Method, Viscosity,. Method No. 11,433-54, contd. P. Plush ca. 80 ml. of the well*shaken (and heated if needed to insure fluidity) sample to be tested through the appa ratus and follow Step C above. G. Drain this out, and'again flush with a fresh portion of sample to make certain any last drops of previous material have been rinsed out. H. Shine a pen-light up through the orifice while looking down into the tube. The orifice should be free of fibers or any other obstruction. If these are present, they should be removed by flushing with sample only, not by use of wires. If flushing with sample fails, inform the supervisor. ADDITIONAL PRECAUTIONS; A. See that the bath oil, when hot, is not less than 1/4" above the level of the overflow rim of the gallery of the tube. B. The bath oil should be a grade of light-coloured mineral oil which has a viscosity of 40 + 5 Saybolt seconds at 210F. and should be replaced when it displays a definite darkened colour. C. For viscosities to be run at 100P. the bath oil temperature shall not exceed 100.25F (+ 0.05F. for 10 Min.). For vis cosities determined at 130C'F., the bath temperature shall not exceed 130.50CF. (+ 0.05F. for 10 Min.). For viscosities determined at 210F, the bath shall not exceed 212.0F. (+ 0.10F. for 10 Min.) D. Use only thermometers standardized to the nearest 0.01F. against a National Bureau of Standards thermometer. E. Use only the stopwatch provided for timing purposes, which should be accurate to within 0.1 percent when tested over a 60 minute period. Electrical timers must not be used unless the available power source is known to be of sufficiently DSW 257364 STLCOPCB4061483 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 114 Test Methods 11,433-54 General Method, Viscosity, Method No. 11,433-54, contd. E. Contd. accurate frequency. The stopwatch must be left in the holder provided, since variations in its position can cause error. F. Never use the plunger, commonly provided, for cleaning the instrument and never expose the viscdfiimeter to a draft during a determination. 3. Blot the cork dry with a lint-free cloth and insert it in the tube. Pour ca. 150 ml. of sample into a scrupulously clean beaker which has been rinsed with sample, and heat the contents to not over 7F. hotter than the temperature of test. Do not use a sample which has overheated, even if it is then cooled to with in the prescribed range. 4. Pour enough heated sample into the tube that it ceases to over flow into gallery. All samples must be strained through the 100 mesh screen which has been carefully flushed with sample. 5. Stir the sample with the standardized thermometer (with attached holder) until its temperature has remained constant within + 0.02F. of the desired temperature for one full minute (with constant stirring). NOTEt Stirring is a very critical point, especially in the case of more viscous liquids such as Aroclor 1260. Use the exact technique described as follows: Stir the sample with the thermometer, continuously in the same direction, at a measured rate of three revolutions per second. Alternately sweep the thermometer against the walls of the tube for five revolutions and then stir in the center of the tube for three revolutions. Do not deviate from the prescribed rate of stirring or the practice of stirring five revolutions at the walls of the tube, three revolutions at the center, five at the walls, three at the center and so on for the one-minute period specified. DSW 257365 STLCOPCB4061484 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 115 Test Methods 11,435-54 General Method, Viscosity, Method No. 11,433-54, contd. 5. contd. Regulate the temperature of the sample while stirring, by adjusting the oil bath until the desired reading holds constant within + 0.02F. throughout the required interval. Do not stir by moving the- thermo meter up and down unless you desire to cool the sample, and under no circumstances stir in this manner during the one-minute timed inter val . . 6. Remove the surplus sample from the gallery, with the scrupulously clean withdrawal tube which is inserted at one point in the gallery without touching the over-flow rim, and which removes sufficient sample that the level of sample In the gallery is be low the level of sample in the oil tube proper. Do not rotate the withdrawal tube around the gallery. 7. Place the receiving flask in position so that the stream of oil from the outlet tube strikes the neck of the flask. 8. Snap the cork from its position, and at the same instant start the stopwatch. 9. Stop the stopwatch at the same instant that the bottom of the meniscus of the sample reaches the mark in the neck of the receiving flask. 10. Examine the end of the cork to see if it has become moistened with sample. This would denote an incomplete seal and a pre mature seepage of sample though the orifice which would produceerroneous results. The time in seconds, after applying the proper calibration cor rection of the tube is the Saybolt Universal Viscosity. Different operators in different laboratories should agree within 0.5$ on all readings. ' Report the results to the'nearest 0.1 seconds. Reference: ASTM D-88-44 DSW 257366 STLCOPCB4061485 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 116 Test Methods 11,433-54 General Method, Viscosity, Method No. 11,433-54, contd. OPERATION OF THE TAG VISCOSIMETER The viscosimeter is heating when the lamp is off. Do not go away and leave the "quick heat" on. The "Quick heat" should be turned off when the temperature of the bath is within 1 degree of the desired bath temperature. The viscosimeter should be allowed 30 minutes to come to temperature equilibrium before making a test. This will allow the metal parts of the viscosimeter to come to temperature equilibrium with the bath. -Note: Every now and then, trouble will be found in getting the bath to hold the proper temperature. This is usually due to dirty contact points. They are found in a small housing between the motor and rheostat. The points may be cleaned by taking off the housing cover and removing any carbon deposits with tissue paper. If possible, this job should be performed by Service Section personnel. Part B; Kinematic Viscosity by Modified Ostwald Viscosimeter. 1. Clean the viscosimeter tube as follows: A. Connect the large side arm of the viscosimeter, by means of a piece of clean rubber tubing, to a vacuum source. B. Apply gentle suction. C. Place ca. 100 ml. of benzene or TCB in a ipO-ml. beaker, . place the capillary arm of the tube in the beaker, and suck the solvent through the tube. D. Repeat Step C using acetone. E. Dry the tube by sucking a gentle stream of air through it or placing in a steam cabinet. 2. Adjust the constant temperature bath to the desired temperature, holding the temperature within + 0.05F. 3. Place a 1 x 6 inch test tube inside a 500-ml. suction flask. Insert a medium porosity Selas glass crucible into the rubber adapter. Place the adapter in the top of the flask with the DSW 257367 STLCOPCB4061486 IX - 117 Test Methods 11,435-5^ IX. SPECIFICATIONS AND TEST METHODS, contd. General Method, Viscosity, Method No. 11,435-54, contd. 3. contd. glass tube extending Into the test tube. Filter, by suction, enough of the sample to fill the 1x6 inch test tube ca. 3/4 full. Have the sample hot enough to be fluid. 4. Select the proper Ostwald tube series number (see chart below) and fill the tube as follows: A. To the large side arm of the Ostwald tube, connect a piece of clean rubber tubing which is connected to a vacuum source. B. Invert the tube and place the capillary side into the filtered sample contained in-the test tube. C. Using gentle suction draw enough filtered sample to fill both bulbs and into the capillary up to the mark etched on it. D. After loading, the tube is turned right side up, vacuum removed, and the excess sample is wiped off the viscosi meter tube. Modified Ostwald Approximate Viscosity Range Viscosimeter . Centistokes Saybolt Universal Seconds Series 50 Series 100 Series 200 Series 300 Series 400 Series 500 0.8 - 3 3-10 10 - 70 23 - 175 120 - 850 800 -56OO 35 - 65 60 - 325 120 - 800 550 -4000 3600 - 25,000 DSW 257368 STLCOPCB4061487 * IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 118 Test Methods 11,433-54 General Method, Viscosity, Method No. 11,435-54, contd. 5. Supporting the tube in a rubber stopper, immerse the viscosi- . meter in the constant temperature bath to such a level that the top bulb is completely immersed. Adjust the tube to a vertical position. This can be best accomplished by either visual examination or using a small plumb bob consisting of a piece of solder and a thread placed in the large side arm of the Ostwald. The plumb bob should not touch the walls of the tube. 6. Allow the sample and tube to come to temperature equilibrium in the bath. 10 minutes will be the minimum time required for this. . 7. After the sample has attained bath temperature, apply vacuum to the capillary arm and draw the s&mple up to a point ca. 5 mm. above the mark between the bulbs. 8. By means of a stop watch, measure the time required for the meniscus to pass from the upper to the lower mark. This is efflux time, t, in seconds. 9. A check determination can be made by re-drawing the sample back above the upper mark and proceeding as in Step 8. It is not necessary to refill the viscosimeter. 10. Calculate the viscosity of the sample as follows: . V = CT Where V = Viscosity of sample in centistokes at TF, C = Calibration constant for tube at TF, and t = Efflux time in seconds for sample at TF.11 . 11. A calibration constant is determined on the viscosimeter as follows: A. Adjust the constant temperature bath to 100 + 0.05&F. . B. For the standard oil use API or NBS oil. C. Repeat Steps 3 through 9 above. DSW 257369 STLCOPCB4061488 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 119 Test Methods 11,433-54 General Method, Viscosity, Method No. 11,433-54, contd. D. Using the viscosity (V), in centistokes, marked on the standard oil lable, calculate the tube constant (C) as follows: where c = Calibration constant at 100P.for the tube tested. V = Viscosity of the oil in centistokes, and t = Efflux time in seconds. E. Determine the constant in duplicate. Duplicate efflux times should be within 0.2 seconds. P. To determine the calibration constant on a tube at other temperatures use the following equations: Calibration constant at 210F.(98.89C.) = 0.996 x calibration constant at 100F. (37.78C.) Calibration constant at 130F.(54.44C.) = 0.999 x calibration constant at 100F. (37.78C.) Calibration constant at 60F.(15.56C.) = 1.001 x calibration constant at 100F. (37.78C.) 12. To convert from kinematic viscosity in centistokes to Saybolt viscosity in Saybolt Universal Seconds consult either the attached graph B-7781* or ASTM D-446-39. 13. The following equivalents are frequently used in connection with viscosity conversions : Poise Centipoise Stoke Centistoke Centipoise Reyn (l lb. = c.g.s. unit of absolute viscosity = 0.01 poise = c.g.s. unit of kinematic viscosity = 0.01 stoke . = centistokes x. density (at temp, under con sideration) sec. per sq. in.) = 69 x 105 centipoises. Reference: ASTM D-445-46-T and D-446-39. *See page IX - 6lb, above. DSW 257370 STLCOPCB4061489 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 120 Test Methods 11,503-52 Date: 9-23/52 By: LDF, DKL, NPA:SMK Material: Trichlorobenzene Test: Stability \ Method No. 11,503-52 WGK Dept. No. 223-246 1. Rinse a clean, dry, 300-ml. g.g.s wide-mouth Erlenmeyer flask twice with a few ml. of the Trichlorobenzene (TCB) sample. Weigh on a beam balance the flask and add 290 (+ 0.05) g. of the sample. Set the dip-pipe into the flask making sure the dip-pipe is not touching the bottom of the flask. 2. Place the flask fitted with its dip-pipe in position by slipping it through the opening provided in the bath lid section and clamp firmly in place. The absorber flask is rinsed with dis tilled, chloride-free viater, and about 20 ml. of chloride-free water is added, to seal effectively the opening of the side-arm bulb. Place rubber stopper tightly on the absorber flask. Seat absorber male joint into female joint of dip-pipe, remembering that the. ground glass joint formed and the inside of its glass tube must be dry; this is accomplished by the use of a clean tissue of Kleenex. Complete the assembly by connecting the dippipe with the rubber tube from the bubbler. 3. The Dewar bottle space is filled with dry ice and methanol around the condenser trap. Use ca. 3" of methanol, then crushed dry ice to the top. Check the dry-ice trap before each run. If water or ice is present anywhere inside the condenser trap, clean the trap with distilled water and alcohol and place in the oven to dry before using. Always blow the dried taap with air before using. ' 4. Immediately turn on the air by releasing the pinch clamp which is. between the dry ice trap and pressure regulator. CAUTION: Do not connect the sample to air line before dry ice has been added to trap, or the cooling air in the trap will suck the sample from the flask into the air line. If this should ever occur, replace the rubber tubing with new Tech. Prod. Co. amber translucent rubber tubing, 3/16" I.D. 1/16" wall -- do not, attempt to clean out soiled tubing, clean out glass capillary tube with methanol, and blow dry with air, clean and dry the bubblers and put in fresh tricresyl phosphate. DSW 257371 STLCOPCB4061490 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 121 Test Methods 11,503-52 Stability Test for Trichlorobenzene, Method No. 11,503-52, contd. 5. Cover the parts of the assembly (excepting the absorber bulb) that are above the bath top with aluminum foil to exclude light, which has proven detrimental. Make certain there is a water seal in the side arm bulb with a water head rising well into the bulb. This assures complete absorption of chlorides. 6. Turn on the variac operating the main bath-heat source and adjust heat to approximately 210C. with this source alone. The stirring motor for the bath is also turned on and allowed to circulate the fluid during the heating. When the proper bath temperature has been reached, the thermo-regulator-relay-immer sion heater.' system- is''plugged in and the bimetallic thermo regulator is adjusted as follows: Loosen locking screw in the base and rotate the Bakelite head until the pointer indicates the temperature desired on the graduated scale. Relock the head by tightening this locking screw. At the instant the desired temperature is obtained, the red contact screw-governing setting should be turned so that it just touches its contact arm button. Usually only a small part of a turn of the adjuster will be sufficient. NOTE: This thermo-regulator is a very delicate and accurate mechanism which is easily broken if mishandled. In no case should it be removed or tampered with except for the setting instructions mentioned above. This adjustment will normally be made by the Instrument man. 7. The manometer in the air line should show a pressure differential of 24-26 mm. of mercury. Markings for the proper reading have been made on the manometer. The rate of air flow should be re gulated to .a value of 44 ml. air/minute t, means of a rotameter applied to the outlet. This flow rate can be regulated by means of a screw clamp on the tubing before the capillaries. The bleed-off valve can also be used to make small changes. Usually, however, it should not be necessary to change the setting of the regulator. DSW 257372 STLCOPCB4061491 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 122 Test Methods 11,503-52 Stability Test for Trichlorobenzene. Method No. 11,505-52, contd. 8. Clean out the mercurous sulfate electrode by allowing some solution in it to drain around the loosened glass plug. (First read instructions appearing later in this method on use of electrode, care, and sources of trouble). Occasionally (every 2 or 3 days) it is necessary to clean the silver wire electrode by dipping it in dilute nitric acid and sanding with fine sand paper. CAUTION: Do not use emery cloth. Emery cloth contains impurities which will affect the electrode potential. 9. Rinse off electrodes by placing a 100-ml. beaker of distilled water under electrodes and turning on agitator. 10. Before titrating the sample, run a blank on the methanol by putting 20 ml. of distilled water in a 100-ml..beaker and adding 50-75 ml. of the methanol, placing the beaker under the electrodes, turning on the agitator, and reading voltages on the previously balanced potentiometer. The voltage should be 60 millivolts, but it might be higher due to. contamination. If 0.02 ml. or less of 0.005 N AgN03 reduce the potential to 60 mv. or less, and methanol is good enough to use. Discard the beaker contents. NOTE: If the methanol is not satisfactory, obtain a fresh supply from the solvent vault. If this fresh supply is not satisfactory, the methanol will have to be purified by distillation as described at the end of this method. 11. The length of run for each sample is two 8-hour periods. At the end of the first 8-hour period, remove the first absorber without turning off the air, and pour its contents into a 100-ml. beaker which has been cleaned by rinsing with 1:4 HNO3, then distilled water. Rinse into beaker, adding a total of 50-75 ml. of methanol, and titrate to a potential of 60 mv., using 0.005 N. AgN03. 12. The absorber must be rinsed well with distilled water, 20 ml. of water then being added to the flask, and water removed from joints with tissue, as before. The absorber is then placed back oh the dip-pipe for the second -8 hour period. DSW 257373 STLCOPCB4061492 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 123 Test Methods 11,503-52 Stability Test for Trichlorobenzene. Method No. 11,503-52, contd. 13. The contents of the other absorbers are then treated as des cribed in Step 11. 14. At the end of the second 8 hour period, repeat'Step 11 for each absorber. 15. At the end of the stability test, allow flasks to drain free of bath fluid and wipe remainder free with Kleenex, empty the flasks,,rinse with alcohol, flush with distilled water and dry in oven. Do not put foils in flasks. Also clean the dip-pipes with alcohol and distilled water and place in the oven to dry. The Dow Corning fluid level should be maintained 1 inch from the top of the bath. During any run where only one or two flasks and assemblies are in use, the remaining positions are occupied by dummy flasks to maintain the proper bath level. Calculation: Parts per million chlorides = ml. 0.005 N AgN03 x 0.6l In the range 0.1 to 0.5 ppm agreement between duplicate samples must be 100$ of one another. In the range 0.6 to 1.0, the agreement must be 50$ of one another. Report results to the nearest 0.1 ppm. NOTE: If the chlorides on batch samples are greater than 1.0 ppm determinealso Stability by Method No. 10,126 (G.E.) on the sample filtered through Attapulgus earth. Preparation of Solution and Apparatus: 0.005 N AgN03: The silver nitrate solution is made up by adding 50.00 ml. 0.01 N AgNGs from a 50-ml. volumetric flask (painted black), to a 100-ml. volumetric flask (also painted), and diluting to the mark with distilled water. This solution is prepared by the Analytical Section. DSW 257374 STLCOPCB4061493 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 124 Test Methods 11,503-52 Stability Test for Trichlorobenzene, Method No. 11,503-52, contd. Checking the electrode system: Standard chloride solution may be prepared to check the electrode system in case the cell exhibits abnormal behavior. To make 1.00 ppm standard, add 1.49 ml. of 0.55 N HC1 to a 1000-ml. volumetric flask and dilute to the mark. Dilute a 10-ml. aliquot with 50-75 ml. of methanol in a 100-ml. beaker, and titrate with 0.005 N AgN03. Calculate the parts per million chlorides indicated by the titration and compare with the standard value. Fresh standards should be prepared from time to time. Calculations for 1.00 ppm std; ml. AgN03 req'd. = 1.00 ppm = 1.64 ml. 0.6l Use of mercurous sulfate electrode:1 1. Do not place electrode too near the heating bath. Evaporation changes the normality of the KsSO^ solution. 2. Before refilling electrode with potassium sulfate from the volumetric flask, pour a small amount over the lip to avoid contami nation . 3. Remove all air bubbles from electrode arm by closing stop-cock, tightening rubber stopper, and turning upside down, allowing glass plug to slide down arm of electrode, forcing the bubble to the surface. Fill arm with potassium sulfate solution from eyedropper. 4. Always close stopcock before removing rubber stopper. Otherwise the suction created will draw air bubbles into the electric arm. 5. Before using the electrode, loosen glass plug and allow some solution to drain out. Sometimes pota'ssium sulfate crystallizes ' around the plug, preventing good electrical contact. Remove rubber stopper before loosening plug to allow solution to drain freely. 6. Make certain mercury in outer arm is in contact with platinum wire which connects outer arm with inner electrode system. DSW 257375 STLCOPCB4061494 ' IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 125 ' Test Methods 11,505-52 Stability Test for Trlchlorobenzene. Method No. 11,505-52, contd. 7. Always keep stop-cock open whileelectrode isbeing used. 8. Always keep rubberstopper inplace whenmaking arun, and never leave stopper off very long. The atmosphere may contaminate the electrode. 9. Always leave electrode tip in a beaker of distilled water when not in use. NOTE; A second electrode has been prepared in case the first one should be broken. This electrode is kept in a labeled box in the Aroclor Room. It is advisable to drain out the KgSO^ solution and refill the new electrode with fresh solution before using. Preparation of a New Mercurous Sulfate Electrode: Before filling the new electrode, clean thoroughly with dilute nitric acid and rinse with distilled water followed by potassium sulfate solu tion. Reagent grade mercury is added to outer arm with an eyedropper. Make sure the mercury is in contact with platinum wire at the bottom of arm. . Punch a hole in a rubber policeman and fit ever arm of electrode. In sert a piece of clean copper wire about 5 inches long. One lead wire from potentiometer is connected to wire. Other lead wire is connected to silver metal electrode. Add enough reagent grade mercury to inner electrode bulb to cover the platinum wire. Add about 1/4 inch of mercurous sulfate, reagent grade, which has previously been washed with normal potassium sulfatesolution. Fill the electrode with normal potassium sulfate. CAUTION; Mercuric sulfate is a poison to the electrode. Mercuricsalts can be reduced by leaving in prolonged contact with mercury and K^SO^ solution. Methanol Still; Using methanol from the can, fill a large roundbottom flask 5/4 full. Add ca. 5 grams Sodium Hydroxide pellets. DSW 257376 STLCOPCB4061495 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 126 Test Methods 11,503-52 Stability Test for Trlchlorobenzene, Method No. 11,503-52, contd. Methanol Still : contd. Use a distilling column packed with glass helices and a waterjackete.d condenser. All joints are glass-to-glass. Do not use rubber. A bulb-shaped funnel on receiver end of condenser protects methanol from air contamination. The funnel fits into a two-hole cork stopper which fits into a receiver bottle. The glass tube from the other cork stopper hole leads into an empty trap which is connected to a "breather" bottle containing caustic solution. Set heating mantle under flask. Discard first 100 ml. distillate. Run a blank test on the next 50 ml. of methanolj 0.02 ml. or less of 0.005 N AgN03 should be required to reach a potential of 60 mv. Leave a sizeable heel in the distilling flask (300 - 400 ml.) Fill receiver bottle close to neck, as bad air in the bottle will spoil the methanol. Use either a receiver bottle with a screw cap or a glass jointed cap. It has been found necessary to add one drop of very dilute nitric acid (about 0.01 N) to each bottle of methanol to give sharper breaks at the end point of the titration. When bottle is full, cover cap with aluminum foil. When bottle of distilled methanol is put into use, use siphon arrangement on shelf in Aroclor Room. The system consists of two empty traps with "breather" bottle between containing alcoholic caustic to absorb chlorides and T'CB vapors. It is necessary to occasionally refill the alcoholic caustic bottle with fresh solution. If good distilled methanol is not available, undistilled reagentgrade methanol from MalUnckrodt Chemical Company can be used. The methanol must be tested before use, however. DSW 257377 STLCOPCB4061496 IX, SPECIFICATIONS AND TEST METHODS, contd. IX - 127 Test Methods 11,503-52 Stability Test for Trichlorobenzene, Method No. 11,503-52, contd. A. Bath B. Stirring Motor C. Main Heat Variac, 20 amp. cap. D. Dewar flask containing cold trap. E. Thermoregulator F. Bubbler (Air) G. 'Flask, 300 ml. H. Dip Pipe I. Absorber Bulb J. Relay (Aminco # 4-37 OB) K. Reserve D-C Fluid L. Mercury Manometer M. Clamp adjustment for air flow. DSW 257378 STLCOPCB4061497 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 5/24/54 Material: Aroclors: 1142, 1148 By : LDF, NPA, GfWM: WJG Test: Acid Number IX - 128 Test Methods 11,532-54 Method No.11,552-54 WGK Dept. No. 246 This method is used for all dark-coloured Aroclors (mainly crude Aroclors). 1. Weigh accurately on a beam balance a 10(+ 0.05)g. sample by difference Into a clean, dry 400-ml. beaker. Record weight of the sample. 2. Add 100 ml. of Carbon Tetrachloride (CCK) and 100 ml. distilled water, previously just neutralized with 0.01 N KOH, using Phenol Red indicator. 5. Stir-^he solution with a glass rod until all the Aroclor is in solution. Transfer the contents of the beaker to a 250-ml. separatory funnel. Shake and allow the layers to separate. 4. Draw off the lower (Aroclor-CCl^) layer into another 250-ml. separatory funnel, and the water layer (containing free acid) into a clean, dry 400-ml. beaker. 5. Add another 100 ml. of neutralized (as above Step 2) distilled water to the second separatory funnel, shake and collect the water layer in the same beaker as before (Steps 5 and 4). Combine water extracts. 6. ' Titrate the combined water extracts with 0.01 N KOH solution to Phenol Red end-point. Record ml. KOH solution used. CALCULATION: ` Acid Number (mg. KOH/gram of sample)= ml. 0.01 N KOH (Step 6) x O.56 Sample Weight (Step l) Upon request only, convert Acid Number to mg.NaOI^.in the following Way mg. NaOH/gram = mg. KOH/gram x 0.715 Report the results to the nearest 0.001 if they are below 0.1, other wise to the nearest 0.01. DSW 257379 STLCOPCB4061498 IX. SPECIFICATIONS AND TEST VE3K&DS, contd. IX - 129 Test Methods 11,533-55 Date: 2-26-53 Material: Pyranol 1467 and 1470 Method No.11,533-53 By:Se,NPA:SMK Test: Tin Tetraphenyl WGK Dept. No. 246 CAUTION: This method is not applicable to product containing more than 0.0055# water. Determine results on two separately weigheu samples. Blow the funnel with dry air 10 minutes. Procedure:1 1. Weigh on a beam balance by difference a 15 (+0.05) gram sample (approx. 10 ml.) at 25C. from a 10-ml. graduate into a 125-ml. separatory flannel. Bubble dry air through the sample 10 minutes. 2. Bubble dry HC1 through a glass tube of small bore into the sample for 10 minutes. Occasionally rotate the eparatory funnel so that any spatter drops are washed down. NOTE: A tube drawn to an almost capillary tip is desirable for the bubbling. 5. Leave the capillary tip in the funnel and bubble dry air through the sample for 50 min. to sweep out excess HC1. Dry the air over Drierite. Occasionally rotate the separatory funnel so that any spatter drops are washed down. Check for complete removal of HC1 by odour. Do not remove air line from funnel. 4. Pipet 25 ml. of distilled water into the funnel, allow to blow for 1-2 minutes and then withdraw air line. 5. Stopper funnel and shake vigorously for 2-5 minutes. 6. Allow separation of layers and decant bulk of water layer into a clean, dry 100-ml. beaker. 7. Pipet into the funnel another 25-ml. portion of distilled water, shake vigorously as before, allow to separate, discard the Pyranol layer and combine the water extracts. SW 257380 STLCOPCB4061499 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 150 ' Test Methods 11,535-53 Test for Tin Tetraphenyl in Pyranol 1467 and 1470, Method No.11,533-53 contd. 8. Mix the -water extracts and pipet a 20-ml. portion into a 250-ml. Erlenmeyer Flask. 9. Add 50 ml. distilled water and 3-5 drops of alcoholic phenolphthalein indicator solution (l g. indicator to 100 ml. 95$ ethanol) and titrate with 0.01 N NaOH until pink colour remains for 5-10 seconds. 10. Determine a blank titration with 0.01 N NaOH on 70 ml. of dis tilled water. NOTE; The distilled water used for the blank and samples must be taken from the same containers. Calculation; $ Tin Tetraphenyl = (ml. NaOH=Step 9 x Normality)-(ml.NaOH*Step 10 x Norma.T-ity) x 40 x 2,5 Sample Weight(Step 1) x Empirical Factor (last page of method) Report the result to the nearest 0.001$ Determination of Empirical Factor for Tin Tetraphenyl Analysis in Pyranols 1467 and 1470. Introduction: In the process of blending Pyranol 146? (or- Pyranol 1470)* the manu facturing department will send a 1/2-gallon sample of Pyranol 1488 (or Tri-Tetrachlorobenzene Blend-Aroclor 1260 mixture in the case of Pyranol 1470) and a sample of Tin Tetraphenyl to the Laboratory to be used in this determination. NOTE; Inasmuch as the laboratory preparation is in fact a pilot run for the manufacturing department, all materials must be the same as proposed to use in the plant production. DSW 257381 STLCOPCB4061500 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 132 Test Methods 11,555-53 Test for Tin Tetraphenyl In Pyranol 1467 ana 1470., Method No.II,555-55 contd. Procedure; 1. Weigh on a beam balance a clean, dry 16 oz. wide-mouth bottle. 2. Rinse the bottle twice with about 100 ml. of Pyranol i486 (or Tri-Tetra-Aroclor 1260 Mixture for Pyranol 1470) sample. 3. Fill the bottle approximately two-thirds full. 4. Reweigh the bottle with the sample an<J obtain the weight of Pyranol 1488 (or- Tri-Tetra-Arcdor 1260 Mixture) being used. Record the weight. 5. Calculate the necessary amount of Tin Tetraphenyl powder to give a 0.130$ solution of Fyrancl 1467 (or Pyranol 1.470). Tin 1 evraphenyl (grams) - g. of Pyranol 1488(or Tri-Tetra-Aroclor1260 Mixture) x 0.00130 Record calculated weight of Tin Tetraphenyl. 6. Weigh accurately on an analytical balance, using a watch glass, the amount of Tin. Tetraphenyl calculated in Step 5. n ( Brush the powder from, the watch glass into the bottle containing the Pyranol 1488 (or Tri-Tetra-Arcclor 1260 Mixture). 8. Effect complete solution by heating to approx:.60C. wl vh constant agitation. This should take about 1 hour and 13 minutes. 9. Analyze Pyranol 1467 (or- Pyranol 1470) prepared by the above procedure, for Inorganic .Free; Chlorides according to Method No. 10,118. Report the result to Department A-246. '0. Analyze the Pyranol H67 (or Fyrar.ol 1470)'in-the regular manner (Procedure at- the beginning c.f this method) as for- Tin Tetraphenyl content. . Calculation % ~ Ph.pir.tcal factor - SLlaOH-X.Normality___ _____ _ x 100 Sample WWeeiigghhtt used x 0.130 r-e s'.n t r, p. y a irest 0.001. DSW 257382 STLCOPCB4061501 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 152 Test Methods 11, ' 4 and 11, 4 Date: 4-22-54 Material: Tin Tetraphenyl Method No. 11,565-54 By: SMK,NPA:WJG Test: Appearance and Colour WGK Dept. No. 246 Tin Tetraphenyl is usually a white to light cream colored powder. 1. Examipe the sample and describe its appearance noting any unusual characteristics. Report as white powder or otherwise if appropriate. 2. Examine the sample for visible foreign bodies such as rust, . lint, wood, etc. Report as none, very slight, slight, moderate, or considerable. Describe appearance of impurities briefly. 5. Report presence of lumps ar.d moisture also. Date: 4-22-54. By: SMK,NPA WJG Material: Tin Tetraphenyl Test: Melting Point Method No. 11,566-54 WGK Dept. No. 246 1. Place 2 g. of the sample in an agate mortar and grind to a fine powder. 2. Fill a melting point tube, which has been sealed at one end, with the sample to a height of 5/4 inch. 3. Place the melting point tube in the melting point apparatus, fastening the tube to a 135 to 235C. thermometer. 4. Determine melting point according to General Method No. 3 (Method No. 10,052) with the following modifications: 5. Regulate the temperature to give a rise of 0,,25C. per minute. 6. Report Seftenir.g Point, Melting Point, and Complete Melt. 7. Duplicate determinations should check to within + 0.25C. Report the result to the nearest 0.5cC. DSW 257383 STLCOPCB4061502 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 133 Test Methods 11,568-54 Date: 10-6-54 Material: Tin Tetraphenyl Method No. 11,568-54 By: WMK,WJG,NPA PLD,RFS:WJGTest:ChloridesWGK Dept. No. 246 1. Weigh a 20 + 0.1 g. sample Into a 500 ml.g.g.s.Erlenmeyer flask. 2. Add 550 ml. CP monochlorobenzene and heat on the steam bath until the sample dissolves. Occasional swirling of the contents will speed solution. 3. Transfer solution to hot, 80 - 100C., 1-liter separatory funnel. 4. Rinse flask with 100 ml. hot water into funnel. Shake for one minute venting carefully through stopcock. 5. Transfer bottom layer (monochlorobenzene - TTP) to second hot 1-liter separatory funnel. 6. Add 50 ml. hot water and extract as before. 7. Draw off bottom layer and discard. 8. Combine H2O extracts and transfer to 250-ml. beaker. 9. Cool to room temperature, add 3 drops cone. HNO3 and 50 ml.2-B alcohol. 10. Chill in ice bath and titrate potentiometrically using 0.0333 N AgN03 from a 5-ml. microburette. NOTE: Add AgN03 in 0.10 ml. increments until potential approaches 200 millivolts. Then add in increments of 0.05 ml. until potential falls below 125 mv. Resume 0.10 ml. increments until a potential of less than 100 mv. is reached. Record all readings. 11. Make a blank determination following steps 1-10 except omitting sample. 12. Determine the equivalence point from the plot of ml. 0.0333 N AgN03 vs. emf (mv) as follows (see Fig.l): DSW 257384 STLCOPCB4061503 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 134 Test Methods 11,568-54 Chlorides Test for Tin Tetraphenyl, Method No.11,568-54, contd. 12. . contd. a. Draw line AA' through the top plateau. b. Draw line BB' through the bottom plateau. c. Draw line CC1 through the step. a. - Draw lines DD1 and EE1 through points 0 - N and parallel to the horizontal axis. e. Draw lines FF' and GG' through points 0 and N and parallel to the vertical axis. f. Draw line HH' through points M and P,, g. Draw line JJ' through point of intersection L and parallel to the vertical axis. ,0.0333 h. Read the volume of N AgNC>3 from the intersection of line JJ' with the horizontal axis. Calculation: ppm Chlorides = (^ml .AgNOg,(sample) - ml .AgNCb(blankf)x N x 0.035457 x 106* * 106 = 1,000,000 ' SW 257385 STLCOPCB4061504 IX. SPECIFICATIONS AND TEST METHODS, contd Date: 10/2/54 By: CM, LJV, NPA WWK:WJG Material: Aroclor, Pyranols, Inerteen, Tri-tetrachlorobenzene Blend Test: Dielectric Strength IX - 135 Test Methods 11,605-54 Method No. 11,605-54 WGK Dept. No.246/233 Introduction: Consult Method No. 11,752 for the sequence of electrical measurements and the terms used with the determinations.' The dielectric strength of an insulating oil is of importance as a measure of its ability to withstand electric stress without failure. It may also serve to indicate the presence of contaminating agents such as water, dirt, or conducting particles in the oil. One or more of these may be present simultaneously when low dielectric strength values are found by test. However, a high dielectric strength is not a certain indication of the absence of all contaminants. Procedure:1 2 3 4 1. Ascertain that temperature of the material under test is 25 (jp.5) C. Exception: For Aroclor 1260 only the temperature of the material under test will be 50 + 1C. NOTE: Testing at other temperature is likely to give variable results which may be misleading. 2. Shake the sample container so as to thoroughly mix the oil before filling the test cup. NOTE: This operation is even more important with used than new oil as the impurities may settle to the bottom and the test may be misleading. 3. Rinse the oil testing cup three times with small portions of the sample to be test-ed. 4. Immediately after final rinse, fill the cup to a height of not less than 20 mm. (Q.787 in.) above the top of the electrodes. DSW 257386 STLCOPCB4061505 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 136 Test Methods 11,605-54 Test for Dielectric Strength of Aroclor, Pyranols, Inerteen, Trl-tetrachlorobenzene bland. Method No. 11,605-54, contd. 5. Rock the cup a few times in order that any entrapped air may escape. Close cover over oil test cup. 6. Allow to stand 3 minutes. CAUTIONt THIS IS IMPORTANTl 7. Turn main toggle switch on front panel to "ON" (or up) position. Both green and amber pilot lights on the top at either side of the voltmeter will now glow. NOTE? The green signal light Is connected across the 115 volt in-put and denotes that line voltage has been applied to operating control circuit. Amber light Is connected in series with sensitive switch located under high voltage contactors and connected to Its armature. It indicates that high voltage contactor Is in Its rest position and away from contacts energizing auto transformer. 8. Turn voltage control (large knob on front) to extreme counter clockwise position. 9. Depress red botton on fronjr^ This energizes high voltage trans former and circuit breaker/is indicated by amber light going out and the red light direc-tly over voltmeter will light. 10. Watch the voltmeter and, while holding the button "IN", turn the voltage control at such speed that will cause voltage as Indi cated on voltmeter to rise at a rate of 3 K.V. per second. 11. Note and Record the voltmeter reading at breakdown. 12. Repeat the test until two successive breakdowns occur on each of two fillings of the test cup which d.e not differ by mere than 10g. Report the average value of these two readings (Step 12) as the Dielectric Strength. If the limit of the instrument is reached before breakdown, report the Dielectric Strength as> 50 K.V. at 25C. or>50 KV. at 50C. for 1260 Aroclor. DSW 257387 STLCOPCB4061506 IX. SPECIFICATIONS AND TEST METHODS... contd. IX - 157 Test Methods 11,605-54 Test for Dielectric Strength of Aroclor, Pyranols, Inerteen, Trl-tetrachlorobenzene blend, Method No. 11,605-54, contd. Cleaning of the test cup s 1. After the test is completed, drain the cup. 2. Plush the cup with benzene. Use warm benzene after the 1260 test. 5. Then-fill with Aroelor 1248 and let stand until the next analysis. NOTEi An exception, when the samples of oil from the plant are brought in for test, the cup must be thoroughly cleaned with benzene and carbon tetrachloride before and after running the test. The electrodes? The oil testing cup has two electrodes. Both electrodes are movable and have twenty threads to t-he inch with index notches on both the electrodes and the lock nuts. To set the Gap?1 1. Arrange ore of the electrodes and the loc-k nuts with the index marks in line. 2. Move the other electrode until it comes in firm contact with the first electrode and lock it. 5. Now unscrew the electrode with the index marks in line (Step l) two complete turns and lock it. This will leave a. gap of C.l inch between faces of the electrodes. Cleaning of tne electrodes and the test- cup free of carbon coating: The following ASTM method of cleaning, shall be followed when it is. apparent from visual inspection that the electrode discs of the cup are coated with carbon. DSW 257388 STLCOPCB4061507 IX. SPECIFICATIONS AND TEST METHODS, ccntd. IX - 138 Test Methods 11,605-5^ Test for Dielectric Strength of Arcelor, PyranoIs, Inerteen, Tri-tetrachlorobenzene blend, Method No. 11,603-54, contd. 1. Wipe clean with dry calendered tissue paper the electrodes and the test cup. CAUTION; It is important to avoid touching the electrodes with the finger or with portion of the tissue paper which have been in contact with hands. . 2. Rinse the electrodes and cup with dry lead-free gasoline, Stoddard Solvent (or dry, water white Kerosene) until they are entirely clean. Car-e should be taken net, to touch the electrodes or the inside of the cup after cleaning so as to avoid possible contamination. Apparatus; General Information.: The electrical equipment necessary to provide high voltage to permit the determination of dielectric strength of liquid dielectric at commercial power frequencies Is basically quite simple. The equipment was assembled in the W.G.K. Plant Laboratory and con sists of a high voltage transformer of good design and with a currentcapacity of 2.43 KVA and with equipment for control of the voltage and a means of measuring the voltage and to provide safety for the oper; tor. It is enclosed in a steel grey crackle finished cabinet- measuring 42" high, 22" wide 17" deep and set. on truck casters for easy mobility. Protective equipment incorporated in this apparatus prevents the application of high voltage unless all safeguards are complied with. The door on rear of cabinet must be closed.. The cover over the cil must be all the way down and the voltage control must be at 0 position. Failure to comply with these requirements will prevent any action when the red button is depressed. The, test cups Transf..roc-r-s Veltmstsr-s, and Accessories DSW 257389 STLCOPCB4061508 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 159 Test methods 11,605-54 Test for Dielectric Strength of Aroclor, Pyranols, Inerteen, Tri-tetrachlorobenzene Blend, Method No. 11,605-54, contd. The oil testing cup type No. 224809 supplied by General Electric Co. is mounted on the top rear of the cabinet. It is protected by a heavy plastic cover, hinged at the rear for accessability to the receptical. It is equipped with safety contactor so placed that the circuit energizing the high voltage contactor can not be completed unless the protective cover is completely lowered and in place. It is impossible for the operator or anyone else to touch the testing cup when high voltage is applied. The High Voltage Transformer manufactured by the Kelly-Koett Manufacturing Co. is of the closed core, oil immersed, shell type design. Rated at 81,000 volt at 400 millampers. It was recovered from a used X-ray machine, purchased quite inexpensively. An auto transformer from the same X-ray machine is connected so as to limit the output voltage of the high voltage secondary to 50,000 volts. The primary of the auto transfowier is connected to the secondary of a 2f KVA powerstat variable autg transformer supplied by the Superior Electric Company. Power to the powa?stat is controlled by a 4 contact 50 amp. solenoid circuit breaker. The voltmeter mounted on top near front edge is connected across the powerstat secondary and is calibrated to read directly in kilovolts in the range of 0 - 50 K.V. The overload circuit breaker consists of a small relay connected between one side of the high voltage transformer secondary center tap and ground. It is adjusted to break contact on a current drain of about 50 milliampers. The circuit for the coil of the solenoid cir cuit breaker is wired through the contacts of this relay. DSW 257390 STLCOPCB4061509 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 140' Test Methods 11,605-52* Test for Dielectric Strength of Aroclor, Pyranols, Inerteen, Trl-tetrachlorobenzene Blend, Method No. 11,605-54, contd. Safety and Operating Controls: (a) Door interlock switch located on rear door. (b) Oil test cup cover interlock switch. (c) Powerstat switch mounted on rear of unit arranged so that high voltage contactor can not be closed unless powerstat is at zero position. (d) Main power switch on front panel. Powerstat voltage control on front panel. (f) High voltage contactor push button on front panel, (red). (g) Signal lamps mounted on top around voltmeter. Purpose and operation described in method of use. // DSW 257391 STLCOPCB4061510 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 141 Test Methods 11,607-54 Dates 5-24-54 By: CM, LJW, NPA GWM:WJG Material: Aroclors, Pyranols and Inerteens Test: Resistivity Method No.11,607-54 WGK Dept.No.246/235 Introduction: Consult Method No. 11,752 for the sequence of electrical measurements and the terms used in connection with the determinations. The Resistivity of an electrical insulating oil is an index of its insulating properties. High resistivity Indicates high resistance to the passage of electrical current and normally, but not neces sarily, establishes the absence of conducting contaminants. Procedure:1 1. Assemble the test cell. Place the recently cleaned (within the last 8 hours -- see Method No. 11,751, Step &) electrodes in an 800-ml. beaker. 2. Measure the capacitance of the test cell (C ) according to Method No. 11,608 (Dielectric Constant and Power Factor measure ments ). 3. Filljrfthe cell assembly until the liquid level is 3/4 inch above the top of the electrodes. 4. Heat the assembly on the hot plate to 100 (+ 0.5)C, 5. Place the assembly inside of the testing oven. 6. Attach top lead (+) on the megohm bridge to inner electrode. 7. Attach other lead to outer electrode. 8. Throw the three switches at the top of the meghom bridge to "ON" position. ' 9. Allow 10 minutes for assembly to reach temperature equilibrium inside the oven. DSW 257392 STLCOPCB4061511 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 142 Test Methods 11,607-54 Test for Resistivity of Aroclors, Pyranols, and Inerteens, Method No. 11,607-54, contd. 9. contd. DANGER; Make sure control knob Is in "CHECK" position. painful shock will result. Otherwise 10. Bring the galvanometer pointer to zero by turning the "ZERO ADJUST" knob in the direction in which the pointer of the galvanometer should move. ` 11. Turn the control knob to "CHARGE" position for one minute. 12. Turn the control knob to "OPERATE" position and return the galvanometer pointer to zero by adjustment of the "MULTIPLY BY" switch and the megohm dial. 15. Read after one minute. Calculation: Resis-tivlty* - megohm dial reading (Step 12) x "Multiply By" reading(Step 11) x capacitance of cell (Step 2) in uuf. x 11.29 x 0.001 Report the result in units of 109 ohm/cm3 . NOTE; It is important that the product under test, electrodes, and beaker be at uniform temperature for this determination. Temperature variations in different parts of the sample will cause the galvano meter zero to change constantly and give misleading results. CAUTION; In as much as measurements must be made at a potential of 500 volts DC a shock hazard exists in the handling of this apparatus. With the control knob in the tfi*ge and operate position full voltage of the bridge (500 volts) Is applied to the + and low terminals and through the test leads to the electrodes. Do not attempt to handle the electrodes or the test leads unless the control knob is in the "CHECK" position. Possible penalty for failure to observe this pre caution -- Painful Shock. * Values of resitivity are qualified by designation of temperature and voltage. These are for this test, 100C. and 500 volts DC. DSW 257393 STLCOPCB4061512 v - IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 143 Test Methods 11,607-54 Test for Resistivity of Aroclors, Pyranols, and Inerteens, Method No. 11,607-54, contd. Apparatus: General Radio Co. Megohm Bridge Type 544-B. This is a combination of Wheatstone bridge and vacuum tube voltmeter for indicating null. The direct measurement of resistance up to 1,000,000 megohms is made possible by the use of a vacuum tube detector which absorbs negligible amount of power. The voltage applied to the unknown resistor is held approximately constant, regardless of the value of the unknown resistance. This condition is necessary to measure resistance properly. The accuracy of the instrument in the range encountered in the measurement of Aroclor resistivity, 100 to 1000 megohm is + 6%. The instrument is equipped with a 115 volt A.C. power supply which supplies all operating voltages for the bridge indicating circuits and in addition supplies 500 V DC for application to the material under test. The instrument is completely enclosed in a waxed finish shielded oak cabinet measuring 8^" wide, 22^" long and 8" high. Approximate weight ----- 26 pounds. Test Electrodes : Two concentric nickel cylinders with feet, obtained from General Electric Company. The inner electrode has outside diameter of 2.8" and a height of 3.25" with area of 184 sq. cm. The outer electrode has Inside diameter of 3" and height of 3.25" with area of 198 sq. cm. The distance between electrodes is, therefore, 0.1" or 0.254 cm. By theory, electrode constant (K) area/length is 191/0.254 or 752 where average area is 191 sq. cm. Also K = 3SIT x 1@J"L x C (in farads with air as dielectric)= 11.29 x C (in uuf. with air as dielectric). Glass Plate; Pyrex about 3|" diameter with concentric grooves to assist in spacing electrodes. Obtained from General Electric Company. Heating Unit s Assembled in the laboratory and is the same unit described in Dielectric Constant Apparatus (see Method No. 11.608; equipment). DSW 257394 STLCOPCB4061513 IX, SPECIFICATIONS AND TEST METHODS, contd. IX - 144 Test Methods 11,608-54 Date: 5/17/54 Material: Aroclors, Pyranols, Inerteens, and Tri-Tetra- chlorobenzene Blends By: CM,NPA,GWM:WJG Test: Dielectric Constant and Power FactorI. Method No. 11,608-54 WGK Dept. No. 246 I. Adjustment of Controls on Electrical Apparatus A. On Panel No. 1 (Top Panel, Amplifier and Null Detector) a. Turn the 4-way (main power) switch on the upper right hand side to the #3 position to determine the Dielectric Constant at 1000 cycles. Turn this switch to the #2 position for measurements at 60 cycles. bo Allow the equipment to warm up 10 minutes. Co Turn "GAIN CONTROL" to 6. d. Depress "NULL DET." button. e. Depress "INPUT> 0.03V." button B. On Panel No. 2 (Oscilloscope) a. Turn "INTEN." to about the 12 o'clock position. CAUTION: Do not allow a high intensity spot to remain stationary on the screen for any length of time. b. Using "H0R. POSITION" and VERT. POSITION" control center the image on the screen. c. Adjust "FOCUS" for sharp line. d. Turn "FREQ. SELECTOR" to 100 KC. e. Turn "FREQ.VERNIER" to 80. f. Turn "VERTICAL GAIN" to 5. DSW 257395 STLCOPCB4061514 IX - 145 Test Methods 11,608-54 IX. SPECIFICATIONS AND TEST METHODS, contd. 1 Test for Dielectric Constant and Power- Factor- of Aroclors, Pyranols, Inerteens, and Tri-Tetrachlorobenzene Blends, Method No. 11,608-54, contd. g. Turn "VERTICAL INPUT" to "10 VOLT MAX.". h. Turn "HORIZONTAL GAIN" to about 20. I. Turn "SYNCHRONISING" to +20. J. Turn "SYN. to "EXT. SYN." k. 'Turn "GEN." to "SWEEF GEN." C. On Panel No. 5 (Capacitance Bridge) a. Turn "RANGE SELECTOR" switch to "100c" for 60 cycle measurements and to 1 KC" for 1000 cycle measurements. b. Turn "METHOD SWITCH" to direct. c. Turn "DISSIPATION FACTOR" selector switch to "0". D. On Panel No. 4 (Oscillator) a. Disregard this panel for measurements at 60 cycles. b. On 1000 cycle measurements, depress the No. 10 "MULTIPLY BY" button. c. Set "FREQUENCY DIAL" to 100. d. Turn "OUTPUT" dial sc that pointer Is at the end of the arrow. ' e. Depress the "UNBAL. 5000 OHMS" button. When all of the above adjustments are made, the electrical apparatus is ready for measurement of Dielectric Constant and Power Factor. DSW 257396 STLCOPCB4061515 IX. SPECIFICATIONS AND TEST METHODS, cond. IX - 146 Test Methods 11,608-54 Test for Dielectric Constant and Power Factor cf Aroclors, Pyranols, Inert-eens,and Tri-Tetrachlorobenzene Blends, Method No. 11,608-54, contd. II,, Determination of Constants for the Apparatus.1 1. Carefully assemble the cell which has been cleaned and dried within the last 8 hours. Refer to Method No. 11,751 for the procedure to use In cleaning the cells. 2. Place the cell assembly in the Fisher oven which has been ad justed to 25C. 5. Connect the back wire inside the oven to the lead on the inner cylinder of the cell and the front wire to the lead on the outer cylinder of the ceil. 4. Connect the cable from the capacitance bridge to the terminals on top of the oven so that the inner wire of the cable goes to the back terminal and the outside mesh casing of the cable (the ground) goes to the front terminal. 5. Remove the thermometer from the top of the oven before going on with the test. This is important. 6. Make all adjustments on the electrical apparatus as directed in Part I of this method. 7. Balance the bridge by rotating the "CAPACITANCE" and "DISSI PATION FACTOR" dials on Panel No. 5 until the wide vertical band on the osoiilisccpe is adjusted to a minimum width. 8. Recor'd the sum* of the readings on the "CAFACITANCE" dial and vernier and call this value A. . 9. Remove the reaker containing the cell from the oven and fill it with C. P. benzene to a level 0.757 inches (ca. 5/4 inch) above the top of the concentric cylinders of the cell. 10. Adjust the temperature of the benzene to 25C. while stirring ' with a thermometer. DSW 257397 STLCOPCB4061516 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 147 Test Methods 11,608-54 Test for Dielectric Constant and Power Factor of Aroclors, Pyranols, Inerteens, and Tri-Tetrachlorobenzene Blends, Method No. 11,608-54, contd. 11. Replace the cell In the oven (at 25C.) and make the same electrical connections as in Steps 3 and 4. DO NOT interchange connections. 12. Balance the bridge again as in Step 7. 13. Record the sum of the readings on the "CAPACITANCE" dial and vernier and call this value B. 14. Calculate the cell constant by the following equation: Cell Constant, K = B - A, (this is usually around 2.27 - 1.0 70 uuf). 15. Remove the cell from the oven and balance the bridge as in Step 7 with the "CAPACITANCE" and "DISSIPATION FACTOR" dials. 16. Record the sum of the readings on the "CAPACITANCE* dial and vernier and call this value F. (capacitance of connecting cable). 17. - Calculate the Cell Lead Capacitance by the following equation: CELL LEAD CAPACITANCE, G = A - F - K (this is usually around 3 uuf.) WHERE: . A = CAPACITANCE OF ENTIRE SYSTEM IN AIR (SYSTEM CONSTANT) G = CAPACITANCE OF THE CELL LEADS (CELL LEAD CONSTANT) F = CAPACITANCE OF CABLE AND WIRES WHICH CONNECT THE CELL AND CELL LEADS TO THE BRIDGE. (CONNECTOR CONSTANT). K = CAPACITANCE OF THE CELL ALONE (THE CELL CONSTANT). DSW 257398 STLCOPCB4061517 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 148 Test Methods 11,608-54 Test for Dielectric Constant and Power Factor of Aroclors, Pyranols, Inerteens, and Tri-Tetrachlorobenzene Blends, Method No. 11,608-54, contd. Tabulate the System Constant (A), the Cell Lead Constant (G), the Connector Constant (F), and the Cell Constant (K) on a piece of stiff paper and post them near the instrument where they can be easily referred to for comparison and calculations. These constants must be checked at least once every three months and in all cases where the Dielectric Constant and/or Power Factor are out of specification. III. Measurement ofDielectric Constant and Power Factor on Aroclors, Pyranols, Inerteens, and Tri-Tetrachlorobenzene Blends. A. Test Run on Cell to Determine Whether it is Clean and* 1 Properly Aligned. 1. Carefully assemble a cell 'which has been cleaned and dri-ed within the past 8 hours. NOTE; Refer to Method No. 11,751 for procedure to use in cleaning cells. 2. Adjust the oven control to hold at a temperature of 100C. for all materials except Tri-Tetra Blends. If a Tri-Tetra blend is tc be tested, adjust the oven to hold a temperature of 25C. 5. Flace the empty cell assembly in the oven and connect the back wire inside the oven to the lead on the inner cylinder of the cell, and connect the other (front") wire to the lead on the outer cylinder. 4. Connect the cables from the capacitance bridge to the terminals on top of the oven so that the inner wire of the cable goes to the back terminal and the outside metal casing (ground) goes to the front terminal. 5. Allow 15 mimtes for the cell to reach temperature equilibrium inside the oven. SW 257399 STLCOPCB4061518 .` IX. SPECIFICATIONS AND TEST METHODS, contd. IX - i49 Test Methods 11,608-54 Test for Dielectric Constat and Power Factor- of Aroclcrs, Pyranols Inerteens, and Tri-Tetrachlorobsnzene Blends. Method No. 11,608-54,contd. 6. Remove the thermometer- from the top of the oven before taking any measurements on the bridge. This is import ant. 7. Make all the 3djustments on the electrical apparatus as directed in Part 1 of this method. 8. Balance the bridge by rotating the "CAPACITANCE" and "DISSIPATION FACTOR" dials on Panel No. 3 until the wide vertical band on the oscilloscope screen is adjusted to a minimum, width. 9. Record the sum of the readings on the "CAPACITANCE" dial and vernier and. compare this value with the SYSTEM CONSTANT determined in Fart II of this method. IMPORTANT; If the value obtained in Seep 9 does not agree with the System Constant A (Part ll) within 5 uuf, the cell must be re-cleaned, re-dried, re-assembled, and the test .ran for the System Constant must be repeated. NOTE; Although the above test run must be made prior to each analysis, the value obtained in Step 9 is not to be used in cal r.riatiors rut is to be used only as a check on. the cleanliness and alignment of the cell. B. Procedure for Testing Materials. .10 Remove the ceil from the oven and fill the beaker with the- material to he tested to a. level 0.777 inches (ca .3/4 inch) above the cylinders of the cell. Adjust :: teyp-vatune of the sample to IG0C. (use hot plate j f c.ail materials except Tri-Tetra blends. For Tri- Terra blends, adjust the temperature of the sample c o ?=- *0. using an ice-water bath if necessary. NOTE; '.pit con.::in.uou.sly with a thermometer while for era tore. DSW 257400 STLCOPCB4061519  ' IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 150Test Methods 11,608-54 Test for Dielectric Constant- and rower Factor- cf Aroclors, Pyranols Inerteens, and Tri -Tetraohlorobenzene Blends, Method No. 11,608-54,contd. 12. Flace the cell era sample In the even and make the same connections from the. cell to the bridge as in Steps 3 and 4, DO NOT 3nt-erchange connections. 13. Allow fifteen rat rot es Tor the cell to reach temperature equilibrium inside the oven. 14. Remove thermometer from the oven before taking a measure ment. This is important. 15 Make the ad.iustm.ent of controls on the electrical appa ratus as directed in Fart I of this method. 16 Balance the bridge b rotating the "CAPACITANCE" and "DISSIPATION FACTOR" dials nr. Panel No. 3 until the wide vertical band or the oscilloscope screen, is adjusted to a minimum width-. 17 Record the sum of the readings cr the "CAPACITANCE" dial and vernier, and call this value X. 18 Record the arm of the reading? or. the "DISSIPATION FACTOR" dial and svi tc-.b. Call this value D. Calculationst Dielectric. Co; yj'K Li -Y'r-- t p K u-ao.tr = o-er i J..-S C -.; - reading^rrom Step 17. Constant (Determined in Part II) Constant (Determined in Part II) art (Determined in Part II) DSW 257401 STLCOPCB4061520 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 151 Test Methods 11,608-54 Test for Dielectric Constant and Power- Factor of Aroclors, Pyranols Inerteens, and Trl-tetrachlorobenzene Blends, Method No. 11,608-54,contd,, % Power Factor = f Where % ff. = D; = Test Frequency (60 cycles or 1000 cycles) frequency of "Range Selector" on Panel No.5 Dissipation Factor reading from Step 18. NOTE; When D (dissipation factor) is less than 0.1, the dis sipation and power factors differ by less than 0.0005. There fore, for our measurements, power factors and dissipation factors are equal. Precision; (Reference; General Radio Manual for Model 716-C Capacitance Bridge). a. Capacitance readings are precise to + 2 uuf x multiplier reading (+ 0.2# of full scale for each range) when the dissipation factor is less than 0.01. b. Dissipation Factor (Power Factor) readings are precise ^ to + 0.0005 or + 2% of the dial reading whichever is larger, for values less than 0.1 for D (Dissipation Factor). IV. Apparatus A. Oscilloscope; Heathklt. Model 0-6. 8, Constant fcerperature Heating Unit; Fisher Isotemp oven. Model 13-245A, modified to include inter-wall connectors. C. A. C. Generator; General Radio type 1302-A. SVV 257402 STLCOPCB4061521 1 IX. SPECIFICATIONS AND TEST METHODS, eontd. IX - 152 Test Methods 11,608-54 Test for Dielectric Constant and Power Factor of Aroclors, Pyranols, Inerteens, and Tri-tetraehlorobenzene Blends, Method No. 11,608-54, eontd. IV. Apparatus, eontd. D. Amplifier and Null Detector: General Radio type 123I-B with type 1261-A power supply. E. Capacitance Bridge: General Radio Company Capacitance Bridge type ?'Io-C. F. Test Cells; G. E. type, concentric cylinder electrodes Catalog # 1,55.9; 667. G. Class E driver transformer: This is used for 60 cycle measurements to excite the bridge directly from the domestic power line. It has 50 volts output with a 4800 ohm resistor in series. H. Tuned Circuit Filters; General Radio Type 1231-P2 (400 and 1000 cycle) and 1231-P3 (60 cycle). These filters aid in obtaining a more accurate frequency for the measurements by removing harmonics, noise, hum., etc. / DSW 257403 STLCOPCB4061522 IX, SPECIFICATIONS AND TEST METHODS, contd. IX - 153 Test Methods 11,732-54 Date: 4/22/54 Material: General Method Method No, 11,732-54 By: DKL, NPA:WJG Test: Color (N. P. A. scale)1 WGK G.M. No, 11 1. Pill a 1-5/16" x 5" N. P. A. glass test jar (N. P. A. tube) half full of the liquid (or molten) sample. 2. Place the jar In the right hand opening in the A. S. T. M. Union Colorimeter and a similar tube half full of distilled water in the left hand opening. 3. Observe the sample and standard colored glasses through the observation opening (hole). 4. Turn the knob that brings the various colored glass standards into view. . 5. Match the sample as nearly as possible with the color standards. The method is precise to + 1/4 N. P. A. units. Report the color to the nearest 1/4 N. P. A. unit. Reference: ASTM Union Colorimeter and the N. P. A. Color StandarcB are given in ASTM Designation: D-155-45T (see 1952 Book of ASTM Standards, part 5> pages 86 to 90 inclusive). DSW 257404 STLCOPCB4061523 v IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 154 Test Methods 11,751-53 Dates 2/26/53 Bys CM, HOH, LJW,WJG, NPAs SMK Material; Aroclors, Pyranols, Method No. 11,751-53 Iner-teens, and Tri-Tetrachloro- benzene Blends WGK Dept.No. 253/246 Test s Procedure for Cleaning of Electrodes. G. E. Cell, and Accessories A. The Electrodes Cleaning Procedures 1. Remove the electrodes from the tested material while hot and allow them to drain. 2. Place the electrodes in hot TCB for 10 minutes. 3. Wash with unheated TCB. 4. Rins& twice with methanol and twice with tap water. 5. Place the electrodes in hot 10$ T. S. P. solution. Soak and heat for 10 minutes. f 6. Wash thoroughly with tap water. ` CAUTIONS After Step 6 -- DO NOT TOUCH THE ELECTRODES WITH HANDS I 7. Wash with distilled water twice. 8. Dry in drying oven for at least two hours at 120C. B. The G. E. Cell Cleaning: . 1. Reciean the Cell before use, if more than 8 hours have elapsed since the previous cleaning. .2 Follow the procedure for- the electrodes starting at Step 4. C. Cleaning of the Accessoriess DSW 257405 1. Apply the same cleaning procedure as given for the electrodes (Steps I to 8} to prepare the glass spacer and beaker for next . test 2 Clean the thermometer in the same manner as the electrodes, except for Step 8. u .-Z. Place the wet thermometer (after Step 7) directly in position in "n? Temperature Hearing Unit (Modified Fisher Isotemp Oven) and STLCOPCB4061524 IX, SPECIFICATIONS AND TEST METHODS, contd. IX - 155- Test Methods 11,752-53 Date: 2/26/53 By: CM, LJW Material: Aroclors, Pyranols, Inerteens, and Tri-Tetrachlorobenzene Blends Test: Electrical Measurements Method No. 11,752-53 WGK Dept. No. 253/246 Introduction: Some of the Aroclors, Pyranols, Inerteens, and Tri-Tetrachlorobenzene Blends have Important Industrial uses based on their electrical properties. Therefore, tests for certain electrical properties are made on these products. General Information: The tests should be run in the following order: Test Method No. 1. Dielectric Constant 11,608 2. Power Factor (if needed) 11,608 3. Resistivity 11,607 4. Dielectric Strength 11,605 The terms, which are used in connection with the above listed electrical measurements, are defined as follows: 1. Dielectric: A dielectric is an insulating or non-conducting material. 2. Pielectric Cons tant; The dielectric constant is the ratio of the equivalent parallel capacitance of a capacitor in which the material DSW 257406 STLCOPCB4061525 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 156 Test Method 11,752-55 Electrical Measurements for Aroclors, Pyranols, Inerteens, and Tri-Tetrachlorobenzene Blends, Method No. 11,752-53, contd. 2. Dielectric Constant, contd. is the dielectric, measured at a specified frequency, to the capacitance of the same capacitor with a vacuum as the dielectric, and is represented by the symbol K. The K of air may be considered equal to that of a vacuum. 5. Capacitor; A capacitor consists of an electrical conductor upon which an electric charge can be stored. In practice, a condenser consists of two or more metallic plates separated by a dielectric. 4. Resistivity: In the metric system, the volume resistivity of a material is the resistance between two electrodes which cover opposite faces of a centimeter cube. It is expressed in ohms/cm3. 5. Dielectric Strength; Dielectric Strength is the rupturing strength of an insulating material when subjected to voltage stress, under specific conditions and expressed in volts/milliampere. Breakdown varies with the shape of the electrodes and does not increase in proportion to the thickness of the dielectric. 6. Power Factor: The power factor of a dielectric is the ratio of the energy loss in the dielectric to the "apparent power" in the dieleotric. DSW 257407 STLCOPCB4061526 .* IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 157 Test Methods 11,784-55 Dates 10/7/55 Bys WRB,DKL DTMsSMK Materials General Method Method No. 11,784-55 Tests Refractive Index WGK G. M. No. 281 1. Study the attached diagram to familiarize yourself with the principal parts of the Refractometer which will be referred to throughout the method. CAUTIONs The glass from which the prisms in this instrument are constructed is necessarily somewhat unstable and is very easily scratched or corroded. It is, therefore, necessary to exercise extreme caution, in using them by following these 5 rules: a. Do not wipe the glass with any rough material or with anything in which there may be specs or grit. fc,, Never touch the surfaces of the Abbe Prisms. c. Clean the prisms only by flushing them with alcohol. Xylol, TCB or water. 2. Make sure that- the surfaces of the prisms, between which the fluid is to be placed, are perfectly clean. This can be accomplished by flushing them with alcohol and allowing to dryin air, 5. Turn on the stirring motor in the constant temperature bath by flipping the toggle switch marked "Line" to the up position. 4, Adjust the prisms to 25C. or other specified temperature as registered on the thermometer. This is done as follows? If the temperature is above 25C., turn on the valve back of the constant temperature bath which allows cooling water to circu late in the bath. If the temperature is below 25C,, flip the toggle switch in the upper right corner to the "Medium" position. This should bring the temperature to 25C. or other level, as pre-set and maintain it at that point. If It does not, an adjustment is required. Report this to your supervisor. DO NOT PERFORM ANY ADJUSTMENTS YOURSELF. Place several drops of pure distilled water on the auxiliary (lower) prism and immediately bring the prisms together and clamp them m position. DSW 257408 STLCOPCB4061527 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 158 Test Methods 11,784-53 General Method, Test for Refractive Index, Method No. 11,784-53, contd. NOTE; Be sure prism Is completely covered with water. 6. Turn on the light back of the refractometer and adjust the mirror until light is reflected into the lower prism. 7. Release the "Hand Positioning Control Clamp" and move the lever arm slowly by hand until a position on the scale, at which the lower part- of the field is dark and the upper part light, is obtained. 8. Clamp the movable arm in this position by means of the hand positioning control clamp. 9. Move the mirror slightly. If the dividing line moves it is spurious. The mirror should be moved to clear the spurious dividing line from the field and the true dividing line sought again. 10. The border between the light and dark portions of the field will usually be coloured. This may be corrected by turning the "Com pensator Control Knob" so that a sharp black and white edge Is obtained. 11. Finally adjust the "Tangential Screw Mechanism" until the black edge just crosses the intersection of the cross-wires. 12. The refractive index is then read by observing the scale of the "Alidade Arm" through the "Scale Magnifier", the fourth decimal place being estimated. 13. If the reading of the distilled water at 25C. varies from 1.3325 (the true index of distilled water at 25C.)record the correction and appl:/ this same correction to the sample reading when it is observed. NOTE; Corrections at other temperatures than 25C. may be made with suitable conversion -- see your supervisor. 14. Repeat Step s 2 to 12 Inclusive substituting the sample in place of the dist. .led water in Step 5. DSW 257409 15. Apply '4hc crr-ecf-ion from Step 13 and record the reading. 16. Repeat Step s 2 to 15 excluding Step 14 twice more, using fresh - ! e e. c - time. The readings should agree within 0,0001 units, Re f r a : i i ve Index at 25 "C. to the nearest 0,0001 unit. STLCOPCB4061528 v .` IX. SPECIFICATIONS AND TEST METHODS, contd. ' IX - 158 a Test Methods 11,784-53 ABBE TYPE REFRACTOMETER Scale \ JMagnifier Line Reticule Alidade Scale Movable Levep Arm Hand Positioning r Control Clamp Tangent Screw Line Adjustment Auxiliary (Lower^l Prism _) Mirror ! Compensator ^Control Knob Heating Chamber Clamp Thermometer Detachable Hinge A-7751 SW 257410 STLCOPCB4061529 SPECIFICATIONS AND TEST METHODS, contd. IX - 158 b. Test Methods 11,784-55 DSW 257411 STLCOPCB4061530 IX, SPECIFICATIONS AND TEST METHODS, contd. Dates 7/30/55 Materials General Method BysDKL,WJGsSMK Test: Turbidity IX - 159 Test Methods 11,788-55 Method No, 11,788-53 WGK G.M. No. 15* 1 The turbidity of WGK Plant Products and Raw Materials is determined by comparison of a sample of the material with a set of ten turbidity standards representing the normal range of turbidity encountered. 1. Shake the sample for 15 seconds. - 2. Compare the sample Immediately to the appropriate turbidity standards in sample bottles of the same size and similarly shaken. Report the turbidity to the nearest standard number, e. g. Turbidity, = Standard No. 5. NOTE; A helpful procedure is to compare the ease which one might see a pencil or window frame through the sample and standards, or to com pare the haze in the sample and standards against a well lighted white back-ground. Turbidity Equivalents: Standard Number H SO^ Std. No. 1 2 3 51 62 73 8^ 9 --10 3 Preparation of- Standards: ~H5P04 Std. No. 1 2 4 8 18 APHA Turbidity ppm Suspended Matter 2 4 8 16 .3^ . 60 125 250 500 1000 Turbidity stock solution, 1000 ppm Fuller's Earth in accordance with APHA 6th Edition, obtained from the Hartman-Leddon Co. (Harleco) Phi 1 ade I phi a., Pa . DSW 257412 STLCOPCB4061531 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 160 Test Methods 11,788-55 Test for Turbidity, General Method, Method No. 11,788-55* contd. The stock solution is Standard No. 10. The standards are prepared by dilution of the well shaken stock solution as follows: Standard ml. Stock Solution diluted to one liter 10 1000 9 500 8 250 7 125 6 60 5 50 4 15 Dilute 100 ml, of the well shaken Stock Solution to one liter and dilute as follows: ml. Stock Solution diluted Standard to one liter 5 80 2 40 1 20 Add 50 ml. of a 5$ mercuric chloride solution containing 1# HC1 per liter- of final standard before dilution. The mercuric chloride serves as a preservative to prevent mold growth in the standards. For verification, the newly-prepared standards may then .be compared with reference turbidity standards (kept by the Service Section) from the Hartman Leddor Company representing the A. P. H. A. turbidity values listed in the Turbidity Equivalents table. DSW 257413 STLCOPCB4061532 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 161 Test Methods 11,861-54 Date; 5/6/54 Material; Phenoxypropene Oxide Method No. 11,861-54 (Glycidyl Phenyl Ether) By;WGM,NPA;WJG Test; Crystallizing Point WGK Dept. No. 246 CAUTION; Phenoxypropene Oxide (Glycidyl Phenyl Ether) is a toxic* 1 irritant. Handle with care and avoid contact with the skin. Wear your Safety Glasses 1. Prepare a dry ice-acetone bath in a 400-ml. beaker. 2. Prepare an ice-water bath in a second 400-ml. beaker. 5. Pill a 1" x 4" test tube 5/4 full with the sample. 4. Insert a -15 to 20*C. range thermometer and place the test tube (supported by a lead disc provided for this purpose) in the dry ice-acetone bath. Stir constantly with the thermometer. 5. Upon cooling of the sample to -2 to 5C. remove it from the bath and seed with previously prepared crystals of Phenoxy propene Oxide (PPO). 6. Replace the sample in the dry ice-acetone bath. Continue stirring scratching repeatedly the sides of the test tube, until the temperature begins to rise or until the sample cools to -15C. IMPORTANT; DO NOT COOL BELOW -15C. 7. Immediately place the sample in the ice-water bath and continue stirring until the temperature reaches a maximum point. Record this temperature. 8. This maximum temperature is the crystallizing point. The method is precise to + 0.1C. Report the result to the nearest 0.1C. DSW 257414 STLCOPCB4061533 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 162 Test Methods 11,862-54 Dates 5/5/54 By:NN,NPAsWJG Material: Phenoxypropene Oxide (PPO) Test: Distilling Range Method No. 11,862-54 WGK Dept. No. 246 CAUTION: Glycidyl Phenyl Ether (Phenoxypropene Oxide: P.P.O.) is1 a toxic irritant. Handle with care and avoid contact with the skin. Wear Your Safety Glasses. 1. Determine the distilling range of PPO according to General Method No. 1 (Method No. 10,006) with the following modifi cations: .1 2. Insert a 250 to 260C. range, 5" Immersion thermometer. 5. Use a transite board with a 2-inch opening. 4. Distill at the rate of 2 drops per second. 5. Apply the thermometer and barometric correction. Report the following temperatures: First drop 95# (1-96 ml.) range 100# (First Drop to Dry Point) range Dry point Report the results to the nearest 0.1C. DSW 257415 STLCOPCB4061534 IX - 163 . Test Methods 11,863-54 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 5/3/54 Material: Phenoxypropene Oxide Method No.11,863-54 By: NN,NPA:WJG Test: REFRACTIVE INDEX AT ' 25#C. WGK Dept. No. 246 CAUTION: Glycidyl Phenyl Ether (Phenoxypropene Oxide: P. P. 0. ) is a toxicirritant. Handle with care and avoid contact with the skin. Wear Your Safety Glasses. 1. Determine the refractive index of PPO at 25C. according to General Method No. 28 (Method No. 11,784) with the following modifications. 2. Clean the Abbe prisms by flushing with Trichlorobenzene. Then follow with benzene and "Mersol" washes. IMPORTANT: Do Not Touch the Polished Surfaces of the Abbe Prismsi Report the Refractive Index (N^25 ) to the nearest 0.0001 unit. / -/ DSW 257416 STLCOPCB4061535 ' IX, SPECIFICATIONS AND TEST METHODS, contd. Dates 7/23/54 By: NN, NPA, GWMsWJG Material: Phenoxypropene Oxide (PPO) Test: Specific Gravity . IX - 164 Test Methods 11,864-54 Method No,11,864-54 WGK Dept. No.246 CAUTION: Glycldyl Phenyl Ether (Phenoxypropene Oxide: PPO) is a toxic irritant. Handle with care and avoid contact with the skin. Wear Your Safety Glasses, . 1. Determine the Specific Gravity 25/15*5#C. according to General Method No. 13 (Method No. 10,497) with the following modifi cations : 2. Use a 1.000 to 1.200 range hydrometer. 3. Use a 0 to 50C. range thermometer. 4. Adjust the temperature of PPO between 20 - 30C. 5. Apply (if any) the hydrometer correction. 6. Use Specific Gravity Coefficient 0.0008 unlt/C. Calculation s A. For Specific Gravity at 15.5C./l55C. Temperature Correction = (Temp.of Sample - 15.5eC.) x 0.0008 Add this correction to the reading obtained if the tempera ture of the sample was above 15.5C.', subtract if below 15,5C. B. For Specific Gravity at 25C./15.5C. Temperature Correction = (Temp.of Sample - 25C.) x 0.0008 Add this correction to the reading obtained if the tempera ture of the sample was above 25C. subtract if below 25cC. The method is precise to + 0.001 unit. Report the Specific Gravity 15.5C./15.5C. and 25C./15.5C. to the nearest 0.001 unit. sw 257417 STLCOPCB4061536 IX. SPECIFICATIONS AND TEST METHODS, contd. Date; 7/8/52 Material: Transformer Inerteen (PPO) By: NN, TT:SMK Test: (Phenoxypropene Oxide) IX - 165 Test Methods 11,865-52 Method No. 11,865-52 WOK Dept. No. 246 NOTE: Run this analysis in duplicate Preparation of Reagents: Indicator - Mix 1 part of a 0.1# water solution of cresol red with 5 parts of a 0.1# water solution of thymol blue. Pyridinium Chloride Reagent - Completely mix 16 ml. of cone. HC1 with 1 liter of Baker's C. P. pyridine. 1. Weigh (+ 0.05 g.) a 100 + 5 g. sample into a 500 ml. Erlenmeyer flask. 2. Add by pipette 20 ml. of the pyridinium chloride reagent. 5. Attach to a reflux condenser and reflux for thirty minutes. NOTE: Measure reflux time from the start of boiling. 4. Turn offthe heat at the end of the reflux period, and add 50 ml. of distilled water at the top of the condenser. 5. Detach the flask from the condenser and wash the end of the condenser with a few ml. of distilled water. 6. Cool the flask and contents to room temperature in ice water or under the tap. ' 7. Add 1 ir4. of the cresol red-thymol blue indicator. 8. Swirl.wfche flask rapidly so that there is a thorough and violent mixing of the contents while titrating with 0.1 N NaOH to a distinct blue colour. DSW 257418 STLCOPCB4061537 . . ' IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 166 Test Methods 11,865-52 Test for (Phenoxypropene Oxide)ln Transformer Inerteen (PPO), Method No. 11,865-52, contd. NOTE; If any doubt exists about the end point allow the layers to separate completely after each addition of NaOH where close to the end point. The end point has been reached when the upper aqueous layer Is blue. 9. Blank; Into a 500 ml. Erlenmeysr flask, weigh, on a beam balance, a 100 + 5 g. sample of Transformer Inerteen which contains no PPO. 10. Repeat Steps 2 to 8. Calculations; A = ml. 0.1 N NaOH for blank. B = ml. 0.1 N NaOH for sample $ Phenoxypropene Oxide (PPO) = (A - B)(Normality NaOH)(15.0) Gram Sample Report to the nearest 0.001$. Reference; Westinghouse Research Report No. 60-94602-9-48. DSW 257419 STLCOPCB4061538 ` ' IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 167 Test Methods 12,033-53 Date: 5/12/53 By:NPA:SMK Material: Trl and Tetrachloro - benzene Blend ' Test: Last Crystal Point Method No.12,033-33 WGK Dept. No.. 246 1. Fill Pour-Point test jar with sample to a depth of two Inches. 2. Insert the thermometer-stirrer assembly so that' the mercury bulb of the thermometer Is near the center of the sample. . 3. Cool, while stirring, until sample is at about -15C. 4. Seed with a few crystals of 1,2,4,5 Tetrachlorobenzene and con tinue stirring and cooling until the sample crystallizes forming a slurry. _ 5. Continue stirring at the rate of one to three strokes per second, while exposing jar and contents to room temperature. NOTE: As the last crystal point approaches, the mercury meniscus of the thermometer under the liquid is invisible, but it is within a range of 0.2 - 0.3C. from surface of the sample. 6. Record temperature at which the mercury column of the thermometer just becomes clearly visible. This is the Last Crystal Point. NOTE: The visibility does not appreciably change during the next 0.5C. rise in temperature. Report the result to the nearest 0.1C. Apparatus: A Pour-Point test jar (see Section 3 a, ASTM D97). A -15 to 20 C. range thermometer accurately calibrated and having 0.1C. subdivisions. A loop stirrer of a heavy gauge wire. A rubber stopper with holes to accomodate thermometer and stirrer. DSW 257420 STLCOPCB4061539 IX. SPECIFICATIONS AND TEST METHODS, contd, Date; 2/6/53 ByiNPAsSMK Material; Tri-Tetrachlorobenzene Blend Test: Distilling Range* 1 IX - 168Test Methods 12,034-55 Method No. 12,034-53 WGK Dept. No. 233/246 1. Determine the distilling range of the sample according to General Method No. 1 (Method No. 10,006) with the following modifications: 2. Use a transite board with a 2" opening. 3. Use a 0 - 360C. range 3-inch Immersion thermometer (corrected at 200 and 250C.) with 1C. subdivisions. 4. Use an air-cooled condenser. Any crystals must be kept from forming in the tube by playing a flame over its length as needed. 5. Report the following (corrected) temperatures to the nearest 1#C. First Drop 5# by volume . 65# by volume 90# by volume 95# by volume Dry Point. NOTE? The distillate is collected "by volume" and not "by weight" as in the case of Pyranol distillations. DSW 257421 STLCOPCB4061540 .` IX, SPECIFICATIONS AND TEST METHODS, contd. IX - 169 Test Methods 12,056-53 Date; 2/10/53 By; TT,NPA;SMK Material; Tri-Tetrachloro- Method No, 12,036-53 benzene Blend WGK Dept. No. 233/246 Test; Composition by Distillation Use a beam balance for all weights.1 1. Weigh a "heel" of 200 (+0.05) g. of Aroclor 1248 into a 2-liter still-pot containing three large Berl saddles and a glass "Perculator" tube. 2. Weigh into the same (tared) pot a 700 (+ 0.05) g. sample of the Tri-Tetra-blend to be tested. .. 3. Connect the still-pot to the distillation unit. 4. Turn on the electrical current to heat up the distillation assembly (DO NOT APPLY HEAT ON THE HEAD AT THIS TIME). 5. Carry out the distillation at an atmospheric pressure and take fractions as follows: a. Fraction 1 (Trichlorobenzene Fract.): Collect distillate from 204 to 220C. (the distilling head temperature), into a 500-ml. Erlenmeyer flask (tared). b. Fraction 2 (1st Intermediate Fract. - Tri-Tetrachlorobenzene): When the distilling head temperature reaches 220C. remove the receiver with 1st Fraction and replace it with a dry, tared 250-ml. Erlenmeyer flask. Collect the intermediate fraction until the head temperature reaches 245C. NOTE: To prevent possible "Freezing" during this stage of the distillation, turn on electrical current in the circuit to the distilling head when the head temperature reaches ca. 230C. c. Fraction 5 (Tetrachlorobenzene Fract.): Collect the distil late at the head temperature 245-255C. into a dry, tared 500 ml. Erlenmeyer flask. DSW 257422 STLCOPCB4061541 . IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 170 Test Methods 12,056-53 Test for Composition by Distillation of Tri-Tetrachlorobenzene Blend, Method No. 12,056-53, contd. NOTE; An additional heat on the distilling head may be required during part of this fraction. , d. Fraction 4 (2nd Intermediate Fract.) - Tetra-Pentachlorobenzene Fract.): Collect all distillate from 255-275C. in a dry, tared 250-ml. Erlenmeyer flask. NOTE; If the Pentachlorobenzene content is not required, the dis tillation may be terminated at this point. If the "Penta" is desired then proceed as follows: e. Fraction 5 (Pentachlorobenzene Fract.): When the head temperature reaches 275C., replace the fourth fraction receiver with a dry, tared 250-ml. Erleneyer flask and collect all distillate until the head temperature is 277C. 6. Stop the distillation. Turn off electric current from the pot heater only. Allow half an hour for the head and column to drain. Turn off the current on all units. 7. Weigh and record all the fractions collected. 8. Upon weighing, determine a crystallizing point of Fract. 3 using a 20-55C. range, 3" immersion thermometer. Record the highest temperature reached after crystallization has taken place. o Determine from Dwg. No. A-5538 on page IX - 173 below the 1,2,3,^- . 'and'1,2,4,5-Tetrachlorobenzene isomeric content of this fraction corresponding to the crystallizing point of the fraction. Record percent for each of the isomers. 9. After the still-pot cools down, determine weight of the residue as follows: wt. of Residue (gms) = [wt ,, of Pot - (wt. of "Heel" + still-pot Step 1)J DSW 257423 STLCOPCB4061542 . IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 171 Test Methods 12,056-53 Test for Composition by Distillation of Trl-Tetrachlorobenzene Blend, Method No. 12,036-53, contd. Calculation; . $ Trichlorobenzene = (wt. of Fract. 1 -t- | wt. Fract. 2) x 100 Sample Weight (Step 2) Total Tetrachlorobenzene (gms) = wt. of Fract. 3 wt. Fract. 2 (Tetra) + ^ Fract. 4) ,$ 1,2,3,4-Tetra Isomer = total wt. of Tetra x percent 1,2,3,4 Isomer (Step 8) Sample Weight (Step 2) $ 1,2,4,5-Tetra Isomer = total wt. of Tetra x percent 1,2,4,5 Isomer _____________________________ (step 8) Sample Weight (Step 2) Examples A 700 g. sample of the blend has been distilled. Total Tetra Fraction weight was 70 g. It was found from Dwg. A-5538 that isomers were present in the following percentages: 1,2,3,4-isomer 90.0$ and 1,2,4,5-lsomer 10.0$. Then the percent of each isomer in the blend will be as follows: $ 1,2,3,4-Tetra isomer = 70 x 90 = 9-0$ by wt. of sample (Step 2) 700 $ 1,2,4,5-Tetra. isomer = 70 x 10 1.0$ by wt. of sample (Step 2) 700 $ High Boilers (as Pentachlorobenzene) = fwt. of Fract. 5 + \ wt. of Fract. 4 + -g- Residue (Step 9)1 x 100 Sample Weight (Step 2) DSW 257424 STLCOPCB4061543 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 172 Test Methods 12,036-53 Test for Composition by Distillation of Trl-Tetrachlorobenzene Blend, Method No. 12,036-53* contd. % Loss on distillation = fwt. of Sample (Step 2) - (combined wt. of Fracts. + vrt. Residue _(Step 9)3 x 100 Sample Weight (Step 2) Report all components, residue, and loss on distillation to the nearest 0.1$ Apparatus;* 1 1 - A 2-liter, S 24/40 Jaeck, round bottom distilling flask (pot). 1 - A four foot stainless steel packed column. 1 - An insulated and electrically heated distilling head with a thermometer (S 10/30 joint). 1 - A 500-ml. "glass-col" heating mantle. 3 - Variacs (to regulate individual heating of the distilling head, the column, and the pot). 1 - A 0 - 360C. range, S 10/30, thermometer (corrected)for the distilling head. 5 - Receiverst ' 2 x 500-ml. and 3 x 250-ml. Erlenmeyer flasks. DSW 257425 STLCOPCB4061544 ix - .173 . Test Methods 1p 15EPT 5-233 . :. STLCOPCB4061545 IX. SPECIFICATIONS AND TEST METHODS, contd. Dates 9/23/5^ BysWWKsWJG Material: Aroclors, Pyranols and Inerteens Test s Sulfates IX -174 Test Methods 12,169-54 Method No. 12,169-54 WGK Dept. No. 246 Scope s This method of test is intended for the qualitative determination oi inorganic sulfates, by precipitation with BaCl2, in chlorin ated biphenyl products. Apparatus s 250-ml. separatory funnel, 1x6 inch test tube, and a burette or 5-ml. pipet. Reagents s 10% (by wt.) aqueous BaCl2 solution and C.P. HC1 Procedure 21 1. Place 75 ml. of distilled water in a clean 250-ml. separatory funnel. 2. Heat the water to boiling by means of a Bunsen flame. 3. Add 100 ml. of sample to the funnel. 4. Shake contents of the funnel thoroughly, venting occasionally through the stopcock, for ca. 1 minute. 5. Allow the layers to separate. 6. Discard the lower or sample layer. 7. Drain 15 ml. of the water layer into a clean 1x6 inch test tube. 8. Heat to boiling over a Bunsen flame. 9. Add 5 drops of C.P. cone. HC1, then slowly add 5 ml. of BaCl2 solution from a burette or pipette, and shake to mix. A white precipitate reveals the presence of sulfates. Report as follows 2 If no precipitate is noted immediately report as "None". If a precipitate is noted report as "present". Referencet ASTM-D117-53T and D878-49. DSW 257427 STLCOPCB4061546 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 175 Test Methods 12,208-54 Date: 8/20/54 By:GWM:WJG Material: Aroclor-Butylacetate Mixtures Test: Composition Method No. 12,208-54 WGK Dept. No. 246 1. Ascertain that the lot number of the Aroclor 1254 (used in the mixture) is recorded on the label of the sample bottle. 2. Determine the Specific Gravity of the mixture at 29C,/15.5C. using General Method No. 15 (Method No. 10,497) with the fciCLcwing modifications: a. DO NOT heat the material to greater than 55C. b. Use a 1.400 to 1.600 range hydrometer. c. Use a 0 to 50C. range paper scale thermometer. 5. Apply the hydrometer correction (if any). 4. From chart A 7780 on the following page, IX - 176, determine if the corrected Sp. Gr. of the Mix at 29/15.5C, falls within the shaded portion of the chart at a point corresponding to the Specific Gravity** at 65/I5*5C. of Aroclor 1254 used in the blend. - Report only the Specific Gravity of the mixture at 29/15.5cC. and indi cate whether or not the material passes the specification limits. (Whether it falls within the shaded area on the chart or not.) Remarks: The diagonal lines on the chart indicate the $ Butylacetate present in the mix. at the corresponding coordinates of specific gravity of the mix at 29"/I5.5C. and the specific gravity of the Aroclor 1254 at 65/15.5C. * This Specific Gravity may be obtained from the analytical ticket file. DSW 257428 STLCOPCB4061547 10X 10tothe%inch. 6thline#accented. STLCOPCB4061548 v IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 177 Test Methods 12,215-54 12,214-54 Date: 8/24/54 By: TT:WJG Material: 1254 Aroclor Butyl Acetate Mixture Test: RefractireIndex Method No.12,215-54 WGK Dept. No. 246 I. Determine the Refractive Index of the mixture at 25C. using General Method No. 28 (Method No. 11,784). NOTE: Do not leave the sample bottle unstoppered, since possible volatilization of the butyl acetate would change the composition of the mixture. Date: 8/24/54 By: TT:WJG Material: 1254 Aroclor Butyl Acetate Mixtures Test: $ Butyl Acetate Method No. 12,214-54 WGK Dept. No. 246 1. Tare on an analytical balance a clean dry aluminum dish. Record the weight. 2. Weigh accurately on an analytical balance a 5 (+ 0.1000) g, of the mixture into the dish and record weight of dish and sample. 5. Subtract weight of Step 1 from weight in Step 2. (This is the weight of the sample). 4. Place the dish into a 108 + 1C. oven for 5 hours. 5. Cool in a desiccator. 6. Reweigh and record weight of dish and contents. Calculation: 5 $ Butyl Acetate = Original sample and dish (Step 2)-Final Wt.(Stey)x 100 Sample Weight (Step 5) Report to the nearest 0.1$. ' DSW 257430 STLCOPCB4061549 . IX, SPECIFICATIONS AND TEST METHODS, contd. Date: 8/24/54 ByiTTsWJG Material: 1254 Aroclor Butyl Acetate Mixtures Test: Color IX - 178 Test Methods 12,215-54 12,220-54 Method No.12,215-54 WGK Dept. No. 246 1. Determine the color of the mixture In terms of APHA units. Refer to General Method No. 2 (Method No. 10,007). Date: 9/29/54 By: WWKWJG Material: Aroclors, Pyranols, Inerteens Test: Light Transmission Method No. 12,220-54 WGK Dept. No. 246 Scope: The purpose of this method is to measure the percent light trans mission through 246 products as compared to distilled water which has a transmission of 100$. Equipment: 1. The Fisher Electrophotometer. 2. An empty plastic filter holder (no filter). 5. Round, 25-ml., matched absorption cells. Procedure: 1. Determine the Light Transmission according to General Method No. l8 (Method No. 10,725-51) with the following modifications: A. Use an empty plastic filter holder. B. Use "A" light intensity. C. Use distilled water as a reference liquid. 2. Read the $ Light Transmission on the "B" scale Repent results tc the nearest 0.1$. DSW 257431 Reference: National Cash Register Co.'s Method 2021.55 (9/24/52). STLCOPCB4061550 * IX- SPECIFICATIONS AND TEST METHODS, contd. IX - 179 Test Methods 12,306-55 Date; 3/7/55 Material; Aroclors and Pyranols Method No.12,306-55 By: WWKsWJG Test: Parlink # 10 Viscosity WGK Dept. No. 246 IMPORTANT: Conduct this test in a room having a temperature of 23-27C.* 1 and away from drafts. 1. Support the cup in a level position on a ring stand high enough to permit the placing of a 50-ml. graduate and your finger under the cup. 2. Center a clean, dry 50-ml. graduate tinder the cup orifice. 3. Strain about 100 ml. of sample thru a funnel containing a 100 mesh or less screen into a clean, dry 250-ml. beaker. , 4. Adjust the temperature of the sample to 25 + 0.5C. 5. Close the orifice by placing your finger under the cup. 6. Pour the sample into the cup, avoiding air bubbles, until it is level full. NOTE: The cup must be exactly level full with the surface of the liquid being neither convex nor concave. 7. Remove your finger and measure the time, by stopwatch, it takes for exactly 50 ml. of sample to be collected. NOTE: Start timing the instant you remove your finger from the orifice. Report the viscosity in seconds to the nearest 0.1 second. Duplicate results should check within 1 (one) second. Reference; Geisman's memo to Schwartz, 8/5/54. This method is the same as that used by Du Pont at their plant in Pariin. New Jersey. DSW 257432 STLCOPCB4061551 IX - 180 Test Methods IXo SPECIFICATIONS AND TEST METHODS, ccntd. Note on the Inorganic Chlorides Test. . See also the comments on pages 12 - 17 in Section VII, above. It will be noted that the chlorides content is expressed in parts chlorine ion per million. The specification limit of 0.1 parts chloride per million calls for very special control technique,' especially in a plant area where the air is liable to be contamin ated with traces of HC1 gas etc. In order to get repeatable results, it was found necessary, at the Krummrich plant laboratory, to set up a special test room with a supply of clean air, and to keep the pressure in the room a little above that of adjacent rooms to prevent the entrance of contaminated air. Pull details of this special room were sent to Mr. Haywood at Newport, October 24, 1950,with drawings, and suggestions for improve ment arising out of Krummrich plant experience. Mr. Harden reported on visit to the Krummrich Plant control laboratory In August 1950* and Mr. Pennington visited the laboratory late in the same year to pick up the technique of the tests. Mr. Haywood, November 19, 1951* reported that Newport had installed such a special room. On February 2nd, 1955, Mr. Beauregard told us that G. E. In America no longer had "wide open" liaison with B. T. H. in England, but that MCL would, nevertheless, be in order in giving details of the G. E. test to B. T. H. MCC consider that the Munch test,in which the "volatile chlorides", formed during heating, are aspirated over into silver nitrate solution,gives a better estimate of the stability of the sample, but that MGC have not yet enough background of experience In the use of the test, and in the figures normally to be expected, to be in a position to recommend a change to the Munch test. MCL Research Progress Report 1151 - 52/1/12, May 1955, deals with Bakelite Cc.'s test of the same type as Dr. Munch's test. The faintly opalescent suspensions of AgCl are unstable, and the turbidity measurements have to be made on a rigid time schedule, using visual comparison in Tyndall beam. Mr. Barire suggested washing the condenser back into the sample,and using a Lumetron or similar SW 257433 STLCOPCB4061552 IX - 182 Test Methods IX. SPECIFICATIONS AND TEST METHODS, contd. Note on the Inorganic Chlorides Test, contd. presumably because the tintetraphenyl, performing its function of removing HC1 formed during the heating, has formed SnCl2 or SnCl^. The G. E. specification allows up to 5 ppm, but Mr. Kuster reports that MCC figures rarely exceed 2 ppm. While allowing the relaxation to 5 ppm, G. E. still insist that the separate main component shall show not more than 0.1 ppm. The same 5 ppm tolerance has been extended to "Inerteens" which contain glycidyl phenylether in place of tintetraphenyl, but experience indi cates that this tolerance is unnecesary. Presumably the glycidyl phenyl ether removes the HC1 by the opening of the alkene oxide ring: /\ -------C C + HC1---------------> / CC1--C--OH giving products /\ which volatilise away, or at least do not react with the silver nitrate. The very dilute sodium chloride standards required for the inorganic chlorides test require very special care in handling, otherwise they increase in strength by picking up HC1 etc. from the air. In practice they are not actually made up, except when a new operator is being trained. An experienced operator works from a visual memory of the Tyndall opacity given by the standard (actually it is about the faintest discernible opacity). Occasionally a high "chlorides after heating" figure on Inerteen has been traced to contamination with traces of tintetraphenyl picked up in the plant. MCL Research Progress report 1152 NR 52/103/3, September 195^> deals with a method of determining tin tetraphenyl in Pyranols. Report 1151 52/1/12, May 1953, shows that Aroclor 1262 is stable at 160C. in air. Report 1151, NR 53/97/1, July 1953, showed some darkening of 1262 in steel at 300C. in air. DSW 257434 STLCOPCB4061553 IX - 183 Test Methods IX. SPECIFICATIONS AND TEST METHODS, contd. Note on Electrical Test Methods. A great deal of work has been done by MCL in the development of electrical test methods and equipment, in consultation with customers, in testing of raw material supplies, and finished products, on the effect of stabilizers, effect of contamination by contact with insulating materials or gaskets, in customer service work generally, and in assembling data for various publications. See the list of reports' at the end of Section VII, above. Finished Product Samples sent to MCL. A complete set of samples of Aroclors 1142 to 5460 was requested April 1, 1947> also of all Montars, and of Pyranols 1467, 1488, 1496, with analytical data on each sample. (Aroclors II69, and 1269 had been abandoned in favour of 1170 and 1270). MCC report 171-1088, 2881, May 1953, compares Anniston and Krummrich plant 1260. Competitor's Products. Dr. Jenkins, February 20, 1952, reported.a statement to the effect that Bayer's equivalent of Aroclor 1254 had a resistivity of 100 to 900 x 109. MCC report 171-1075, 2887, discusses an Italian sample of "Fenclor". Ruabon Development Division Annual Report, 1951, page 4, discusses ICI's "Cereclors" as plasticisers for PVC. Aroclors were better for this purpose. Certain MCL research reports under job 1151, discuss.competitive products, for example, 1151 DF 53/86/5, March 1954, on French "Pyralene". . DSW 257435 STLCOPCB4061554 X. PLANT OPERATING DATA x.:- l Operating Data Plant Capacity In 19^6 the working rates of the different units at the Kruiranrich Aroclor plant were as set out in the table below. DSW 257436 STLCOPCB4061555 T IM E T A B LE - AROCLOF co P oo 3$ o in pi < in vo a .=t 3-=i- co ini ft vo m in 4S CM 1 Pc Sp rH O (0 ft ft oo ft O 3 Mh O' B3 J-3 CO p 3 O 43 ! OS E tCM n rH PI oo rH t'C) CM O iH PI < 0\ VO XJ CM ft rH iH I OCO CO VO CM -P S3 C ft OS Ik, P rH O C() ft rH >OO ft O 3 *& O' CO < W 43 i-3 n P 3 0 43 1 4) 6 CM VO CM rH CO I PO O VO rH CM O iH OI P --i" < in CM XJ rH rl I 3 CO cr-=tft CM -3 rH CM =)- CM P S3 C *h ftp rH O CO 4-t r-H >OO ft o 3wP CT42 < W -3 CO p 3 0 43 1 4> E C fot P cO P o> p. o ooo ooo movcM vovovo * o o mo o o o-sf CM O O O o CM O iHj4-j^-CO rH CM CM CM I II inino cm -=i- in --^--'snsr ino o o o m o o o o O =* COJ4-VO rH rH III inino vovovo injc-^ cm =*- in <D <1 *. o oo o o o o o in-=r cn ooo ooo O CM CO t^-t-VO o ino o o o =* coo 6 o o o o O co-^voco CM CM CM CM IIII CD ONO rH VO VO t'-C"CM CM CM CM ** ooo o o o o ooo o o o o VO ,=*- -=t COCO VO ft CM CM CM IilI I CO OVO rH CO VO VO t-t'-VD CM CM CM CM CM rH (H H H H * * ooooo ooooo rH t"- CM CO in vo int-t'-co oinoooooino ^coooooocoo o o coinovo h oj^ rH rH H CM CM IIIII CM CO = O CM si-jtf- in vo vo CM CM CM CM CM 'ST O O CM Sh O -P as rH S3 >ft a> S3 P E?g 4S O 43 rH S3 CO Q g-O f0t.4O3 O ft S3 bO as Was bO S3 C c C ft ft ft bOP -p a.p o rH O E as rH OS 3 43 43 fcoo 44 vp bO fSt3 -P as eo Sh e as 2 as xs fot O ft ft ft Sh to a] 44h) fCt 4C0 rfHt 00 ft ft ft S3 as X -p as Sh as ao Sh 4) Sh tH tHCfift Oo oo ** oo oo in cm co bO cn a> oo 40 rl Sh 00 -p 4> Sh erf 4) Sh E BJ C C O 2S a -p -p H -P 00 a) oo oo ft .4) S3 S3 O Sh 0.8 O O -P SJ. ft cs bC cs to S3 bo bO to S3 40 ft bO S3 S3 S3 <H C Sh S3 rl 3 rl 4) a $3 S CH ft rH D. as as OS rH rH j-H o as -'p rH *rH Sh rH o SQ &H fe &h P O 4) E C o H ft o 3 o o Sh a o S3 -p W 4f3t 4) rH O >> O bO e hH ft as P 4) P. O 4} 4ft3 bO fCt P 3 XS 00 4) E 43 o 300 -p as o as o <p P 4> a a> P as oo C o ft P as P v ft o -P oo a> o 00 rH 4S 43 CO X-1 Plant c i oo Capacity OJr-H -P *rH rH P -P 3 3 n oo Or) 0) 43*0 P P H TO 42 SCO OS *H r-H W 43 * Cs H--' O ^ H XS O-P 0) p as -p C 4) >jhH rH rH P ft POE IS rH O rH 43 O H O EP H 4) rl _a *4>3 c o o 0) C *H E OP P <h OS O -P p 4-t o as P 3 ft 0) T3 O ft o Pc oo ft o rco Tt r io CM 5 CO Q a> bO p as 43 o hH P 00 4) c co CM as as xs 43 as O 43 -P to a) H 43 C ri P o p p as C fot <H P i--OI 43 rH 43 oo ,,o as co as vo p V-H p> C O as op H 4) 4> PP (d as as o 43 P -P 3 as O X >3 43 as as E as p ft P P 4) 4) 43 oo 4) as 'E o ft 43 -P O bO rH bp43 tH C -P H as S3 +3 3 43 o +3 . as ft Vp as KP O3 P to ft . . ft ft as as faO o P C ft +3 o 4) H 3 as p as as P Cp 3 xs 4) *0 rH 43 4> H P o pc as as fcts P -43 rH rH xs p - 4) >3 X >rH O 4) +3 43 a] C o> ft 3 xs HXC O' rH oo o w a3> as as 3 43 O H ft as % cas as P 4> P as in P C 4h C as o o o 00 i P *H ID P X3 as P P P> C hO C o as o as P as 03 3 as to H *o oo XJ P O S3 O as c 43 as cs ft o PoP o 3 ft -h ft as C X3 +3 oo O O C as 4-H P "H p O as as 43 K> ft as +> p as 4) ft oo as P 4J E o oo 43 -H O P -P ChH O E H K o S> I--1 aS fftt C p H as p 4) 00 -P ft as 3 O (d c ft o 5 rlrHrl < * * STLCOPCB4061556 .X. PLANT OPERATING DATA, contd. X-2 Operating Data Plant Capacity, contd. See also page 5 of Section VI, above, for chlorination time cycles. With four main chlorinators, one air-blowing tank, and two vacuum stills, 9,624,188 lbs. of liquid Aroclors, and 121,812 lbs. of solids were made in 1944. The best month up to 1947 had produced over 1 million pounds. The capacity in 1954 (five main chlorinators, two air-blowing vessels and two vacuum stills) was given as l million pounds per month. In 1954 the capacity for Aroclors was given as l million pounds per month. The Pyranols plant was rated at l million pounds a month in 1953. Typical operating times for Pyranols were given in 1947 as follows: Pump Aroclor to mixer Pump TCB to mixer Mix and sample Adjust composition and mix again Add tin-tetraphenyl, mix and sample Clean the press 8.0 hours 5.0 hours 2.5 hours 5.0 hours 2.0 hours 0.5 hours 21.0 hours * This period is required for each separate adjustment found necessary The elapsed time from starting a batch to finishing and loading was about 5 to 6 days. It took about 5 hours to load an 8,000 U.S. gallon rail tank. Labour. At Anniston one operator per shift looks after six to seven chlorin ators, and another looks after the two stills. The chief operator of the area helps as necessary, and extra labour is available for drumming off and similar occasional heavy loads. See page 25 Section VI, above, for the labour needed for the distillation of solid Aroclors. One man, per shift, borrowed from the Aroclor department, does practically all the Pyranol work at the Krummrich plant. DSW 257438 STLCOPCB4061557 X. PLANT OPERATING DATA, contd. X-3 Operating Data Yields The departmental monthly returns are complicated because of the number of finished products, each with its own requirements of raw materials, and of services. Another difficulty is that the receipts of chlorine into the department are not measured in any wayj the "consumption" of chlorine is reckoned back from the "make" of Aroclors. other In the Krummrich plant Aroclor department, receipts of/raw materials, and despatches of finished goods,are totalled for the month in the usual way, and the month-end inventory made as described in Section VI, above, pages 47-. True theoretical yield figures cannot easily be set up because the products are quite complex mixtures, but what are called "Theore tical Conversion Factors as Obtained from Experience", are tabulated on page X-13 below, each crude Aroclor being lumped with its corresponding distilled product, and each month the "Theoretical" requirements of chlorine and Diphenyl are calculated from the month's production figures for the different Aroclors as set out below. See also the letter, E. Mather to L. D. Stuart, June 2, 1947# discussing the origin and use of these "theoretical" factors.(l) Type Aroclor DETERMINATION OF THEORETICAL YIELDS Pounds Aroclor Produced * Diphenyl Required Cl2 Factor Factor To Finish 1148 + 1248 1134 + 1254 1260 1262M 1271 32,683 187,407 97,147 U) 1,800 3,000 0.9664 1.0972 1.20 1.2270 1.4190 0.5304 0.4669 0.4038 0.3930 0.3200 31,587 205,623 116,576 2,209 4,257 TOTAL 322,039 (2000-1800): b 200 ' 322,239 (1262 m: l2L)________ 360,252 Diphenyl Required To Finish 17,336 87,500 39,228 707 960 145,731 (l) Use 90$ of total 1262 mix produced, or 1800#. * From page X-13. DSW 257439 STLCOPCB4061558 X. PLANT OPERATING DATA, contd. X-4 Operating Data Yields, contd. "Standard Conversion Factors" also have been established as set out in the table on pfege X r. -12b, in this case, the crude and the distilled products being taken separately. Each month the "Standard" requirements of chlorine and diphenyl are calculated back from the month's production figure for each crude and distilled Aroclor separately (except that each crude Aroclor is bracketed with its corresponding distilled Aroclor where one is made, and the factor used for each pair is a weighted average of the single factors) as set out in the example below. Type Aroclor DETERMINATION OF STANDARD YIELDS (VI 0--1 1 Produced Factor Diphenyl Factor Cl2 Required Diphenyl Required 1148 + 1248 1154 + 1254 1260 1262M . 1271 32,685 187,407 97,147 (1) 1,800 3,000 1.040 1.181 1.2952 1.5225 1.4995 O.5687 0.5011 0.4575 0.4210 0.5458 33,992 221,528 125,825 2,581 4,499 TOTAL 322,059 588,025 2000 - 1800 = 200 (1262 mix) 522,259 gross total production l) Use 90% of total 1262 mix produced or 1800 18,588 93,910 42,502 758 1,31 156,789 The gross total production is then compared with the "theoretical", "standard", and "actual" consumptions of chlorine and diphenyl, as set out in the example on the following page (X-5). The HC1 production is compared with half the chlorine received, (i. e. used). DSW 257440 STLCOPCB4061559 X. PLANT OPERATING DATA, contd. X-5 Operating Data Yields, contd. Dept. 246 Monthly Inventory 8 A.M. - June 1, 1946 CHLORINE: Theory- 322 360 239 252 B x 100 = 89.45, taken as 100$ Standard 322 239 x 100 388 025 $ 83.05 J|t|- x 100 = 92. Actual 322 239 387 025 * x 100 = 83.26 x 100 = 93.08$ DIPHENYL: TheoryStandard Actual 322 239 b x 100 = 221.12, taken as 100$ 145 731 322 239 156 789 ^ 205.42 x 100 = 205.42, 221.12 92.95% 322 239 x 100 = 206.18, 156 289 * = 93.24$ 100$ HC1; Short tons 100$ HC1 produced Short tons Cle received + 2 x 100 - 898*^394 21x 100 = 93.00 93.00 _ HC1 (36.5) 102.84 x 100 = 90,43 * Note 102-84 *= x 100 b These figures are the totals from page X-3. jrf These figures are the totals from page X-4. * These figures are the totals from page X-7. DSW 257441 STLCOPCB4061560 X. PLANT OPERATING DATA, contd. X-6 Operating Data The combined departmental monthly return covering all Aroclors on one statement is then set up as shown on pages X-7 and 8, and summary sheets are made out comparing the current month with the last three months and with the previous year, and giving a fore cast of production for the next month, as on pages X-lOa, b, c, and d. The Inventory methods in the Pyranol department have no special features. DSW 257442 STLCOPCB4061561 v . X. PLANT OPERATING DATA, contd. X -7 Operating Data MONTHLY STOCK REPORT CRUDE MATERIALS USED May 11, 1946 Cla Cla Gas Liquid Cla Tolu Lime Att. Di ene Earth phenyl 1. No. of Material 2. Stock First of Month 5. Received 4. Total #251 #252 Total #529 6,400# 0# ' 6,400# 400# (i) 575*975 (2) 582,575 4,000 (5) 4,000 379,975 586,573 0 400 #565A #608 #611 (5) 1000# 225# 159,178# 2450 (4) 5450 200 (4) 425 100,000 (6) 259,178 5. Stock Last of Month 6. Difference _ 2,548 (1) 580,025 0 4,000 2,548 584,025 200 200 1500 500 102,889* 1950 125 156,289 7. Required to 2,000 Finish Previous Month - 8. Difference 578,025 0 4,000 2,000 582,025 0 200 9. Required to + 5,000 Finish This Month 10. Total 585,025 0 4,000 5,000 587,025 0 200 150 0 0 1800 125 156,289 100 0 0" 1900 125 156,289 11. Credit _ 12. Net Used 585,025 4,000 587,025 200 1900 125 156,289 15= Per 100 lbs. 118,86 Finished Goods 1.24 120.10 10.00 0.59 0.04 48.50 REMARKS 2 (1) In scrubber liquor. (2) From Dept. 251(Chlorine) (3) From Dept. 252(Chlorine) (4) From Dept. 565(Warehouse) (5) 1178# in scrubber liquor (6) Purchased. DSW 257443 STLCOPCB4061562 X. PLANT OPERATING DATA, conta. MONTHLY STOCK REPORT X -8 Operating Data May 1946 High Boiler Labor Crude Distilled Operating Repair Packing Total 1. No. of Material 618 619 2. Stock First of 0# 0# Month 5. Received 00 0. 0 1150 120 00 150 1400 4. Total 00 1150 120 150 1400 5. Stock Last Month 6. Difference 00 00 0000 1150 120 150 1400 7. Required to _ Finish Previous Month 8. Difference 0 0 0 0 200 0 0 200 950 120 150 1200 9. Required to 0 finish this + month 10. Total 0 0 0 150 0 0 150 1100 120 130 1350 11. Credit 12. Net Used 15. Per 100 Lbs. Finished Goods 0 0 1100 /' 0.54 00 120 130 1350 0.04 0.04 0.42 DSW 257444 STLCOPCB4061563 X. PLANT OPERATING DATA, contd. MONTHLY STOCK REPORT PRODUCTION, Dept. 246 X-9 Operating Data May 1946 1. Products or By-Products 2. Stock Last of Month 2 Delivered to Packing Room or shipped 4. Del'd to 363 Storage 5. Delivered to Departments 6. Total 2, 3, 4 and 5 7. Rec'd from Packing Room 8. Rec'd from 363 Storage 9. Rec'd from Departments 10. Stock first of Month 11. Total 7, 8, 9 and 10 12. Produced 13. Per Cwt. Main Product Aroclor Montar #4 (1) 31,479# 0# 560,385 0 250,131 0 (2) 52,109 0 894,104 0 00 540,000 0 00 (1) 31,865 0 571,865 0 322,239 0 By-Product 100# HC1 0 tons 0 0 (3) 93.00 93.00 0 0 (4)4.66 0 4.66 88.34 (1) Process Goods Stock (2) To Dept. A-246 (Pyranol Dept.) 48,509# To Dept. D-246 (Permasan Dept.) 5,600 Total ........................ 52,109# (3) To Dept,,D-2l8 (Muriatic Acid Dept.)90.00 tons To Dept. 217 (Chiorsulphuric Acid ' Dept.) 3.00 tons 93.00 tons (4) Prom Dept. C-248. (Santolube) DSW 257445 STLCOPCB4061564 X. PLANT OPERATING DATA, contd. MONTHLY STOCK REPORT YIELDS, DEPARTMENT 246 X - 10 Operating Data May 1946 Products or By-Products Yield on chlorine Yield Last Month Standard Yield Theoretical Yield Yield on 6ll Yield Last Month Standard Yield Theoretical Yield Yield on Yield Last Month Standard Yield Theoretical Yield Aroclors 1 HC1 83 c 26 (93.08#) 93:00 (90.43#) 81.93 (92.80#) 92.79 (90.22#) 83.05 (92.85#) 92.56 (90.00#) 89.45 (100.00#) 102.84 (100.00#) 206.18 (93.24#) 208.87 (92.98#) 205.52 (92.95#) 221.12 (100.00# Aroclors. Produced 1148 200# 1248 32,485 1154 300 1254 187,107 1260 97,147 1262M 2,000 1271 3,000 Total..... 322,239 _______________ DSW 257446 STLCOPCB4061565 X. PLANT OPERATING DATA, contd. X - 10a Operating Data SUMMARY OP MONTHLY REPORTS Dept . 246 Production: Products Month: ------- March 1. Aroclors Liquid 2. Aroclor Solid 3. Aroclor Total 4. Muriatic Acid 100$ 400,000# 0 400,000 April 350,000# 0 350,000 May 319,239# 3,000 322,239 Yields: Raw Materials Inventory: Raw Materials 1. Diphenyl 2. Chlorine 3. Chlorine (HC1) 1. Diphenyl 2. Chlorine 94.20$ 94.50 91.00 95.28$ 95.43 90.75 95.24$ 95.08 90.43 150,000# 5,000 220,O0C# 2,000 102,889# 2,348 Process Goods 1. Aroclor 1254 2. Aroclor 1260 3. Aroclor 1271 3,000# 7,500 10,000 25,500# 0 0 0 51,479# 0 Finished Goods 1. Aroclor 2. Muriatic Acid 0 00 0 00 Liquidation Reserve: Raw Materials 1. Diphenyl 2. Chlorine 5,000# 2,000 1,000# 3,000 5,000# 1,000 Process Goods 1. Aroclor 2. Muriatic Acid 0 0 2,631# 00 0 Goods of "No Value": 2. 5. _ ----- __ ------ ----- COMMENTS: (See attached report for detailed remarks0) Signed: Brief Comments Inserted Operating Supt ._________ DSW 257447 STLCOPCB4061566 X. PLANT OPERATING DATA, contd. X - 10b Operating Data Rate of Operation OPERATION REPORT Dept c 246 May 1946 Year Month Liquid Aroclors Solid Aroclor Total Aroclors 100$ by Produce HC1 1945 12 5,400,000# 500,000 5,700,000 2,200.0 tons 1 5 to date 1,500,000# 50,000 1,550,000 500.0 tons 946 April May June Est. 500,000# 519,259# 500,000# 0 5,000 50,000 500,000 522,259 550,000 90.0 tons 88.54 t. l80,,0 t. Brief Comments On; (1) Number of days operated. (2) Reason for rate of production. (5) Reason for estimated rate of production. Crude Materials and Yields Crude Materials/cwt Aroclors Year Month #251 #252 Total Chlorine #611 #6l8 #6179 #565A #529/cwt 1262 mix #608 ' Hours labor pkg. Hours labor oper. Hours labor repair Hours labor total 1945 12 118.0 4.0 122.0 47.2 0.2 0 0.5 11.6 0.05 0.05 0.54 0.02 0.42 1 5 to date- 117.0 5.5 120.5 47.0 0.2 0 0.6 11.0 0.05 0.02 0.52 0.02 0.59 9 April 117.5 4.2 121.7 46.9 0.2 0 0.4 11.5 0.05 0.02 0.58 0.02 0.45 4 May 118.86 1.24 120.10 48.50 0 0 0.59 10.00 0.04 0.04 0.54 0.04 0.42 DSW 257448 STLCOPCB4061567 X. PLANT OPERATING DATA', contd. OPERATION REPORT, Dept. 246 , May 1946, contd 0 Percent Yields (Theory 100$) Year Month Aroclor on Chlorine on #611 100$ by-prod.HCl on Chlorine 1945 ' 12 95.24$ 92,17 94.58 1 5 to date 92.74$ 94.46 95.51 9 April 92.80$ 92.98 97.61 4 May 95.08$ 95.24 90.45 X - 10c Operating Data Brief Comments on Yield. Service Charges/cwt. Aroclor Year Months Steam M lbs. KWH Power KWH Lights KWH Total Comp.Air M Cu.Ft. City Water Cu.Ft. Well Water M Gals . Fuel Gas M Cu.Ft. 1945 12 0.22 2.14 1.00 5.14 5.01 0.11 26.00 0.05 1 5 to date 0.42 5.09 1.40 4.49 0.14 21.90 0.42 O.56 Stocks Stocks as of Warehouse Department ' 5-1-46 552,000 571,000 1, 9 April 0.55 2.40 1.27 5.67 0.10 24.50 0.44 0.05 4 May 0.55 2.47 1.55 4.02 0.11 24.00 0.47 0.42 6-1 -46 100, 000 250, 151 550, 151 000 0 1--t Brief comments on present stock and amount shipped. DSW 257449 STLCOPCB4061568  X. PLANT OPERATING DATA, contd. OPERATION REPORT, Dept. 246, May 1946, contd. Operation X - 10 d Operating Data Brief comments on: (1) Operating difficulties. (2) Operating changes or unusual occurrences. (3) Major repairs. (4) Future changes or major repairs contemplated. Personnel Note changes in personnel. DSW 257450 STLCOPCB4061569 v X. PLANT OPERATING DATA, contd. X - IT Operating Data . The month's yield figure for the Aroclors, as explained above, is a composite one, depending to some extent on the ratios between the different Aroclors made. With this restriction,- the following data give the results for 1946 at the Krummrich plant. Raw Materials Consumption lbs, per 100 lbs, of Aroclor Chlorine Diphenyl Lime Attapulgus Earth 122.22 47.22 0.44 0.02 Toluene 11.67 (lbs.per 100 lbs. 1262 M blend) Crude and distilled high boilers are not included because the amounts used were small. Krummrich plant standards, for 1954 were, per 100 lbs. Aroclor produced: -- 1248 1254 1260 1262 mixture mixture 1260 Diphenyl consumed 56.50 49.75 59.54 58.02 41.78 Chlorine consumed 105.25 117.56 117.21 119.47 151.29 Lime consumed Attapulgus Earth consumed Toluene consumed Muriatic Acid produced 0.50 0.50 0.46 0.46 0.50 0.04 0.04 0.04 0.04 0.04 - 46.55 _ 52.75 1.40 US 1.40 US gallons gallons 52.02 55.60 -- 58.9^ 1262 45.45 128.80 0.50 0.04 57.82 DSW 257451 STLCOPCB4061570 X. PLANT OPERATING DATA, contd. X - 12 Operating Data Krummrich plant standards, per 100 lbs. Aroclor, for 1954, contd. 925,0001bs./month 1,250,000 lbs./month production rate production rate Labour, man hours 1,622 1,622 Steam, lbs. 1,850,000 2,500,000 Electricity KWH 27,800 37,500 Compr.Air,cu.ft. 925,000 1,250,000 City water, U.S.gal. 278,000 376,000 Plant water,cu.ft. 46,300,000 62,500,000 The report "Process Description for Aroclor, Dept. 246", Schwarting and Schwartz, March 15, 1955, gives more recent figures. Yields of Aroclor (as # of the "theoretical figures on page x - 13). On chlorine consumed On diphenyl consumed 93.24# (93.25) 92.17# (9^.73) /The figures in brackets' are for the first 9 (months of 1953. j Yield of HC1 On chlorine consumed 94.58# (90.12) of the "theoretical" figure. DSW 257452 STLCOPCB4061571 X, PLANT OPERATING DATA, contd. X - 12a Operating Data Services Consumed Per 100 lbs. Aroclor (Production at the rate of 356,100 lbs. of solid Aroclor plus 6,753,775 lbs, of liquid Aroclor 7,089,875 lbs. of Aroclor per year.) Steam 1000 lbs. -----------------------------------------------0.228 Power KWH----------------------------------------------------------- 2.l4l Lighting KWH -------------------------------------------------1.003 Comp. Air, 1000 cu.ft. -------------------------------- 0.110 City water, cu.ft. ------------------------------------ 25 ;,990 Well water, 1000 U.S. galls---------------------- 0.464 Fuel gas, 1000 cu.ft. ---------------------------------- 0.049 Labour, man hours See also the report "Process Description for Aroclor, Dept. 246" Schwarting and Schwartz, March 15, 1955, pages17- for more recent figures. DSW 257453 STLCOPCB4061572 X. PLANT OPERATING DATA, contd. X - 12b Operating Data Department 246 Standard Conversion Factors (1946) AROCLOR CHLORINE DIPHENYL DISTILLED CRUDE HIGH BOILER HIGH BOILER 100$ HC1 1142 1148 1154 1160 1162 1168 1169 1170 1171 1242 1248 1254 1260 1262 1262M 1268 1269 1270 1271 2565 4065 4465 5060 5460 0.875 0.992 1.130 1.235 1.253 1.369 1.433 1.505 1.565 0.921 1.044 1.186 1.300 1.327 1.331 1.740 1.828 1.908 1.345 1.320 1.466 1.290 1.573 0.6075 0.5475 0.4825 0.4160 0.4o60 0.3625 0.3450 0.3485 0.6385 0.5765 0.5080 0.4385 0.4267 0.3900 0.4060 0.4100 0.2860 0.2400 0.2667 ---- __ 1.164 0.180 0.418 0.510 0.095 0.3829 0.4341 0.4945 0.5404 0.5485 0.5991 0.6271 0.6586 0.6880 0.4030 0.4568 0.5192 0.5689 0.5809 0.5827 0.7614 0.7999 0.8350 0.5886 0.5776 0.6415 0.5645 0.6883 A somewhat different set of factors, in use in 1953, is given on the following pages X - 13 and 14. Molten diphenyl stocks (at about 90C.) taken at 8 lbs. per U.S. gallon. DSW 257454 STLCOPCB4061573 ` X. PLANT OPERATING DATA, contd. X - 13 ' Operating Data DEPARTMENT 246 - CONVERSION FACTORS Theoretical Factors as Obtained from Experience (1946). AROCLOR 1142-1242 1148-1248 1154-1254 1160-1260 1162-1262 1168-1268 1169-1269 1170-1270 1171-1271 4065-4465 2565 5060-5460 CHLORINE 0.8492 * 0.9664 1.0972 1.2000 1.2270 1.3330 1.3760 1.4190 1.4500 1.2682 1.2950 1.2800 DIPHENYL 0.5874 0.5304 0.4669 0.4038 0.3930 0.3523 0.3314 0.3200 0.3100 0.2303 0.2781 .----- DISTILLED HIGH BOILER 0.457 These factors were still in use in 1953= Aroclors are not pure compounds, but are mixtures of two or more compounds, consequently, they do not have a definite composition, we and for this reason/cannot calculate the theoretical factors. * See the Note by E. Mather marked * on the following page. DSW 257455 STLCOPCB4061574 * X, PLANT OPERATING DATA, contd. DEPARTMENT 246 - CONVERSION FACTORS, contd. X - 14 Operating Data * Note by E, Mather - May 1955 Theoretically 100 lbs. of an Aroclor containing x# of chlorine should give a chlorine conversion factor of 2x 100 and a diphenyl or high boiler conversion factor of Thus l 54,,5x " 5550 % chlorine in Aroclor 42 48 54 60 62 65 68 69 70 71 conversion factor chlorine diphenyl or high boiler 0,,84 0.591 0,96 533 1,08 475 10 20 4l6 1,24 397 1.50 368 1.56 339 1,38 330 1.40 520 1.42 510 By this test the Krummrich plant figures for chlorine for 4065 seems to be impossibly low, and so do the "diphenyl" figures for 4065 and 2565 (taken as representing total hydrocarbon used). DSW 257456 STLCOPCB4061575 X. PLANT OPERATING DATA, contd. X - 15 Operating Dara The # yield figures (on theory) at the Krummrich plant in 1954 for Pyranols, etc. were: 1467 Pyranols 1470 1481 1488 Inerteens PPO PPO-TTCB mix TCB standard actual 1953 TTCB standard actual 1953 99.0# 99.85 - - 98.0 98.81 99.o# 98.51 - 99.0# 99.85 - 99.0# 99.85 - 98.0# 98.81 Aroclor 1254 std. actual 1953 - Aroclor 1260 std. 99.0 actual 1953 99.0 99.0 99.0 99.0 99.0 --- _ 99.0 99.0 - 99.0 99.0 - 99.0 99.0 1 1 1 The consumption figures were Aroclor 1.254 Aroclor 1260 60.60 45.45 75.75 - 60.60 60.60 45.45 TCB TTCB 40.40 - 55.56 25.25 - 4C.40 - 40.40 - 55.56 'TTF 0.128 0.128 - - - - 0 o ro Attapuigus earth Glycidyl ph,, ether 0,02 - - 0OJ 0 0.02 0.02 0.02 t1 - _ 0.220 0.220 DSW 257457 STLCOPCB4061576 X. PLANT OPERATING DATA, contd. X ~ 1.6 Operating Data Labour, man hours Steam, lbs. Electricity, KWH Comp. air. cu.ft. City water Plant water PYRANOLS 956,000 lbs./month 1, 250,000 lbs./month 815 815 278,000 57^,000 5,700 5,000 -- -- -- Figures for earlier years are given by Lyles, Soffranko & Miller, March 24, 1947, pages 51-58. Krummrich Plant records for Aroclors up to 1946 are summarised on the following pages DSW 257458 STLCOPCB4061577 -st av ' rH n CM S-i (D X> O P O o p s o iH *fc CH 11) rH .GVO P.^fc H * 00 rH CM CJ o on st st st o ON OJ O 00 b- bin- o Oo 0 CVJ on on on st st St st s--t t-- i--i b- on c o e OO vo .st st st X - 17 Operating cvj Data CM o st un 00 ON 00 o 0 rH in VO on m b- rH CM st b- rH ON ON VbD- st ON o st on CVJ in vo b- CM on -sa o on CM in rH rH CM CM in CM on rH On CM on oooo t00 On b- rH st in CM 0in0 O on on st st on a in D Lbs on 116 Note 1 0 0 vo inCO in VD ON on b- st st CM o-P rH 00 VO ON CO CO rH 00 00 CM 0o 0 Oo0 o CM\ rH b on On o St on in rH voin c- rH voon CM VO i--i rH rH rH On st r--1 CM on C1--M! CVJ rH CM rH CM rH CM rH &H O rH G) sH o* < <0 .=t -P o VO OO g st st on CM st on in CvOoEh a> ON on VO CM VC rH o in in b-&H to o oo st b- b- in st CM rH o oK X3 E $ oo st CM 00 in ON CM in in b- o< Gl ID 00 ON on CM rH o vo oo vog -P on on ON VO st on vo O COs O. rH in on on b- i--i rH t=> a> rH rH rH CO CO Eh Ke O o vo cino in on inCM, G o o oo in og 0) -P O \c s <<H on in oe ON VO on st CM in rH CM in ON e eee fmb- St 0<6 o E G rH H O -p oo on CM on on on CM b- in st st os G\ C3 CM O fc 3 rH r--i rH H rH o Eh CM o CO O O'") G t> CM p. 9 'O o H o o o orH st VO ON on CO O o 3 CO st rH 00 CM in, St O 00 00 o vo voP-, o* m H ON VO vo b~ ON st coH P -P VO CM 8 --i t-- st on rH a. on on onG1 t-3 H 00 rH CM On o vo in onc on in rH CM M rH rH rH 0) G TO k> p S o CD 0) rP H P G OO rH \ X! =*fc o 00 CM rH on o CM rH in b b- vo0 b-- CM 0 =t ON O st o\ 0in- 00 on o it--n o CM in VO VD VD VD VD ON rH rH 0J CM rH rH rH rH rH rH rH rH rH rH rH rH 03 rH 3 on O CM G Lbs <D=4fc CO 3 oin 00 rH rH CO 00 CM rH O O sa st b- brH 00 00 CM ON O ON crH O rH vo h- CM in -st* on VD VO VO ob0o--- on t-- VD on co ii--ni st ON st t rH in VVoDD o st 0000 on on rH CVOD on st VO CM 00 rH rH VO st CM P a g 3 VD lm on on 00 on ON on C rH st sCMt cn -=t ID VD -st sd- CD Q ID ON On ON ON Q\ ON ON G\ Ov crv Ov rH rH rH rH rH rH rH rH rH rH rH STLCOPCB4061578 =[4-- ON u01 PO -oP o si KM < wQ oec u0) o P n bO \o =*fc KH H00 to & tAC VO in tvc o VCOO Oinv in 0rH0 rH 1 I CO O i Of-ln Cr--Ol ee6oe oo ooo oo o o o CO o =4in in VO o ON rH o VO CVJ iH 0 0 0 o oo CO o pH CVJ P 0) Sa5 E 'o <in ap>vino CTJ =*= M -a >5 to Wp iP in J4- co rH Ch in ON pH ON =4" c- vo rH OJ rH ^4" CVJ ON co ct-o 0in0 CVJ vo On CO in J5j- OO Ooooe 1--1 pH rH oin in CVJ o o o in o c\j 00 oo oin o o o in o -=t CVJ vn oin =4" t-~ On pH OJ in c- co in voo CO VO CO CVJ vo 00 CO CO rH -=f X - 18 Operating Data O CO CNO. L CNJ w <Q CO o e LO l CVJ ooooooooo in =4-1111111:1 in o oin oooooooooo i=nt V.=O4- OJ (<0D| vo CO ON c- 00 CO CO ON ON ON CO .O=4- ON ON rH iC=\Jt <7\ m C\ Q\ in -K=dO" o\ CTs ^1 rH pH 1--t pH pH rH rH rH rH rH rH STLCOPCB4061579 O cto b e r 7, 1947 DSW 2574( -p .CP Ph \?o CO W CO b2o CO o rH 3 arP0 -P < o CO S oo cCoM .C=M*- o oo ON o JS- .=3co CO CM =t CM 1 oOo e o o rH e o oe O o o in rH rH rH oin o rH rH CCVOJ rH CinM .O=N* CtinMco iCCnM- CinM rH CiCnOM CM CO CM oc c- rH X - 19 ' Operating Data -p o <D cQ> On 3 rH CinM a Eoh sfe f-H o K CO W g o r*PQHh) tOH CQ -P \O *4* bO K OrHN TJ 00 ooo cVD O CO CO O ON 0o0 On 00 O \8 o CO CM co tr CM ON ee O o ON rH rH rH t-- C=M? co -=S" CO VO rH .iznt in CM cto.=in1- CO rH in in t- ON CO o CM VO <=t G=f\ zt CO icn- rH CinM 00 zt rH in t- OinN rH -=t ON CM Ocoo rH rH rH o oo o ON CO (H rH 0 oON oo o ON ON c- o o o VO ON o ON 00 t- -i=nt rH in CM CO rH 0 0 cooo oo o rH CM Pi 003) CCOO ON rH cco- CCOO ON rH Oi--n1 COOn On rH ozt ON rH rH sj- ON rH CM =i- ON rH -ctn -=t o^ ON rH rH jijn- ON rH VO ON rH D e p t. 246 Lbs STLCOPCB4061580 X - 20 Operating Data c=J-- on CXU0) -op xP. >R >OR C- CO j3t- 00 vo in ein- oE' in VO coon OE-n cCoO ON oj--i in On V0O0 oOn 0J orH en orH i--i oi--f OONN i--! -=} o1--1 On o OrH t i--! O X p so on COo in in OrH9 OJ O9 in -=t VO9 VO9 i=nc9 oOJe 00 VOo OJ rH rH COON 0O0N COON rH rH rH VOrHO o rH 0J o pH o rH DSW 257462 OEJ- OoJ orH -C=Mt 0CV0J oON 00 00 0O0 -O=Jt O co <U OJ C co rH 00 OrHN rH <J\ rH ON rOHN rH ON OOJn COUN COON 0J On 9 H OJ wtH o rH O p OC \%o =te 0i--Jl V0O0 rH E' OrHN 0oJ C=Mt COM -==frt CO c- o0o- 0EJ- en 00 E- 0- E- V0O- D~0- 0o0 1--l 00 >srH C rH JCHCU>V%0 o p oc \Sos =*= rOHN9 eO-Ne crHoe rH <J\ 0o0 VOOo VrHOe CrHM rH0 O VO0 cOoN OEN 0O0n a=J-\ On COON VOON O=iN- CM ON iOnn oine CrHOo OoN9 .=in3- -=*- sC iinn coo sjvo CO rH CO VCOM 0J CM CO CCMO CCMO CM CCOM CM 0C0M CM oo CCMM riHn CM CrHM CM .V=1O- OJ Pu <D U (CMD >H VO CcO--ONt E' eOrHnN co CO1--ON1 ON o COrHON -St <rHJ\ -t=Ht o\ rH -C=Mt o\ rH 00 .=** rH .st in =t On G\ rH rH VO C\ rH STLCOPCB4061581 O peratin Hours Hrs DSW 257463 hD -t3-cb b fECCCpHtO-i P2toO X - 21 Operating. Dat a. p QJ rO O ft oO $ o rH 00 o=t VO ^4 ibno ba\ on e b- b- Cb CM CO COo iinn CMe oin O MO voo CM CM CMo Cb COo P60 po ft CO H rH K 3 CO O P ft O tPo 2 VO rH O m =t rH VO rH oo oo CM vo CO CM rH CO CO bo=v-t oo Cb b- bo rH CO CO o ft eo O in .=* CM O CO o CM in CO CM rH E--1 CM trH CM CM CM r--1 o ft so bO tPo cw o pto 2O (CXO, pto 2o w s(c0 ft Sos to fPt Kp CO Kf(1t) PCO wo2 V1--O1 CM =t CM CM ov CM in CM -=t oe oe o O o oo c~- cb o oo o CCOb Ot--i 4CM- rh-- 4rH rH CM CM CM so bO I--1 .=4 CO -o=JVD0 .=}mb- CCbOb- CbbCO0 ooCOo CCMO VCOM CM0 CM rH CO CMO in 0CM0 rH CO ft ft P Pc P <D E OP in P Ov co cH ft a> 10 'O ft s: o) s: cO to ft fOt f<tD bO oc C ft GO cC ~ CO Coto OJ CQ O 60 ss o pao> fpt c CD 0a) Eo CO CO rLHP\ rH VC=OM)- VrHO o b- riHn rH CinM -=4 v-rc4Hco- o CoM CrHM CVCOOM <=& CoM rH 00 as cvrHoo o vo voCoM CCCCinMMMb bb 0orH0 rH 4Cop2tS 52 o Q, 0) Q p c<OD vCoO Ct--b1 CbOof--\! CO CO1--OV1 Cb ro cb p O rCHb rH orH\ CM C!--=Jb"1 -C=Of rCHb zt -=4 CrHb rCi=Hn4b vo OrHn T3 XOo>J < STLCOPCB4061582  s w 257464 X - 22 Operating Data t on t~F<Dh &4O3 O m o c o CUL, EoH r-H >iO mw o VOo vo 0 o ONe -i=nt o ONo CoOn 0rH00 00 =iVOe coo o vo0 rH 00o on VO OoJ rH rH 00 oo-- .r=Hjo\ rH roLHTV in oo rtH- On -O=JNOJ 00 0c~-OJ rOoN COOJ OorHJ OJ OJ OOrHn o T3 H 3 CT'O *H rH J rH O rH CO 4c3d U OC Eh cd vo rH rH o =d- CVJ o 00 in in OoJn .o=n* CO n- o vo OJ oOnn vo rH OJ Oin OJ IO--J1 in t- oon On vo rinoi--t m co roHn oino on on 00 =t o 00 =J- o ON on oon =J- =t ,--! t- on Ov C- 00 on 00 o rH -=t -=J- on 'voOn c'--DCOI 0) >1 C "Ho "Uo roH Uo CO i--oI Cf-LH, rH O cd k op < Eh C=~t-- OJ o -=rH 1-1 OJ -O=JN- 0rH0 VrHO VCOti ON rWH oCnO WOJ fOn O uo 4c3d < O Eh 0rH0 -O=Jin o0n- vOrHon OJ iinn oi[*nnvo in .ooOs0=d*nN--- V-O=OJt Fh cd QJ >H VoDn Oi--n( on ON rH 0o0n ON rH ON on On rH ^o=t <T\ rH rH -t 0J -=t C\ CT\ rH rH OO zt -=f o\ CT\ rH rH -l=nt 0\ rH STLCOPCB4061583 X - 23 Operating ts-j" Data ov !--I C'- u v OP ov vrHo o oin ooo o o o o o o o o If) to V o r~iCnM 00 vrHo rH O st OinJ o ioH o oin o OV 00 o 00 SCVtJ 0 0 0 6 oo 5 in a 0J vo rH O . -0i=n0t in st st in s ov in o rH -vsot o o oin o o rH rH rH Ov rH Qow otoa K o vo OOOOCMt'-OOOOO t-- OJ vo Pl. CO KO o o < st in rH rH o o o o o o o in O oo VD aoin\ vCoO CM CooO CM rH om c.=o1- o o st o Oo o ocHind- ooois00tnooo sf rH OJ st rH rH oo in vo CO t00 oonoo\ =iCO rH CM in OV oo t- 00 i--1 .=) rH t-- CinO rH o in CM CO C- CM c- V=Ot" o a\ o O o o o o o o o OJ o vo St 00 -P Oh 01 Q vo CoOv rH nhoCO rH oo CO CiHSV Ov CO -o=t rH st OV o\ <J\ rH rH rH OJ satv rH CO s-=tt C7\ G\ rH rH Sint VC o\ 0\ rH rH STLCOPCB4061584 [*_ =t ctv t- Pl 0) no vOOi--oJi oo .=4=4" vCVoI vCoO =t vCoTv r--1 rH OJ OJ VOOJ ^400 vOoJ O=4J-=J- LO rH o in vo i--i -=4" o 0O0J pH CTV OoJ OJ =* oo rH 00 0- OJ t- O'. OV OfOJ s 0co0 vvoo >o- =4" OV cOoN oino 4* OJ OJ p o O =t CinVI t--i =4" CO in rH COOJ OOJJ oOoN OCTJv pH 00 t00 oCSoV vo OJ vvoo rH o 00 OJ oo -=4" o=4v- voo rH OoJo vooo rH o vo vo C4V"I rH -4" oino t-- oOooJ vo co vo i--t voCooTov O CO -4~ CVJ rH . o o ooo rH OJ vooo oo in oo vooo in OJ O1--O1 oo ov in oo rH O cOoO OV ot-v c~- OJ CVJ oo o cCVoJ in ov c=o4- t- 0o0o =t rH OV O O Wo rH rH to O O K 0-i co K O 4 oo CVJ -4* CVI rH OO -=3" OV in 00 -oo4o- in 00 ocv- o in cv OJ 1--1 00 .=4- Q o vo vo rH CVJ in =4- t-- 00 00 t00 .=4- VinO in rH CVJ =t =4" CVJ OO i--i -=0 t'- OO (K < o o o ooo oo o X - 24 Operating Data DSW 257466 o t- o in ih imn o o o o o o o v-=o4- CVJ aP 0) Q Pi aOJt voCoToV rH ee'n cooo CTV rH Ci--T!v CTv OO CTv rH o -<tJ\ rH rH C4VJ<J\ rH rH m4" *4" av o\ rH rH -i4n* o\ rH v-=ot o\ rH STLCOPCB4061585 O cto b e r 7, 19^7 ^ X - 25 u o -Operating \ " Data o t- oooooooooo 'ax:*-' <u o to <u o -h CU CO "H +3 tfl O "H in o o) o -p .-H QJ O X Ct--Vi QKi OV^)*P<D rH 0)4-3 CO'w' ~ 0 cu iH 4 0 0 c!--uI 0 =t~ 0 CSV OcN^ ON rH on OOON t- oinn t- on ON -O=3N" .--1 ON 0 ti-nV0O cu 0 1--1 C0O CO cu i--1 CO CO ON VcOu .=3cu i-H c- i-H cco- in co rH 00 co ON VO t- VO rH O oew B 00 -=t CT\ in 0 0 ON KoCu, vcou rH rH in st t- CO 0 ON 00 m -si- 0 rH st on rH in 1- co -c=3u- CO oo P*3S3 X ss cu VcOu 0 00 V00O rH OOO in O ccuo -O=!N cin- c=ut COU cr--u1 =t- in 0 .==3t- .=1- in rH vo rH cCoU CCCUUU CinU Ncohm- CM 5tQo cu vc1--ou1 0=t vOoN CO tcou cinu vo rH sCcOt3uU-" rH VO rH CCOU CO -0V0=tO30"- rH Vc0i0nOo cu v0ino rH Oi rH VcCCinOuOO -si- CJ rH -O=** VsOt sSs0r0Httt u cdd> >H vo CO On rH cto- ON rH CO CO O1--N1 ON CO ON rH -Ost- ON rH rH st rH sC\tJ <J\ rH O=Ot Q\ st st G\ rH rH in .=3ON rH VD st o\ rH D e p t,, 246 STLCOPCB4061586 O ctober 7, 194 Hi O oo| ooovooooooo vo o ooo ooo oooooo o vo ln c=oj-ost- rH O VO -c=jo- om CooDoo o X - 26 Operating Data 00 C"birtO-ft CM 5(a/) o voo oo^-ooooooo oin o-=ot- in Q w o & fot CL, eoo in v-=ot o rH tin CoOn iif-nnt ON rH ON C=O*- VO ON rH on ON rH -i=n* rH rH rH o Ko c in o ooooooooo v-oeo- =t o (M in vino CVJ On CM 0=4" in -=t CVJ rH o =r OJ o On on On CO 0- on ON to rn in vo o CM u cfl vooo t- 00 CO OO CT\ o OO .SI rH .=** -CeM- CO -=t in M3 -=J* 0) On On On CT\ ON ON ON ON ON ON ON tH rH rH rH rH rH rH rH rH rH rH rH Depto 246 1 0 0 0 0 7 STLCOPCB4061587 X.___PLANT OPERATING DATA, contd. X - S'7 Operating Data Cost sheets for the Krummrich plant Aroclors Dept, were sent to London, February 1946, and those for Anniston were sent February 24, 1947. Anniston cost sheets for crude Aroclors, distilled Aroclors, and Muriatic Acid for August 1947* as included in the visit report, Mather and Havercroft, September 1947* are repeated on the next 3 pages. In these, all the Aroclors are bulked together; records relating to single Aroclors are put on to "budget sheets" which are really forecasts of cost, the total cost figures being arbitrarily split between the separate Aroclors on the basis of previous experience. (Copies sent to London, see letter Mather to Durgin, May 24, 1945). Copies of the Anniston monthly returns for August 1947* as given in the report of Havercroft and Mather just mentioned, come a little nearer to giving consumptions of materials for each Aroclor; the services consumed are, however, bulked for the whole of the Aroclors. Raw material consumption figures for Anniston in the early part of 1947, are set out on page X-31 below, and the Anniston monthly returns are given on pages X-31 - 36 below. DSW 257469 STLCOPCB4061588 X - 28 Operating Data '' J MONSANTO CHEMICAL COMPANY moduct . i^judx Ar^'^Ly^'i _ U-tc * - n*OOUCTlON-TMII MONTH. _ . + 0%. AATCD CAPACITY _ * OP**ATl_ PCffCCNT TICLO OM PCACCMT YICLD OM_ CO*T REPORT ______________ ^ riAA TO DATX_ *1. tit . coot u**rr_ - OAT* OTWAHU AT_________% or ACTVAt M. * C. INWaTHIKT- Lith OAACKCT le n*<4jC/ J > ^ -4. w a i > > PS ACTUAL OVACTTTT UOOD 3 n a.? ? or- r ouAMTrrr used a 7f 7J"0 7c: a.7 i IMfT ft % 5 OMMM *' > Mimri IMS WAT MM tfM nan M* TA. T Tt dSAol tfAfr/g N9*k^ *`J 5"j. If 3 *.5 '-A . -C ? L 1 * i/ Ilfe-MW -*-L 4 i -a/ 1* III, ,, w 5 a < i rriAM 4 OJCTAKITY COMMUHO Al* *T(A FUKKUID wat** - aanr run, o|. coal. Oil '-'Wls 'C Sm-a p*o/ tatvmimt op PMOOUCTION COST ACTUAL CO*T AMOUNTS INVCNTONT OTANDAND COST VAAIANCC riiMirr unit COOT* TLA* TO OAT* ACTUAL LAST VCAP ACTUAL ----- -y(. i ^r*-. -.-Cc * ft 3 ^----<_ ri t i Ta^J <> g i\CeU.t 0 MTT TOTAL. MAT'L* fTUM ILSCT>ClTY COMPOCSACO Al ATSA- PUIKHUHO WATS* PLANT fun. OAI COAL. OIL i u LAPP*-- MPO 9 *up*pyi*in-mp* i t S S TAX. COMP IN* . P*NSK>NS s PAIN* MIMO* * HPAIPt MUM Vc >gp^.m B LAOOOATOHT CLOTMlAO AMO LAWNDAT PCPPlOCPATIOM A ICI IH CSV 3* l- 1! J 7<r 1 *1 S'? 9S 1T til r t $sr 'f *a Hiy u7 5"t A J 2 da. 3 3f 3' 2 -frl 7 * -*.r/ a r? 3 i^aj 5'06 A i , !. 0,7 a /o.* 5 277 S- J'71 v ^ *- -(/ *q f-3 i-*') Cl j 5 A S* j a =** >* ert `7, S- 7 T* 1 0A - / or <? / 1 A / iO C /M If 1 5a. o/ `A d 0* 09c O 44 -*r It X/ (Cu a/ 2> > Hf f; % LIT wo? 5/ 1*7 >? 7/ >2- id r 7* X7 !,S" Cl *+ >5 * 68 2-7 - )>a Si 37 if - i 7 44 13 9J S"7 17 ~ 3/ 5** kt ?<4 >5 }>(. "t ?// 0*7 0/0 T "?*/ 0 te 0^9 ?l> *f ** T'iAl "'a / ' J av 007 80/ / ST 0* / ^ o/i 'CS3 0 >7 C/T c<?8 0 0 A 1 or 008 *> // 8m-7 Oil OH O V OAT r3P O/p 3<* '0/1 `08X 0<V -?* ^0 1 8 VU 0w ,? Oi * -'3 a" o>a* :7 001 OOZ- - '8/2 IP TO PINIOM OPCAATtOM TOTAL OIPtCT CO**V OtPXICIATMH % COMTPOqAAJ PIC s1 NON-COMTPOLLAOLC -P 1 C TOTAL IMOIACCT COO TOTAL MPO. COOT TOTAL PACK MO COOT rrfii .> F .'is *** 1.3 "7/ *>*- <p% MX 3 A. *r 2M 4/ 9 t*Xl H* 101 4k 2V 1 T*T it A Yu fro -- *n >7 7 -0*0 0 S\ alf *s m ' -MS T'iaOO naO/ 04? orr 1X7 *d4V ov CWC OlO 877 6- >3/ 7JV 24 > OJ7 7ov 'fld -/>* a // 3 >oi ru sw 257470 STLCOPCB4061589 X - 29 Operating Data MONSANTO CHEMICAL COMPANY moduct I *sJ*M*r* asi*-g PMOOOCTIOM-TMIO MOMTH. _ . -5 it Z_ QSlSl.___ MATEO CAPACITY% < PEMCENT YtCLO * - lucent yield on... COST REPORT 6- C* nrr no._ MCMTH. 4--L*-`CCL'-f ------ TIAP TO OATI----- i 4 1 y. 3 9 ? _______ COVT UNIT__ ----------------------------- DAYS OMCMATVD AT______ % OP TANOAM------------fTU*1 M. M. INVUTMMT ____ VTAMOANO------------ACTUAL M. B. '.1 _ MACKET t ,,,/. I#' !+ i-C - 6- 1-0 b - /-J 2 -- " " '*ro5 t i^ii >-*>? - - -a-- Ury-i^+JCLJ '/'.S oT-al , *4 t nq. MANTITT IWO *-4 <"/ 069" -> ** * V 6 42- J* V2JT '7J-* ooqi 9 1 ITUH oectm terry COMMIUU AIM WAT*- miKHAKO MATSU--PLAMT run.--u, coal, oil STATEMENT OP PMOOUCTION COAT z P**.if/j 0 1/ S~'+-* 1 >5 > 5i i gT7w A // 5o < (2-a t i S'**3 ^ -JS^I fry 6!ws< 0 " l<-- 1 *ajU MAT TOTAL MAT'LA fTIAM eLACTWtCrTY CBIIUIMU km AT--PVMHAM9 NATS*--PLANT PUCL--AS COAL. OIL 6 : LAOOn MPA. i SUPSPViSlON--MN i ss A A TAX. COMP. INA . PEMStONS PSPAIPS MWM i MPilDI - MAMA i wiun LAOOMATOMY CLOTHIMO AND LAUMDNT PtPfttOCRATIOM ICC >ij*+ -- jjem. /* # - JSMig COAT AMOUNTS ATAMOAPO COOT i * 6/ VAPIAMCC -- OT\M. UNIT COOTS TCAA ACTUAA. a 5 3* -L 1,07 f-p >/ a or 4 3 * a 7 33 ** f f 7 A i /% /<?a. ' 57 `001 0 9+ LAST ACTUAL 5i Am s .-r 40a J 06 0i 1h *45- cv .47 rt> 32 6^A TA-b 1ST ,i`l - 101 S I-'? 1 7* 7SW Of o 3. > J>l P i<?o *4 < * c ' *4 4* 4 o r n f 3 327 LA 4* 2 A/ fb /Of o-r Ml 7na <3i M-r <1 *l s /I i ^ f A-3 `v* 8 1 J >t aS - (2 3T ~ *7 ' A| >5 3o^. 7 1 lx* li>? (.r ** * 33 .*> A/ o /A . J-pC -fi J*s oaf oa/ (9 AAA 0/0 - (^4*0 O i7 oaf O >A oef OaS - 9/m. fTI 3/ O o if -'A8 *32* 3a;? 5 a;/ ou Oil 3<3 1/3 3. i .* T7 '3tZ 0*3 3.7 BXP. TO PMtEM OSEMATIOM TOTAL 0*ACT COMV OCMPSCIATIOM % COMT*OLL*ELE--P. 1. K 6 NOM-COMTOOLLAELE --P 1 c I Si TOTAL IMDIPECT COMV TOTAL Aft. COOT TOTAL PACRMA COOT r.-u c.r>+ F.e> & <"<vv< til 6/ 3 >2--. -7 li 77 a- ><*<? tp >7 4U AS 4 77 xm Mr ML < *7 Am.a 09 i - q c| f 31 U * _^7 - -t"? - fk e1 - Ya aa 3<? ir i S' _ nn -- at e 48 */ / CS7 2.If . -r. ^ TJf 07 a-o 0Pi. -i JW 04 a. .**7T 3>2 A*#r j T6/ a 3/ j- *3* M* --nsr- / 3 t* / 0; 1>7 =- fss i* a * N o>-> 257471 STLCOPCB4061590 MONSAffTQ CHEMICAL COMPANY mnnri f COST REPORT Ilufu+jCLi hX*. . S >A9 <?4* 3a<? X - 30 Operating Data zTATtMorr or z 0 > oA o z < <3 e 0 u# WT TVTM. HAnj ITtAM uemciTT fmiwfii aw AtW--PIMCMAHO "***" n-nrrr run.--a* com- *. ,, LAW-MM l m t s tax. cew mm . avmmmi j 9AIOV HM* OAlAt- MAJOO s IWI LAO LAODOATOOY CLOTHm* AM> LA4ANMT ZTHWZJtA-nOM * KC ACTUAL COOT MV1NTOAT RANOAIO COOT WAOIANCZ * J >+ =>9 2^3**- 9? r . HHl UNIT Will aoh f -- 1"1 tca TO OAT* ACTUAL LAST VILA * a-115 Uj x a 3~ A `T T aa0' ' /t* <?S 3-.a / d ^5 o: a* 1 J~0 a** / *5 3T '>#- 3t <5" 3^ * X4. i 1 a2 O/f ' 0 3/ nr OCX om9 Au V -"t v7 Y7 13V --o 7 >7 73 1 f3 - T 3 ro -A 7 - 3 wA < >t /W t oC 33 - z** -t * 3 ? 9^ 0>i ocaT - 0->2 J/O >o >3 OOS o.>i- ->^a '' ^ '>V * 3C*T Oif JO O OC7f P/7 J>/7 Ocy 3j - - ->-3" 7JS* ' ^72 3^7- Oof J Of ZXT TT> FM04 aOATW TOTAL OAMCT CflHV OOWCCIATM % cohtwh.1 i>j r. r * m - --.c,, , .-- , t z TOTAL. IZIBK1 COOT nrr-. con TOTAL. MUM COOT o-r f. o. o . T-- a.5"r /* <cT3 fcf *?/ T' *r <? 5T '7* '3 1 <73 'J -rit 33 < 33 A* Sf "*Xa -?/ xxa a*-m -- a / -- SU > - 67 /2 / i- J<r5 /A^o r-i.6 o/t *44 ut 99 V.V0 . o\J ----A* m 3*7 J/2 O Tb -- a-y 3 3-/ J** CSf yil OH o ttT 3f J o 3* iT>2 DSW 257472 STLCOPCB4061591 X - 5: Operating Data X. PLANT OPERATING DATA, contd. Month of Aug,,19^7 % 0 O.98 65.12 33.90 100.00 Per Lb. 0.600 0.472 0.419 Pounds 6,000 396,500 206,400 608,900 6,728 Pounds 3,600 187,200 86,400 Production Aroclor 1142 1148 1154 1160 1162 1164 1168 2565 4065 5042 5060 Crude Aroclor Total !1 " lbs/ChlorDay Raw Materials Used (1) Diphenyl 1142 1148 1154 1160 1162 1164 1168 2565 4065 Pounds 6,000 4,935,373 1,178,200 324,225 258,000 561,600 7,263,396 6,719 Pounds 3,600 2,329,200 493,200 87,750 58,500 --------------------- ---- , Year to Date 1947 % .08 67,95 16,22 4-u6 3.55 7 7k 100,00 Per Lo, ,1 0.600 0.472 0.419 ' 0.271 0.227 1.000 1.110 1.226 6,000 440,000 253,000 (2) Santowax C 2565 29,250 (3) Santowax R 4065 39,000 5042 5060 234,000 (4) Santowax Isomers (5) Chlorine 1142 1148 6,000 1154 5,525,000 1160 1,463,700 1162 1164 1168 2265 4065 . ' 431,000 342,000 5042 5060 692,000 0 ( O 0,151 0.417 i. 0 --' 11119 1.? 4-2 i.3?9 j 1.726 i 1.232 CRUDE AROCLOR REPORT DSW 257473 STLCOPCB4061592 X.___PLANT OPERATING DATA, contd. X 32 Operating Data Month of Aug.1947 Per Lb. Quantity Services Quantity 1.117 680,000 Steam - Lbs. Water - City Cu.Ft. 7,466,000- 0.246 150,000 Water-Recovered,Cu.Ft. 1,512,000 0.064 39,000 Gas - Cu.Ft. 1,234,000 0.008 5,000 Electricity - KWH 100,500 Lbs.M.H. 'lan Hours Labour Man Hours 825 2,859 738 Operating 213 Maintenance 7,571 2,201 Packing 218 Shipping 148 % 100.00 Chlor.Hrs. Operating Time 4,464 Hours-Calendar Chlor.Hrs. 34,992 48.95 51.05 2,185 2,279 107 2,172 Hours - Shut Down Hours-Gross Operated Hours - Delay Hours - Net Operated 8,027 26,965 1,017 25,948 4.70 Delays $6 of Gross Oper. Delays: Out of Chlorine Waiting on Charge Clean Chlorine Lines Clean HC1 Lines 15 8 Clean Circ. Lines Change Cooking Coil 15 169 Change Distributor 10 Change Chlorine Valve 15. 19 Repair Circ. Pump 14 Repair Chlorine Lines 155 70 12 Repair Acid Towers 28 Waiting on Blowing Tank Low Steam Pressure 3 Repair Water Line 27 Miscellaneous 32 Repair HC1 Line 95 152 166 Repair Charging Line 13 Change Water Line 58 Repair Cone Traps 48 Pounds Shipped and Packed 12 Shipped 12 ' Packed Repacked Containers Pounds Containers Used Pounds 40 Gal.Black Steel Used 343,934 40 Gal.Black Destroyed 33 Gal. Fibre Dms-Used " Destroyed 100# Fibre Drums Used 650 " Destroyed Textile Cans - Used 250 " " Destroyed 50 Gal.Galv.Drums 1000 Year *e Date 1947 Per Lb. 1.028 .208 .170 oOlU Lbs. M,H. 959 3,300 1,491 2.102 % 100.00 22.9h 77.06 i 11 I | ; j 74,15 3.77 ; 1 1 1 Pounds 311,080 325,033 1,867 Containers 661 I 7 2 ________2 ..... CRUDE AROCLOR REPORT DSW 257474 STLCOPCB4061593 X. PLANT OPERATING DATA, contd. X - 33 Operating Data Month of Aug.19^7 Pounds Production Aroclor - 1242 Aroclor - 1248 79.25 20.75 450,109 117,868 Aroclor - 1254 Aroclor - 1260 Aroclor - 1262 Aroclor - 1264 Aroclor - 1268 Aroclor - 4465 Aroclor - 5442 100.00 567,977 17,476 Aroclor - 5460 Dist.Aroclor - Total Dist.Aroclor lbs/Still Day % Recovery Pounds Raw Materials Used Aroclor 1142 Aroclor 1148 96.05 98.80 468,598 119,299 Aroclor 1154 Aroclor ll60 Aroclor 1162 Aroclor 1164 Aroclor 1168 Aroclor 4065 Aroclor 5042 Aroclor 5060 Per Pound Quantity Services 1.160 659,000 Steam Lbs. - Water-City,Cu.Ft. 1.144 650,000 Water-Reeov'du.ft. 0.751 427,000 Gas - Cu. Ft. 0.026 15,000 ' Electricity KWH Lbs/M.H. 666 1,995 2,927 10,349 Man Hours 853 285 225 76 Labor Operating Maintenance Packing Shipping Pounds 4,882,430 1,066,967 240,581 11 488,608 6,678,597 19,948 Pounds 5,014,936 1,091,108 259,998 559,601 Quantity 6,856.000 - 6,518,000 4,641,000 82,000 Man Hours 8,103 1,206 1,520 1,074 Year to Date 1947 73.10 15.98 [ 3.60 7.32 100.00 * Recovery 97.36 97.78 92.53 87.31 Per Pound 1.026 - .976 .CIO Lbs/M.H. 824 1 5.538 4,241 5,58C DISTILLED AROCLOR REPORT DSW 257475 STLCOPCB4061594 X. PLANT OPERATING DATA, contd. X - 34 Operating Data Month of Aug.19^7 % 100.00 44.76 55.24 5.11 Still-Hours 1,488 666 822 42 780 - `7 Pounds 567,619 106,599 2 5 27 1 4,999 107.282 " 786.499 655,890 2,580 Containers Pounds 215 106,000 101 59,725 9 970 19 ^ 1,125 . Year to Date 1947 Operating Time Hours-Calendar Still Hours % 11,664 100.00 Hours-Shut Down Gross Hrs. Operated Hours-Delay 2,989 8,675 658 25.63 74.37 Net Hours Operated Delays % of Gross Oper. 8,057 68.90 7.35 Delays: Out of Crude Clean Goosenecks Clean Still 17 62 Change Coil 21 Change Pump Change Cotton 79 15 Change'Coke Drain Scrubber 13 Drain Trap 2 Repair Ejector Wait on Blend.Tank 19 56 Low Steam Pressure 266 Mlsc. InBtall New Steam Jets Shipped and Packed ^5 32 Poundb Shipped Aroclor 1242 1248 1254 1,500 4,603,798 1260 948,895 1262 1264 1268 4465 5442 5460 Total Packed - Total Repacked Containers Used . Pounds 1,627 99,893 607 389,371 5,992,bbl 6,445,898 17,644 Containers Drums: 55 Gal.Galv.Locktop Used " Destroyed 40 Gal.Galv.Bung Used 254,252 " Destroyed 470 C 50 Gal.Galv.Bung Used 1,333,930 " Destroyed 2,288 50 Gal.Galv.Used " Destroyed ' 53 Gal.Fibre-Used " Destroyed 467,115 150 939 33 1 100# Fibre-Used 3,960 38 " " Destroyed Slack Barrels-Used H Destroyed 7,268 30 Textile Cans-Used Destroyed 3,8S6, #4 5 490,520 1 106,000 Paper Liners-Used " " Destroyed Tank Cars (1254) Tank Cars (1260) 5,364,800 942,315 1 J.4 9j DISTILLED AROCLOR DSW 257476 STLCOPCB4061595 x - 35 Operating Data X. PLANT OPERATING DATA, contd. - Month of Aug.1947 Pounds Production 19,311 Muriatic Acid - Total Pounds Day % Recovery Pounds Raw Materials Used Anhydrous HC1 -Equiv.l8Be Acid -Equiv.20Be Acid 100.00 17,1^3 Per Pound Quantity Muriatic Acid, 20Be Services Water City - Cu. Pt. Water Recovered-Cu.Pt. Electricity - KWH Lbs.M.H. 1,207 Man Hours 16 Labor Man Hours - Operating Man Hours - Maintenance 568 34 Man Hours - Packing 1,315 * 12 Man Hours - Shipping Tower-Hrs . Operating Time Hours - Calendar Hours-Shut Down Gross Hours Operated Hours - Delay Net Hours Operated Delays % of Gross Oper. Delays: Out of Chlorine Clean Acid Lines Clean HC1 Lines Repair Acid Lines Repair HC1 Lines Repair Vent Lines Repair Drowning Tower Repair Absorber . Repair Coke Scrubber Work on Chlorinators Storage Pull Pounds Used and Wasted Used in 18 Be'Acid Used in A1C13 Wasted Pounds Shipped and Packed , 15,777 19,311 Containers Pounds Shipped Packed. Containers Used Tank Cars - Monsanto Tank Cars - Foreign 138 15,732 Carboys "A" - Used Carboys "A" destroyed Carboys - Stranger Pounds Year to Date 1947 Pounds 174,610 % Recovery 155,009 Quantity 100.00 Per Pound Man Hours 75 24 650 37 Tower Hrs,, Lbs.M.H. 2,328 7,275 268 4,695 % Pounds Pounds 74,700 99,522 co Pounds 173,698 174,040 Containers ]_ 1j! 1 1 i | MURIATIC ACID 18 Be REPORT DSW 257477 STLCOPCB4061596 PLANT OPERATING DATA, contd, X - 36 Operating Data ' Month of Aug.1947 Pounds 993,329 63,066 % Recovery Pounds 349,000 90.37 Per Pound 1,099,213 89,960 Quantity O.58O 576,000 Lbs.M.H. 4,415 41,389 36,324 28,707 i 100.00 47.85 52,15 0.026 Man Hours 225 24 26 24 Tower-Hrs. 744 356 388 10 378 4 4 Pounds 17,143 107,458 Pounds 688,976 944,436 Containers 10 154 2 Pounds 671,420 17,556 Production Muriatic Acid - Total Pounds Day Raw Materials Used Pounds Anhydrous HC1 4,228,850 -Equiv.l8Be1 Acid -Equlv. 20Be Acid 13,334,941 Muriatic Acid, 28 Be1 Limestone 640,160 Services Quantity Water City - Cu.Ft. 292,000 Water Recovered-Cu.ft. 6,572,000 Electricity - KWH Labor Man Hours Man Hours - Operating 2,847 Man Hours-Maintenance 274 Man Hours-Packing 319 Man Hours-Shipping 180 Operating Time Tower Hrs. Hours - Calendar 5,832 Hours-Shut Down Gross Hours Operated 1,191 4,641 Hours - Delay 401 Net Hours Operated 4,240 Delays # of Gross Oper Delays: Out of Chlorine Clean Acid Lines Clean HC1 Lines Repair Acid Lines 13 Repair HC1 Lines 10 Repair Vent Lines Repair Drowning Tower Repair Absorber 360 Repair Coke Scrubber Work on Chlorinators 14 Storage Pull Used and Wasted Used in 18 Be' Acid Used in A1C13 Wasted Shipped and Packed Shipped Packed ' Containers Used Pounds Tank Cars - Monsanto 6,187,314 Tank Cars - Foreign 1,695,570 Carboys ''A'' Used 80,612 Carboys "A" destroyed Carboys - Stranger MURIATIC ACID 20 Be' Report Year to Date 1947 Pounds 8,529,464 48,282 % Recovery 63.96 1 Per Pound 0.034 0.771 Lbs. M.H, 2,996 31,129 25,595 44,241 * 100.00 20.42 79.58 , 72.70 8.64 i Pounds 155,009 i ! 4,801,323 | Pounds i 7,963,458 : 8,164,674 ; Containers; 91 23 708 nQlrt/ nr-,, STLCOPCB4061597 to c t*- *"* m" tn <3 1 V 4* v a X OQ ' 4b> a VO4 Ec 0) -p "g O > c 3b KC e> J? o >c G O`Bt IK 1 in in in m m m mm Ohmh- CM 5w o cUouoo W CD 4 o W CD js- in vo \o ^o vo in \in> CVJ in \oo ja- ocvj Ej- \o oo in in STLCOPCB4061598 X. PLANT OPERATING DATA, contd. X - ;,3 Operating Data. Mr. J. E. Crouch, in a letter dated May 18, 1955a shows that the theoretical figures for chlorine consumption at Anniston are on a different basis from those given on page X-3 above for the Krummrich plant. As an example of the Anniston methods? Aroclor 1268 should contain 68# of chlorine, therefore at theoretical yield 100 lb. of Aroclor should be made from 2 x 68 = 136 lbs. of chlorine. The theoretical yield on chlorine, therefore, should be 100 x 100 136 75.5# The Krummrich plant Theoretical Conversion Factors obtained from Experience are a little different in most cases. The Anniston Production Standards for 1955 for Aroclors per 100 lbs. product are: lbs. Diphenyl lbs. Chlorine 1221 1232 1242 1254 1260 1262 1268 86.1 74.1 63.20 49.20 43.70 41.70 50.1 46 70 92.10 115.20 127.8 133.50 165.8 Santowax C Santowax R 2565* 44655460 5442 1248 28.60 26.10 -- 55.0 . 132 151.5 148.20 104.5 101.5 9.50 -- ' -- -= 17.40 50.2 69.2 *Mr. J. E. this page) amounts of available,, Crouch in his letter of May 18, suggests that this figure is 2365 -ad been made at Anniston, rhe 1955(mentioned ar/top of rather low. only small so good data were not DSW 257480 STLCOPCB4061599 X - 39 Operating Data X. PLANT OPERATING DATA, contd. Anniston The/standards for utilities, services, Aroclors, as follows: etc, are grouped for all the Crude Aroclors: Steam 106 lb./lOO lb. crude Aroclor Electricity 1.21 K.W.H. Plant Water 18.69 cu. ft. Fuel 11.84 cu. ft. (natural gas) Laboratory 0.01 unit Labour 0.06 man hour Maintenance 12$f Supplies 14 Distilled Aroclors (from Crude): Steam 109.5 lb. per 100 lbs. distilled Aroclor. Electricity O.69 K. W. H. Plant Water 76.95 cu. ft. Fuel 67.09 cu. ft. (natural gas) Laboratory 0.1 unit (4^) Labour 0.1 man hour Repairs 8^ Supplies 2^ Mr. Ellenburg, January 20, 1948, gave 0.66 cu. ft. gas/lb, Aroclors the gas being about 1060 B.t.u./cu.ft. DSW 257481 STLCOPCB4061600 XI - 1 Hazards XI. HAZARDS. Toxicity There are many literature references*to harmful effects of the type of "chlor acne" resulting from exposure to chlorinated diphenyls* especially in cases where people working with small electrical com ponents have been exposed to the fumes of hot, highly chlorinated, Aroclors. Chlor acne is sometimes accompanied by gastric troubles, and there are literature references to liver troubles. There was some trouble of this kind among the production workers at Anniston in the early days of the development of the Aroclors. At that time highly chlorinated Aroclors were being made from diphenyl which had come from low grade benzene. Since good benzene has been used, the same Aroclors have been made without trouble. In March 1955 it was reported that the Anniston diphenyl and Aroclor plants had run 12 years without lost time accident. Prom the start of Aroclor manufacture at the Krummrich plant the operators have been supplied a clean change of clothes every day, and time has been allowed at the end of the shift for bathing. Operators are advised to wash hands and face before eating. The Anniston operators do not have the same issue of clean clothes. * Percy May, "Chemistry of Synthetic Drugs" , 3rd edition, page 19, The "Chemist Analyst", September 19^7, Volume 36, No.2 page 33, and a report by Dr. M. C. Lester, Anniston plant, 1937, give data on the toxicity of diphenyl. ,(new edition) ,, MCC Bulletin P-ll^/mentions 0.5 to 1.0 mg. per cbm in air as the highest safe concentration of higher Aroclors, and 10 ng. for more highly chlorinated Aroclors. H. B. Edkins "Chemistry of Industrial Toxicology", page 1^9 gives 0.5 to 1.0 mg. as the allowable limit in working rooms. The MCC Bulletin "Physical Properties of Aroclors" mentions sys temic effects arising from the oral injection of Aroclors. See the letters, E. Mather to P.J.C.Haywood, December 17, 1957, and Mather to Newman, January 8, 1952, reviewing the literature on the toxicity of Aroclors. See also correspondence relating to the article in Chem. & Eng. News May 17, 195^> pages 2038 page VI-3t above. and the warning labels mentioned on 6 DSW 2574ti2 STLCOPCB4061601 'V HAZARDS, contd. . XI - 2 Hazards XH St. Louis, Main Office Mr. P. J. C. Haywood Newport (Airmail) cc: Mr. W. E. Hamer, Ruabon Mr. W. H. Ritchie, Ruabon Dr. H. R. Newman, Ruabon Mr. S. M. Kulifay, Krummrich Dr. D. S. Weddell, St. Louis Mr. F. T. Marshall, St. Louis December 11, 1951 AROCLORS::TOXICITY Since writing to you on December 3rd I have come across a letter of mine to Mr. W. M. Cooper, London, June 24, 1948, (copies to W.D.S., W.H.G., and others), calling attention to an article in the J. T. Baker Company's "Chemist Analyst", Volume 26, No. 2, page 33, September 1947. . I attach a copy of this article, and I think you will agree that the warning relates only to really bad exposure, not such as should occur in ordinary analytical work. On October 27, 1947 Mr. Barbre of the Krummrich plant sent a copy of the Journal to Dr. Jenkins at Anniston for comment. Dr. Jenkins did not make any comments at the time, but the following extract from Mr. Barbre's letter is inter esting s "During the 11 years of production here only one man evidenced dermatitis. He had also shown similar symptoms in several other departments. When making Aroclor #1270 which is flaked, a noticeable amount of fine fume solidifies in the air. If men are exposed to it during hot humid weather, the skin is irritated, but we have not had any difficulty in curing cases of dermatitis from it". . DSW, E. Mather STLCOPCB4061602 XI -__ HAZARDS, contd. XI - 5 Hazards The Chemist Analyst, Vol. 36, No. 2, page 35, J. T. Baker Chemical Co., Phillipsburg, N. J. September 19^7 ON THE TOXICITY OF THE "AROCHLORS" (sic) Robert M. Brown, Chief Industrial Hygiene Section, Division of Health Dept, of Public Welfare, City of St.Louis, Mo. A recently published article (Maglio, M. Martin, Chemist Analyst, 35 94. (1946) ), has recommended the substitution of one of the "Arochlors" as the melting-point bath liquid in preference to the customary sulphuric acid. As stated in that article "Arochlors" are a group of chlorinated diphenyls produced by the Monsanto Chemical Company. There is need therefore to give warning. For the toxicity of these compounds has been repeatedly demonstrated, both from the standpoints of their absorption from the inspired air, as well as from their effects in produ c.ing a serious and disfiguring dermatitis when allowed to remain in contact with the skin. Since these effects have been repeatedly observed, industrial hygienists have taken care to see that the proper controls have been established wherever these products are used. For example, the maximum allowable concentration of chlorinated diphenyl for an 8-hour working day is 1 milligram per cubic meter of air. It is probable that nothing like an uncontrolled industrial expo sure will occur in the laboratory. However, whether an individual is subjected to a possible acute exposure to chlorinated diphenyl, and its serious consequences, will depend upon the size of the melting-point bath, the caution with which it is used, and the temperature to which it may be heated. Likewise, with careless handling of the material and the resulting contamination of the skin, clothing, laboratory towels, work table surfaces, etc. the way is left open for the producing of dermatitis. Scrupulous cleanliness must be insisted upon wherever this material Is handled. The foregoing remarks have been prompted by the belief that in re commending the use of a material with which is associated a potential hazard from the health standpoint, it is very important that the possible consequences be presented together recommendations for correct handling. DSW 257484 STLCOPCB4061603 XI. HAZARDS, contd. XI - 4 Hazards Mr. A. C. W. Pennington of Newport, reporting on his American tour, December 29, 1950, page 5 writes: "HEALTH AND SAFETY": "At Anniston, no special protective clothing is provided for the Diphenyl and Aroclors operators. A daily change of clothing was provided in the past but this practice ceased before the war. Gauntlet leather gloves and face shields are, of course, available as required on the plant. " Tins of cold cream ointment, theatrical quality, are to hand in the building, but the application of the cream is left to the operators decision of the job in question. The men are expected to take a bath, in their own time, at the end of the shift. A good quality soap, and alcohol for rubbing down purposes, are provided. The operators are sufficiently trained in the need for personal cleanliness that a record of bath taking is not warranted. "Emergency showers are provided on each floor of the Diphenyl building and safety notices are widely used. "At St. Louis, Plant B, the Aroclors building is rated a toxic department. Each operator is provided with a complete set of clothing comprising hat, coat, trousers, combination under clothes, socks and rubber shoes. A clean change of clothing, except shoes, is placed in the operator's locker in time for the following shift. Men working extra shifts are given a clean set of clothing. Canvas gloves and goggles are provided and 'Ply' hand barrier cream is available for use when necessary. "Twenty minutes' paid time is allotted for bathing at the end of the shift but,- again, no record is kept that baths are actually taken. Theoretically, food is not allowed to be eaten within the Aroclors building. Instructions are issued that hands and face should be washed well before eating. "Employees in toxic departments are given an annual medical examination and a lung X-ray every three years." DSW 257485 STLCOPCB4061604 XI - 5 Hazards XI. HAZARDS, contd. Toxicity, contd. A good deal of work has been done on determination of the vapour pressure of the Aroclors, and on the determination of./concentration of Aroclors in air. See pages 9-, Section III, above, for a summary of this work. In 1950 (letter April 20, N. F. Rapps to E. Mather) the Admiralty expressed interest in the determination of micro-quantities of Aroclors. MCC have a method for the determination of traces in air by means of the "Halidometer". ' Mr. Ellenburg, March 15, 195^, mentions work done by H. B. Richards Jr., of MCC, June 17, 1955, on the determination of the concentration of Aroclors in air. Mr. Ellenburg also states: "------------- work on the safe limits of Aroclor vapour concen tration in air is being carried on by the Medical Department at the Kettering Laboratories in Cincinnati. This work on animals is well under way, and will help us to know a iittle better just what is the safe limit of Aroclor Vapours that one might work in." A question has been asked about the possible harm to plants if Aroclorcontaining paints are used in greenhouses. The reply is that most paints are somewhat harmful, and there is no evidence that Aroclors make them worse. Aroclors have been used as rabbit repellants, with out doing any harm to vegetation. Care is needed in laboratories etc. where Aroclors are used in heating baths; there should be very positive ventilation. The vapours of hot Aroclors are distinctly irritating to eyes and nose above a concentration of about 3 mg per cbm in air. Newport plant report for December 1951 records burns by hot Aroclor -- a case of a splash into a man's eye -- without serious damage. Packages of Aroclors leaving the Krummrich plant bear a label calling attention to possible toxic effects. DSW 257486 STLCOPCB4061605 XI - 6 Hazards XI. HAZARDS, contd. Fire Hazards Diphenyl, of course, will burn, and reasonable care is needed in handling it. Precautions with toluene are mentioned also on pages VI-29, and under "Special Risks", below. . The Aroclors are handled as if non-inflammable. Drums of material are melted in the middle of the operating building, by open gas flames, and open gas flames are freely used to heat pipe lines. An instruction, dated April 28, 19^8, calls for a daily Inspection of safety showers, fire extinguishers and gas masks, a check list being provided. Flanged joints on Aroclor heating system can be a source of fume. See the notes on gaskets, page 2, Section XII, below. Phosgene may be generated in electrical flashes and fires in trans formers containing Aroclors, but this is not thought to be a major risk. Safety Equipment Each operator in the Krummrich Aroclor plant is supplied with goggles, rubber covered gloves, canvas gloves, rubber shoes and fume respirator. See also page XI-1. A spare suit of clothes is kept in a case in the department. The department has the usual first aid cabinet, gas masks, (chlorine), fire extinguisher, (toluene, diphenyl), stretcher, safety showers, drinking fountain, eye bath. Special Risks The usual care is necessary in dealing with chlorine, in lighting the gas furnaces, and in handling hot materials, steam lines etc. Diphenyl might start to burn in chlorine gas if conditions in the chlorinator were badly out of line. A Davis "Vapotester", model M-l, Type A, (Division of Davis Emergency Equipment Co., Inc., Newark, N.J.) is held in the department for use in testing the air of the working building after toluene has been used, and for testing vessels before men are permitted to enter, and before "flame certificates" are given. The instrument contains a DSW 257487 STLCOPCB4061606 _. XI - 7 Hazards XI. HAZARDS, contd. Special Risks, contd. catalytic cell electrically heated to a fixed temperature, and the air to be tested is aspirated through it by means of a "squeeze ball". If combustible vapours are present, the temperature of the cell rises, and the indicating thermocouple registers on a cali brated scale. The instrument has a zero adjustment, and it is checked twice a month by the instrument department. Flame certificates must give the number of the Vapotester used, also the data of its last cali bration by the instrument department. The instrument has been use ful in detecting gas escapes, and in tracing spills of gasoline, etc., from a neighbouring oil refinery into a public sewer which runs under Monsanto territory. Mr. Benignus, of St. Louis, September 1955, discussed the dangers of using Aroclors in indoor paints. He discounted the possible dangers from phosgene formed by flash discharges in transformers charged with Aroclors. See the references to safe handling of glycidyl phenyl ether on pages IX-161 etc. DSW 257488 STLCOPCB4061607 .* XII. EQUIPMENT LIST XII - 1 Equipment List The following details are largely drawn from pages 18 - of the report by Lyles, Soffranko and Becker, November 19^6, and they relate to the plant "B" (now Krummrlch Plant) equipment, unless otherwise stated. A list of Aroclor equipment at the Anniston plant was sent to MCL June 7> 19^6. . General Note Since diphenyl and some of the Aroclors become solid, or viscous, at ordinary temperature, attention has to be paid to steam tracing or jacketing of pipe lines, and to the provision of gas flames for local heating where necessary. With due care, because of the presence of diphenyl and in some cases of toluene and butyl ace tate, naked flames are quite freely used in the plant. (See oper ating instructions. Section XV, below). Pipelines used for Aroclors need heat insulation, also proper allowance for expansion where high temperatures are involved. Flanged crosses are freely used to assist in locating and clearing blockages in the pipe lines. Lines for diphenyl and heavy Aroclors should be blown clear after use. This also refers to outdoor water and steam lines, for example rail tank coils, in cold weather at the Krummrlch plant. Schwarting and others, "Process Description -- for Aroclors" November 12, 1953, page 5 state "Since iron has a deleterious effect on Aroclor electrical properties, the distilled product is handled in monel, monel-clad, zinc or tin-sprayed, and 504 stainless equipment. Galvanized iron or stainless steel is used for the process piping beyond the distillation stage--------- ", DSW 257489 STLCOPCB4061608 ` XII. EQUIPMENT LIST, contd. . XII - 2 Equipment List Gaskets and Packings The following gaskets have been found suitable for use in the Aroclor process(l948); #901 Garlock - 1/16" 1" - l|" - 2" - 5" and 4". Used for all crude material transfer lines. #900 - Yellow Garlock l/8"and 1/16'.', sheet Gasket. Used for finished material transfer lines. Metallic Asbestos Goetze gaskets 1" - 2" and 2". Used for solid Aroclor line flanges; will stand heat. Goetze Aluminium Asbestos. 16" I.D. 21^" I.D. and 9" I.D. Used for Pyranol Car heads. Goetze Metallic Asbestos 2" flange gaskets used inside, top and bottom of 18" sparkler press. #262. 1/2"x 3/8" square Garlock gasket. Used in flange face of Sweetland press. Gum rubber flange gaskets used in HC1 valves and lines. #900 Garlock gaskets used on all Chlorine flanges, tank manhole .covers, inspection plates, inspection plates, and between all pump and tank flange connections. Gum or Garlock red rubber gasket material used on all HC1 tank flange connections. Samples of Goetze corrugated copper-asbestos gaskets were sent to MCL, April 9, 1947, and again June 24, 1948. The 2" I.D. x 4" gaskets at that time cost .f 0.189 each. SVV 257490 STLCOPCB4061609 XII. EQUIPMENT LIST, contd. XII - 5 Equipment List Gaskets and Packings, contd. See also the London Engineering Dept. Final Report on the start-up of the Newport plant, for a discussion of gland packings for use against hot Aroclors. ' See also MCL Research reports on packings and gaskets for hydraulic fluids, for example: -- 547 50/175/2 November 1950 555E 51/91/1- August 1951 1151 DF 54/26/5- June 1954 - DF 54/27/1- April 1954 - 1152 DF 54/16/5 April 1955 Some gaskets failed under test, others damaged the goods. Samples of the washers used for the bungs on Aroclor drums were sent to MCL, April 9, 1947. The 1" size cost $0,004 each. DSVV 257491 STLCOPCB4061610 XII. EQUIPMENT LIST, contd. XII - 4 Equipment List PUMP PACKING LIST EQUIP.NO. PUMPS P-0629 " 578 " 579 " 1056 " 751 " 575 " 604 " 575 " 574 " 580 " 1509 " 594 " 1277 " 565 " 1258 " 578 " 1054 " 1260 " 585 " 592 " 584 " 585 " 929 " 617 ' SERVICE #1 Chlor Pump #2 " " , #5 " #4 " " " #1 Scrubber Pump #2 " " #5 " #4 " " " #1A " " #1 Blow Tank Pump #2 hi u 1 ' " #lj.'Stlll' Pump-- . 2 - t. - 11 Re e . Pump #2 11 n " City Water-Pump to Tourrill " " " " Tantalum 18" Sparkler Press. Pump 18" " Head Gasket #1 Diphenyl Stg.Tk. Pump ^2 M nM n #5 Aroclor Stg. Tank Pump it n m 11 ^ n 11 11 11 CT0347 - Diphenyl Stg. Pump SIZE PACK. 5/16 inch It If . It 3/8 tt It II II 5/16 II 1/2 H 3/8 II 1/8 II 3/i6 1/2 x 5/8 1/2 II 1! II II 3/8 TYPE AND NO. OP PACKING #254 Garlock 1! 11 II It II 11 II It II tt 11 It II 11 It n 11 11 it it 11 11 tt Palmetto 11 #117 Garlock II II II tt #262 #254 V M II tt " " II II 11 It Palmetto P-0595 P-0427 P-0945 P-01119 P-0725 P-0346 P-01111 Plaker Drum 1170 Stg. Pot Agitator #1 Still Condenser Pump D 218 Dept. Inhibitor Acid Pump Wilfley Pump at #1 HCL Stg. " " " HC1 Tr.Tk. Dept. A-246 #7 Sweetland & GE Press Pump #6 Stg. Tank Pump TCB Unloading Pump 1/2 3/4 1/8 1/4 -- 3/8" -- #534 Gar-look #254 Garlock #117 Garlock #254 Garlock: Do not use pckg. II II II II Cutno or Palmetto No Pckg. r-eq`d. -- Palmetto \ 00 DSW 257492 STLCOPCB4061611 .v XII. EQUIPMENT LIST, contd. Cocks and Valves XII - 5 Equipment List A 2" Crane all Iron Gate Valve #475| Durimet Stems. New Style 2" Merco cock - Cast Iron) 2 ii ii ii ii ii j Powell, Rising Stem flanged 1^" Stainless Steel Valves. Clip gate valves. Brass or all iron. Barstock Needle Valves. 5" Crane #475^ New Style with Durimet stems. For all 2" Chlorine lines. For all crude Aroclor lines. Blow Tanks, chlorinators, scrubbers. For all finished Aroclor lines, also for all Pyranol lines. For all city water lines. On all Manometers for chlorine and vacuum. On all HC1 off gas lines between scrubbers and HC1 absorbers. NOTEi Mr. D. G. Furzey, December 5, 1951, reported that cast steel valves were used throughout for the hot process liquors. Merco lubricated cocks with special high temperature grease are widely used. Monel or bronze valves, or cocks,, are used wherever their use appears to be desirable. See also the note on the use of Teflon lined cocks for chlorine at the Anniston plant, page 3, Section VI, above. DSW 257493 STLCOPCB4061612 -" XII. EQUIPMENT LIST, contd. XII-6 Equipment List B-054-0148 Blowers B-054 Blower from American Blower Company. Type 5V. Used to exhaust fumes from around the Pyranol filter press, P-0159 On roof of CR. Motor M-01752. B-094 Blower from American Blower Corp. Serial #5364. Print G-46215. #50-CCW-BHD-FH type E fan with LS wheel. Welded steel pedestal for motor. Drive thru couplings. Clockwise rotation, horizontal bottom discharge. Order B7377 on 4/14/56, Req. 69122 on 4/14/56. Price $104.21. Driven by M-0852-5HP-1220 RPM In lean-to on second level platform. On flaker D-012. B-0105 Clarage Blower purchased from Anniston. Pan #47561, Type Cl #7 with outboard sleeve bearing."V" belt drive to M-0904.Used with cyclone CT-O852. On platform in lean-to. Driven by M-0904. On flaker D-012. B-0148 " Blower from American Blower Co. Size #1-5/4 Sirocco utility blower. Direct connected counter clockwise up blast discharge. Includes supports of steel. Order B1776 on 1/22/40, Req. 5788 on 1/22/40 Charged out $154.55 on 5/29/40. At CT-0765, Bldg. CR. Direct connected to M-01710. On melter and still tapping drums. All blowers are of ordinary steel construction (EM, March 10, 1947). Drawing D-6945 shows the fume exhaust system at plant "B". DSW 257494 STLCOPCB4061613 XII. EQUIPMENT LIST, contd. XII - 7 Equipment List CT-0347 - 0744 Closed Tanks CT-0347 Tank 401 dia. x 161 3i" high, 1st course 1/2" metal, 2nd course 3/8" top sheet - 2-6" Cl nozzles on bottom, 4-4" Cl noz. on top. 1-20" Cl manhole on side shell near bottom, 1-20" th. steel hatch on roof. May 1927. Drawgs. D-978 and C-1117 (tank and foundations) (diphenyl store). CT-0745 Jacketed vaporizer. 2 parallel vertical 10" dia. x 4'4" tanks surrounded by a 2'0" ID x 4'0" jacket. Use XHy pipe - jacket of plate, Drwg. C-818. Order B9038 on 5/6/36, Req. 69670. Price $180.00. 2nd floor 12' level south side Bldg. CR. CT-0744 Middle chlor. tank made by Nooter. 3' ID x 161 lg. with fig. head, shell 3/8" and head 7/16" thick, 3/16" jacket over lower half of tank. 3/16" inner shell and 2 sets of 1" xLy pipe coils. Order B9037 on 5/6/36, Req. 69669. Price $716.00. Same as CT0745. In 1947 there were four chlorinators In use, CT-0744, -0745, -0833 and -01283, all essentially similar, and later CT-01432 was installed, only slightly different. Each chlorinator is a vertical steel vessel 3'0" ID, l6'0" high on the straight side, with bulged bottom and flanged cover. Drawings E 880, E 6209. Relief connection drawing C-822. Chlorine inlet, drawing B 659. The body of each chlorinator has the following fittings; -- 1. A jacket for water and steam, starting about 18" up the straight side and ending below the level of the charge. This arrangement leaves the bottom of the vessel available for flame heating, and it leaves room for a simple manlid low down on the straight side, for the chlorine inlet fitting described below. There is a spiral baffle In the jacket space, to increase the cooling effect, but the baffles favoured the accumulation of mud in the jackets, and at the DSW 257495 STLCOPCB4061614 XII. EQUIPMENT LIST, contd. XII - 8 Equipment List CT-0744 Closed Tanks, contd. CT-0744, contd. 1. contd. overhaul in November 1948 most of the spiral was removed, leaving only enough to preserve the spacing between jacket and liner. It was also planned to put two 4" nozzles, low down on the Jacket, to facilitate cleaning. City water is used rather than well water, and the jackets are cleaned occasionally by means of inhibited acid. The used cooling water goes to a collecting drum CT-0752. There does not appear to be any trouble from flashing of water into steam in the jacket, in spite of the high temperatures used. Seef however, the note below on the bursting of a jacket due to trapping of water in it at high temperature. The walls of the chlorinators, above the Jackets, are thermally insulated, partly for safety and partly ' to keep down the temperature of the building. 2. Formerly (but now abandoned at the Krummrich plant . except In the new chlorinator CT-01422) an internal coil for steam and water. 3. An Internal cylinder, about 24" ID, with perforated bottom, and a retaining grid on the top* containing about 8' depth of iron-turnings. See page 1* Section VII, above, for a description of the turnings. 4. A bottom outlet, with cock, to the circulating pump, P-0578 etc. Also formerly, from No. 1 chlorinator, to the gas heated chlorinator CT-O808, used for. making the higher Aroclors. A piece of heavy gauze is placed over the outlet to retain stray pieces of metal, and at the Anniston plant there Is a small catch pot in the line to the pump, for the same purpose. The lines are arranged for easy clearing, and have steam tracing. (Aroclor jackets at Anniston'. * See page XII-10. DSW 257496 STLCOPCB4061615 XII. EQUIPMENT LIST, contd. XII - 9 Equipment List CT-0744 Closed Tanks, contd. CT-0744, contd. 5. A manlid very nearly at the bottom of the straight side, carrying the chlorine inlet fitting. This fitting consists of a shallow round box, set hori zontally below the internal cylinder of iron turnings, and having about 240 round holes 3/16" diameter on its upper side and a 5/4" drain hole on the under side. The chlorine enters the box horizontally from the chlorine inlet control valve. It is advisable to have a spare inlet box, because'the holes slowly become enlarged, the corrosion being a little faster on the Side further from the inlet valve. Messrs. Hosmer and Soffranko, October 15, 1948 describe a distri butor of cast nickel. Cast monel has also been mentioned. Nickel cast iron is the more usual material. The chlorine inlet line is thermally insulated with asbestos paste to prevent the use of flames intended to clear blockages from the line. Overheating at this point may cause very rapid corrosion, and organic matter might even take fire in the chlorine. The cover of each chlorlnator has the following fittings: 6. An inlet, with sight glass for diphenyl from the measuring tank CT-O767, and formerly for high boilers from the melter CT-O765. 7. An inspection cover, carrying the return inlet from The circulating pump. This inlet is carried through to the centre line of the chlorlnator, above the internal cylinder. 8. A vertical 10" central pipe for the off gas,leading to the bottom of one of the scrubbing columns CT-0759 etc = and so to the HC1 absorber. This exit pipe has a hand hole with cover, on the side, for cleaning, and has a sw 257497 STLCOPCB4061616 , - XII. EQUIPMENT LIST, contd. XII - 10 Equipment List CT-0744 Closed Tanks, contd, CT-0744, contd. 8. contd. relief disc of 4 lb, lead at one connection, (See sketch on page 10a, Section VI. ) ' If the relief disk bursts, the gas will go directly to the HC1 absorption unit. The disks rupture at about 25 psig, but they usually last for at least several years. There is a mercury manometer on the 10" pipe to give warning of blockage in the off-gas system, 9. A return line from the scrubbers CT-0759 etc, goes into No. 1 chlorinator. 10. A vent valve, hand controlled, to a drum outdoors. 11. A thermo well, reaching down into the charge. The fifth chlorinator, CT-01432, which has been installed at the Krummrich plant, is of the- same type as the previous four, with jacket and internal coil, but the coil has been retained, whereas the coils had been removed from the older chlorinators. (At the Krummrich plant, the internal coils had been abandoned as being more liable to put water into the batch, but at Anniston it was the jackets that were abandoned, because on one occasion a jacket had burst when water was trapped in it when the chlorinator temperature reached a high value). To give still mere cooling capacity, the stream of liquid circulated frem and to the chlorinator, during the chlorination, can now be passed through a homemade cooler consisting of two vertical lengths of jacketed pipe in parallel. (2" pipes in 2" shells). There is a thermometer well (glass thermometer' in the top of each length of jacketed pipe. The water goes up one jacket then down the other, and so out to waste, no special provision being made to keep the second jacket flooded. DSW 257498 STLCOPCB4061617 XII. EQUIPMENT LIST, contd XII - 11 Equipment List CT-0744 Closed Tanks, contd. CT-0744, contd. The old uncooled circulation line has been left in position, so that this external cooler can be byepassed. The circulation pump, therefore, delivers to a horizon tal header which has four outlet cocks facing upwards, plus a sample cock facing downwards over a drip vessel (see sketch).* One of the four cocks will direct the flow of liquid to the air blowing tanks, one will byepass it directly to the top of the chlorinator, and the other two will direct half the stream through each of the external coolers, and so into the top of the chlorin ator. This same No. 5 chlorinator has been equipped with a flow recorder-controller on the chlorine feed. An orifice plate with a sulphuric acid U tube is used on the chlorine line, as with the older chlorlnators, and the gas feed to the chlorinator can be hand controlled, just as with the older units, but in addition, the same ori fice plate Is piped up to a differential pressure cell which operates the flow recorder-controller on the instru ment panel. That instrument in turn actuates a 2" dia phragm valve on the chlorine line (see sketch). The valve has steel working parts, but a tantalum stem, and it has given very satisfactory service. Similar recorders would be obtained for the other chlorlnators, except that the expense cannot be Justified at present on any saving of manpower, or on any necessary Increase in production. These two changes both make for shorter average time cycles in the chlorination. Research work indicates that faster chlorination (at the same temperature) gives essentially the same product, though infra-red analysis suggests a slightly different isomer ratio. This mainly concerns the higher Aroclors, and a suggestion has beenmade that more rapid chlorination might increase *page 10a, Section VT. DSW 257499 STLCOPCB4061618 v XII. EQUIPMENT LIST, contd. XII - 12 Equipment List CT-0744 Closed Tanks, contd. CT-0744, contd. the proportion of (waste) highboiling material produced. Not much experience has yet been gathered on the chlorin ation speed which may be attained, but 800 to 900 lbs. chlorine have been fed per hour on occasion, and a batch of 1260 has been run in 14 hours, and one of 1248 in 10 hours. The Krummrich plant has not been pressed for output, and the present scheme of working is to run the chlorinators at a moderate speed, using each in rotation, over lapping the cycles of the different units, so as to maintain a fairly steady consumption of chlorine. This suits the chlorine department, which has no outlet for snift gas when the Aroclor department is not taking chlorine. The off-gas from each of the older chlorlnators leaves by a 10" pipe running about 12' up from the centre of the cover of the chlorinator, but the new chlorinator has only a 4." exit pipe with a very small cyclone, draining back to the vessel. It has its own Raschig tower with Aroclor circulation, then a cyclone, etc., just like the older units. Aroclors above 1262 are no longer made at the Krummrich plant, so there is much less chance of getting much chlorine in the off-gas, and the off-gas scrubbers, con sequently, are of less Importance. They are still used, and they give a cleaner HC1 for the absorption unit, but If they should be out of action for a time, no par ticular harm results. The Aroclors involving the use of diphenyl high boilers are no longer made at the Krummrich plant, and the melterblow case, CT-O765, for handling the highboilers, has been taken out. A second air-blowing tank, CT-02086, like CT-O75O, has been installed for the ordinary Aroclors. DSW 257500 STLCOPCB4061619 XII. EQUIPMENT LIST, contd. XII - 13 Equipment List CT-0744 Closed Tanks,contd. CT-0744, . contd. At the Anniston .plant there are eight chlorinators, similar in shape to those at the Krummrich plant. They have internal coils for steam and water, but the water jackets have been put out of use. The chlorinators are located in an open-sided steel structure, outdoors, and hang from brackets about 50" bfelow their rims, so that they are free to expand downwards as they become hot. This expansion distorted the connections to the pumps, which at first were rigidly mounted, so that pumps were given spring moun&ng3on slotted clips. More recently the pumps on two of the chlorinators have been mounted on rubber pads on steel frames hung from the vessels them selves, so eliminating the distortion due to the expansion of the vessels. The new pumps are larger ones, Taber horizontal Centri fugal pumps, direct coupled to 5 h.p. motors, 1730 RPM. All the^chlorlnator pumps have jackets for heating by Aroclor. The hot Aroclor comes from a standard gas-fired unit in a building near the chlorinators, passes through the pump jackets, then through the jackets of the pipes and of . the cock on the bottom outlet of the chlorinator, then through the heating "pad" on the bottom of the chlorinator, and so back to the heating unit. The other parts of the ' circulation system on the chlorinators are steam Jacketed, and the pad was formerly used for steam. The return, stream of process material from the circulating pump enters the chlorinator by a pipe projecting a little way through the cover. This location of the return pipe perhaps favours entrainment of liquid in the off-gas, but if the pipe goes further down, it may dip in the charge, and permit siphoning at an inconvenient time. There is a heavy steel grating over the bottom outlet of the chlorinator, and there is a heavy stool, of steel grating, with a perforated plate on it, to support the catalyst basket. The top of the basket has a screen welded over it to confine the catalyst, an arrangement which prevents easy "topping up" of the catalyst, but by the time that DSW 257501 STLCOPCB4061620 . . -v ' XII. EQUIPMENT LIST, contd. XII - 14 Equipment List CT-0744 Closed Tanks, contd. CT-0744, contd. the topping up is needed, there.is usually some other repair to be done inside the vessel. There is a screen over the bottom outlet, and a small catch pot, both intended to trap stray metal. The connections to the inlets and outlets of the steam and water coils in the chlorinators go in through the sides of the vessels. The following notes on an overhaul of the Krummrich plant chlorinator, November 1948, are of interest: - 1. Chlorlnator cover was taken off and all old catalyst was removed and discarded. It was found that a solid mass of catalyst, mud, residue, etc. was in the full length of the annular space between the inner sleeve and chlorinator. This solid mass was also present to some extent within the inner sleeve. In addition, there was a hole approximately 8" in diameter the entire length of the catalyst bed. 2. The sleeve was removed from the chlorinator and the top half was renewed with 3/16" steel. Although the top half of the sleeve did not have holes, it was considerably thinner than the lower half. 3. "Ears" were welded on the sleeve to make for easy removal next time. 4. Installed new screen on top of sleeve, between sleeve and shell to keep catalyst from falling into annular space. Screen had 4 rows of 1/2" holes and was 1/2" thick. 5. A new cast iron chlorine distributor was installed. The old distributor was discarded because many cf the holes were enlarged and beyond repair. DSW 257502 STLCOPCB4061621 XII. EQUIPMENT LIST, contd. XII -15 Equipment List CT-0744 Closed Tanks, contd. CT-0744, contd. 6. A new grating, above the distributor was installed to hold the catalyst in place. The grating made of x 1" strips, was purchased as such. 7. A new monel screen plate was put over the bottom outlet of chlorlnator to keep catalyst from going into pump. 8. Welded corroded portion on inside, lower flange of 12" off-gas line. Corrosion was at the weld where the pipe and flange are welded. 9. 7 x 55 gallon drums of catalyst, which filled the basket of the chlorlnator were put in. Below is listed additional information that may be of interest and serve as information for future use c Chlorlnator Number 2 54 Outage measurement of top of sleeve 92" 92" Outage after charging 3600# Biphenyl 76" 68" 85" Outage of finished 1160 batch 18" 13" 37" All measurements taken from top flange of shell and i the manhole. DSW 257503 STLCOPCB4061622 . - XII. EQUIPMENT LIST, contd. XII - 16 EQUIPMENT LIST CT-07^ Closed Tanks, contd. CT-0744, contd. The performance of the chlorinator was improved as evidenced by the following figures? Before Overhauling After Overhauling Chlorinator Chlorinator Time required to chlorinate batch. Sp.Gr. increase per hour after reaching 1.450 at 90C. Chlorine pressure entering chlorinator during last 6 hours of chlorination. 50 - 55 hours 0.012 - 0.015 20 - 24 hours 0.018 - 0.026 10-11 lbs.gauge 7-8 lbs.gauge Valve in cooling water line to jacket wide open after 4 hours of chlorination 5-2 turns open during entire chlorination Chlorinator tempera ture toward the end of chlorination 150 - 165C. 140 - 150cC. Scrubber liquor build up. Past (Every 4-8 days) Normal (15-25 days) Still bottoms pro duced, for all chlorinators, after every 4 still batches 2500 - 5000# 1000 - 1500# The above data are only approximate but do show a very definite improvement after overhauling the chlorinator-. DSW 257504 STLCOPCB4061623 v - XII. EQUIPMENT LIST, contd. XII - -7 Equipment List CT-0744 Closed Tanks, contd. CT-0744, contd. Number 3 chlorinator was overhauled January 24, 1949 with similar results. In this chlorinator the chlorine dis tributor was found to be fit for re-use and the new grating installed to support the catalyst was ordinary floor grating. The water jacket was found to be reason ably clean, but two 4" nozzles were welded on at the bottom of the jacket, to serve as cleaning openings. There are no deflectors in that jacket. The measurements down from the flange of the shell were: Before overhauling After overhauling To top of sleeve 92" 92" To level of 3600# biphenyl charge 68" 88" To level of finished 1160 batch 13" 31" To level of finished 1154 batch 46" To level of finished 1148 batch 56" DSW 257505 STLCOPCB4061624 XII. EQUIPMENT LIST, contd. XII - 17 a Equipment List CT-07^5 -0750 Closed Tanks, contd. CT-07^5 West chlor. tank same as CT-0744. On Dept, struct, steel MCS-O65O. #1 chlorinator. CT-0748 Diphenyl storage tank made by Graver Drwg. C609* 10' dia. x 26' long straight side, dished heads 9/16", shell 1/2", welded const. 2" xHy pipe coils, 1" risers, manhole covers, outlets and sump. Pump P-0585. Order B7700 on 4/17/56, Req. 69220. Price $1000.00. drwg. 609. Underground west of CR, 1st from south. Same as CT-0749. CT-0748 was originally installed for general use, mainly on Aroclor brought from Anniston for use in the scrubbers CT-0759 etc., and CT-O749 was piped up to receive material, in emergency, from the vacuum stills. Both 0748 and 0749 are now used to store diphenyl. CT-0749 Aroclor 1148 and 1142 Aroclor stg. tank. Same as CT-0748. Horizontal boilers in pits outside the shed. Submerged pumps actuated by remote control from near the scrubbers. Molten diphenyl in from rail cars. Return overflow lines from the scrubbers, (disused}. Vent lines protected against weather and fire. Steam coil. One point of the thermo recorder is in CT-0748. The submerged pumps are carried on the manlid covers. Return line from overflow connections of diphenyl head tank, CT-0767. CT-0750 Blow tank made by Graver. Dwg. E-865. 7' dia. x 7' str. sides, dished heads shell 5/8". 5 turn coil of 2" xHy pipe supported on brackets welded. Order B7704 on 4/17/56, Req. 69224. Cost $525.00. On steel MSC-O65O dept, steel, 12' level, 2nd floor level Bldg. CR. 8/10/54:Network of pipe with 1/8" holes. Air jet in sta'k DSW 257506 STLCOPCB4061625 XII. v - EQUIPMENT LIST, contd. XII - is Equipment List CT-0750 - 0752 Closed Tanks, contd. CT-0750 The cover of Blow tank CT-0750 carries the following connections s - Inlet from chlorinator pumps, with sight glass. Float with indicator scale. Compressed air in, to a grid of perforated piping. Connections to steam coil. Haveg vent column through the roof. There is an angle thermometer on the side. Bottom outlet to Pump P-0580 for delivery to the stills S-043 and S-062, or to drum filling on the floor immediately below the tank. Side manhole. The float has a simple brass chain passing over two pulleys to an indicator hanging in front of a scale. Drawing D-01292 replaced E-863. CT-0751 Cyclone collector purchased from Graver. Dwg. B645. 48" dia. x 27" on str. side. 5'6" long and tangential inlet near top of side. 5/16" steel throughout, of welded construction. Order B7712 on 4/17/56, Req. 69232. Price $84.00 On 2nd floor level, lean-to of CR. CT-0752 Vertical steel closed tank made by Graver. Dwg. C-8o4. 4' dia. x 5' high with flat bottom and dished flanged head. Sides, bottom and top of 5/16" flange welded cons'1: . with outlets. Order B7709 on 4/17/36, 'Req. 69229, Price $120,00 On 1st floor, west side of CR. (Hot Well). This tank for recovered hot water from the chlorinatcrs. Formerly received the barometric legs of ejectors MSC-0760 etc.. ' DSW 257507 STLCOPCB4061626  ' XII. EQUIPMENT LIST, contd. XII - 19 Equipment List CT-0753 Closed Tanks, contd. CT-0753 (also CT-01396) Coke scrubber on the vacuum still system. Scrubber tank made by Graver. Dwg. C-807. Steel, closed tank, 3' dia. x 10' long with dished bottom and flgd. dished head, shell 5/16", bottom 3/8", head 5/16" with 1" thick flanges. Price $155-00 On 3rd floor elevation bldg. CR. Coke scrubber on #1 still. Vapours from the still receivers CT-0771 and 01377 enter at the top and the unabsorbed gases leave at the bottom via a cock, to the ejectors, MSC-O76O, 01392, and 01686. The scrubbers are filled with coke, which is flushed with caustic soda solution a few times a year. There is no history of serious corrosion trouble in the ejectors. Mr. D. G. Furzey reported, December 5, 1951> that cotton wool in the scrubbers was renewed every few years. Wide hand hole at the top for charging with coke and for flooding with caustic soda solution. Drain to sewer. It is convenient to divide the distillation system into sections by means of isolating cocks and to have a manometer connection to each section to assist in locating vacuum leaks. Mr. Soffranko points out the need for an inspection cover on the top of the scrubber. There is a layer of cotton wool on top of the coke in the scrubbers. The scrubbers are needed mainly for the distil lation of high boiling Aroclors, because there is a Hide HC1 formed by decomposition, but they also trap water which might come back from the ejectors. Mr. Pemberton. December 1950> reported that Anniston gave up the use of caustic soda in the coke scrubbers after the'Karbate ejectors were in stalled. The cotton wool becomes glazed over with heavy Aroclors and the vacuum lines may choke. See also the comments on pages VII - ^ and 5. DSW257508 STLCOPCB4061627 ,v XII. ' EQUIPMENT LIST, contd. XII - 20 Equipment List CT-0754 Closed Tanks, contd. CT-0754 Scrubber liquor pump tank made by Graver. Dwg. C-800, 4'6" dia. x 5*6" on str. side with dished heads, shell 3/8" thick. Heads 1/2" thick, welded seams, pads and nozzles. Coil 3 turns of 1-|" xHy pipe. ' - Order B7703 on 4/17/36, Req. 69223, Prise $208.OQ. Tank mounted on steel, east tank on 38s level. Same as CT-0755 and 0756. Of tne five scrubber liquor pump tanks, three are coil heated and the two newer ones are Jacket heated. Jacket heating is preferred as being less liable to put water into the Aroelor circulation system. These tanks were formerly charged with Aroelor {coming originally from Anniston) stored in vessel CT-0749, and pumped from it by its submerged pump. It is now found more convenient to charge them from a partly chlorinated charge in #4 ehLsrlnator, pumped up by means of the chlorinat-or pump. With slow chlorination, especially in the early stages of chlorination, the scrubbers tend to pick up diphenyl, and the liquor becomes less dense. With faster chlorination, the circulation liquor tends tc increase in density. When the liquor needs to be renewed it is dropped t the melter CT-O763 for return to one of the chiorinators. The foreman calculates from the density what volume should be taken to give the equivalent of a fresh diphenyl charge t the ehlerlnator. See page 10 Section VI, for the method of calculating the equivalent. See letter E.M. to M. B., May 17, 19^8 n the handling of the scrubber charges. DSW 257509 STLCOPCB4061628 XII. EQUIPMENT LIST, contd. XII - 21 Equipment List CT-0754 - 0756 Closed Tanks, contd. CT-0754 contd. The cover of the scrubber liquor pump tank carries the following connections: Vent line with hand operated valve normally open to a drum outdoors. Steam coil, in and out unless a Jacket is used. Arcelor line in from CT-0749. Aroclor line in from chlerinator. Return line from tower and cyclone, with sight glass. Dipping hole. Submerged pump with its delivery line. There is a thermometer well in the side of the vessel above the steam jacket. An angle thermometer is used. Exact- temperature control is not needed. Bottom outlets to chlorinators and to melt tank GT-O765, and t-o a levelling line by which material may be passed from one scrubber tank to another Overflow {disused} to CT-0748 and 0749. CT-0755 Scrubber liquor pump tank. Center tank. Same as CT-0754 and 0756. CT-0756 #1 scrubber liquor pump tank. West tank. Same as CT-0754 and 0755. DSW 257510 STLCOPCB4061629 XII, EQUIPMENT LIST, contdo XII - 22 Equipment List CT-0759 Closed Tanks, contd,, CT-0759 #4 East Aroclor scrubber,used on CT-0754. Made by Graver, Steel tubular tank, 12" dia. x 8' high, removable head, Pkgd. with 6! of Raschig rings, Chg. out $84,00, Drg, C-798 and B-660. 15" dia. cyclone. Gas in at bottom by wide descending pipe from the top of the chlorinator off gas pipe (the HC1 manometer branch comes off the top of this line) and out at the top to the cyclone CT-01259*( 01279, 01280, 01281 and 01282.) Liquor in at the top from the submerged pump in the corresponding circulation pump tank, and out.at the bottom by seal bend with sight glass to the same tank. There are four water-cooled chlorinators and one gasfired one and for these there are five scrubber systems all alike except that the one on the fired chlorinator ' can be gas heated. The off-gas from a water-cooled chlorin ator ascends in a wide pipe to the bottom of a packed column with Aroclor circulation. Prom the top of the column the gas goes via a cyclone to the header leading to the absorption system of the Aroclor plant or to that of the chlorbenzol plant as required. The Aroclor for each column is circulated by a submerged pump in a scrubber liquor pump tank, and the liquor draining from the tower, plus any trapped in the cyclone, returns to the liquor tank via a deep seal bend and a sight glass. There is a sampling cock at the bottom of the seal bend, and there is a thermo-well near the S. G. The gas from the gas-fired chlorinator goes to the monel gas chamber CT-01258 where it deposits most of its entrained solid Aroclor, and thence by wide steel lines, with cleaning flanges, to a scrubber system which is similar to the pthers, but which has arrangements for gas heating. (The gas-fired chlorinator went out of use in . 1949)o DSW 257511 STLCOPCB4061630 XII, EQUIPMENT LIST, contd. XII - 23 Equipment List CT-0759 Closed Tanks, contd, CT-0759 Only chlorinator #1 is normally used to feed the gasfired chlorinator and #1 is not recharged until the gas-fired chlorinator is empty. Nevertheless, there is a scrubber system for #1 chlorinator as well as for the gas-fired chlorinator. The gas from #1 can be put to either of these scrubbers. It can in emergency be vented to atmosphere. Mr. D. G. Furzey reported, December 5# 1951# that the scrubbers and separators sometimes block with solid which has to be melted out with blow torches. A scrubber was installed at Newport, but after some experience the Raschig rings were taken out of it and the circulation was stopped. It was found that the off-gases from high boiler chlorin ation batches deposited rather viscous material in the empty tower. This raises the question of the contamination of diphenyl liquors in the scrubbers, with high boiler products, but the contamination appears to be unimportant. The towers were finally bye-passed, very little material was collected in the cyclones which came next in line of flow, and there was no evidence of trouble due to organic matter in the HG1 absorption unit. At Krummrich plant the increase in volume per scrubber came to about 10 Imperial gallons per week. The cyclone at Newport corroded through. The seal bend was removed from its drain line as being unnecessary,, DSW 257512 STLCOPCB4061631 XII. EQUIPMENT LIST, ccntd. XII - 24 Equipment List CT-0760-0763 Closed Tanks, contd. CT-0760 #2 Center Aroelor scrubber. Same as CT-0759. CT-O761 #5 scrubber tank made by Graver. Steel tubular tank 12" dia. x 8' high, removable head. Packed with 6' of Raschig rings. On CT-O968. Chg. out $84.00. Drg. C-798. CT-O762 Vent line scrubber stored in CR lean-to. Made by Graver. Steel tubular tank, 12" dia. x 8' high (50# std. pipe 5/8") removable head.' Dwg. C-798. Packed with 6* of Raschig rings. Drg. C-798. Supports B-665. CT-O765 Melt and feed tank made by Graver. Dwg. C-810. Closed steel tank 4'6" dia. x 5'0" on str. side, shell 5/8", dished bottom and bolted dished head all 5". 2" xHy pipe coil, 10 tumjwith 5 supports welded to head. Tk,, test 90# and coil 500# Hydro. Press. Order B7710 on 4/17/56, Req. 69250. Price $516.00. J way in floor, south side of CR. The cover carries the following fittings: -- Manhole and cover, with handhole for admission of broken lumps of diphenyl highboiler. Steam coil in and out, C. air connection and vent (Dry air from FC-046.) Inlet from all scrubbers CT-0759 etc. Outlet to drums and to header leading to chlorinators. There is a hand operated hoist with lifting hooks for drums over the manhole, and a ventilation hood connected to blower B-0148. The melter is set in the ground floor of the crude room. DSW 257513 STLCOPCB4061632 XII. EQUIPMENT LIST, contd. XII - 25 Equipment List CT-0764-0767 Closed Tanks, contd. CT"0764 ' North Hopper Storage Bin made by Graver. Dwg. D-512. Vertical, 6' x 6' x 10'8-5-" high overall, with sloping bottom and bolt -angles. 5/16" plate throughout with reinforced flat bolted on cover with trap door. Entire inside of hopper and underside of cover and trap door sprayed, 1st with .005" zinc and then .005" tin. Order B7713 on 4/17/56, Req. 69255, Price $288.00 Southwest end of CR lean-to. Same as CT-O765. CT-O765 South hopper storage bin. Same as CT-0764. CT-O766 Circulating cooling tank made by Graver.On No. 1 Still. Dwg. B644. Steel tank 2'6" dia. x 5'0" str. side with dished head and welded on pipe legs, shell ", heads 5/8". Coil of 1^" dia. xHy pipe, 4 turns on supports welded to Inside of shell. Test tk. 225# and coil 500# Hydro press. Safety Valve. Gauge glasses. Order B7706 on 4/17/56. Req. 69226. Price $110.00. On 58' floor level. Bldg. CR. 1-0510 Taylor Fulscope temperature indicating controller, 0-110C., with steel diaphragm valve on the steam inlet to the coil in CT-O766. Operated from the temperature in CT-0766. CT-O767 Diphenyl measuring tank made by Graver. Dwg. C=799 Steel tank 4'6" ID x 5'6" str. side, dished heads, shell 5/8, top head 5/8 and bottom head 5/4" with " jacket over it and extending 9" up on tank side. Welded through out. Test tk. 60# and jacket 105#.Hydro, press. Return line to store tank. Order B7701 on 4/17/56. Req. 69221, Price $529.00. At 58* level. Bldg. CR. Drg. C-799 o DSW 257514 STLCOPCB4061633 XII. EQUIPMENT LIST, contd. XII - 26 Equipment List CT-O767-O77O Closed Tanks, contd. CT-O767 contd. Steam traced vent to drum outdoors. Manlid. Dipping hole with cap. Fixed overflows at 4 levels back to diphenyl store tank CT-0748 by steam traced line with sight glass and right angle cross pieces with blank flanges. Lower part of vessel jacketed for steam from the 70 lb. main. Angle thermometer 30" long through side of vessel. Bottom outlet to header leading to the 4 chlorinators. S. G. at each chlorinator. CT-O768 # 3 Aroclor 1260 finished product storage tank. Made by Graver. tag. C-609. Horiz. steel 10' dia. x 26' long on straight side, dished heads, shell J", heads 9/16". Test tank 60# and coil 300# Hydro. Press. Coil 2" xHy pipe with 1" xHy risers. Welded construction throughout. All inside and fig. surfaces, colls, supports, etc., to be sprayed first .003" zinc and then .003" tin. Same as CT-O769. Order B77H on 4/17/36, Req. 69231. Chg. out $1385.00. CaCl2 vent trap. CT-O769 # 4 Aroclor 1254 Finished Product Storage Tank. Same as CT-0768. CT-O77O . Tubular heat exchanger made by Nooter. Dwg. B65I, Plant A, Size 12" dia. x 5'0" lg. having 19 x 2" OD 11 ga,, Monel Tubes, Monel tube sheets. Monel reducer and carbon steel jacket and back-up rings on flanges. Order B8848 on 5/1/56. Req. 69605. Price $660.00 Above No. 1.still S043, supported by 3rd floor steel. Plant "B" (Krummrich Plant) coriinue to recommend monel for the condensers on the vacuum stills. See also item CT-01378. Only monel in contact with the goods on the "descending" side of the condensing system. DSW 257515 STLCOPCB4061634 XII. EQUIPMENT LIST, contd. XII - 27 Equipment List CT-0770 - 0771 Closed Tanks, contd. CT-0770, contd. Mr. Thrift, December 5> 1949* raised the question of the necessity of using monel for the vacuum still condensers and subsequent vessels. Mr. Ellenburg of Anniston replied, 15th December, 1949, stating that iron contamLnotf&on of the Aroclors would have a bad effect on the resistivity and the power factor of the products. Steel also hastens the darkening of Aroclors at temperatures of 80C. or higher. Messrs. Hodges and Barbre of the Krummrich plant replied that monel was satisfactory for the condensers and receivers but that there were no reasons to believe steel would not be satisfactory. Although General^Electric Company report that steel is satisfactory for storage and treatment vessels, Krummrich plant do not care to risk the use of steel because of the high standards required by G. E. for Aroclors. CT-O77I Monel vacuum receiver made by Nooter. Dwg. C-795. (Plant A). Size 5*6" dia. x 5'6" str. side, 5/8" shell, bottom and removable head, 4 support brackets on outside of tank of steel. 2" IP size xHy Monel coil with 2" inlet and 1" outlet with Monel bars and U bolts. 5 turns 5' dia. along side and 5 turns spiral on bottom. 60# Hyd. test on tank and 500# on coil. Order B7379 on 4/14/56, Req. 69118. Price $5240.00. On second floor level, 12' level, Bldg. CR. No. 1 still. Return line, for spoilt material, to the still, of the vacuum still receivers The covers/carry the following connectionss Inlet from condensers CT~0770, 01578 via sight glasses. The cylindrical surface of the sight glass fitting is steam jacketed and so is the pipe from the con denser to the sight glass. Manlld with hand hole and dipping opening. DSW 257516 STLCOPCB4061635 XII. EQUIPMENT LIST, contd. XII - 28 Equipment List CT-0771-0779 Closed Tanks, contd. CT=0771 contd. Dial vacuum gauge and mercury U-gauge. Thermo recorder well. Vent cock. Steam coil in and out. This coil goes well down into the bottom dish of the receiver. Vacuum line to the top of coke .scrubber CT-0753 and -01396. Bottom outlet to pump P-0984 for delivery to the Sparkler press and to Blackmer pumps, P-O565, "01037* for delivery to the blending tank, CT-0779. Electric strip heaters to drawing C-847, formerly used on these vessels have been abandoned, so no copy of the drawing has been requested for MCL. Material 1268 requires H. P. steam in the coil to keep it molten.. There is only one receiver for each vacuum still in the crude room,no fractionation being attempted. There is no gauge glass or level Indicator, only a gauging hole.* A receiver will hold a full batch from the still. CT-0779 #1 blending tank made by Graver. Dwg. E-862. Welded steel tank 7* dia. x 7' high dished heads shell 3/8" All inside surfaces and nozzles sprayed .005 zinc then .003 tin. 2" xHy pipe coil and supports. Yoke and drive supports. Cast bronze turbine stirrer and bronze shaft. Test tank 60# and coil 300#? hydrostatic Pressure. Order B7707 on 4/17/36, Req. 69227, Chg. out $599.00. On 2nd floor level, 12' level. Bldg. CR. Same as CT-O78O *But see page 21, section VI. DSW 257517 STLCOPCB4061636 XII. EQUIPMENT LIST, contd. XII - 2.9 Equipment List CT-0779-0780 Closed Tanks, eontd. CT-0779 contd. See also CT-01399# #2 Blender and CT-O78O* Filtrate Receiver. Drawings E-862 and E-6838 are essentially the same. Drawings A-459 and A-8853 of the bearing have been requested. Drawings D-2076, 2077# show the agitator rotor and stator. Anniston* December 15# 19*19# state that their blenders are of steel* sprayed with zinc then with tin and that the agitator in one case is of Tobin bronze (stated to be 60# Cu. 39-25# Zn, 0.75 Sn), and in the other case is of steel* sprayed with zinc then with tin. The sprayed agitator is said to be satisfactory. Plant "B"* January 5# 1950, state 0.005" Zn then 0.003" Sn for the tanks, and their agitators are of bronze of unknown compo sition, probably "ordinary commercial bronze". Anniston and Plant "B" agree in distrusting plain steel for these vessels. Anniston suggest Aluminium. CT-O78O #1 filtrate receiver tank. Dwg. E-862. Made by Graver. Welded steel tank 7' dia. x 7' high* dished heads , shell 3/8". Same as CT-0779- Materials 1260 and 1254 can be run from the receivers CT-O78O and 01400 to bulk store tanks. Other materials are filled off into drums. To save time, most of the control tests are done on samples taken before filtration. Material 1268 needs H.P. steam to keep it fluid. The filtrate receivers are like the blenders CT-0779 and 01399. except that the filtrate receivers have no agitators. DSW 257518 STLCOPCB4061637 XII. EQUIPMENT LIST, contd. Closed Tanks, contd. XII - 30 Equipment List CT-0785 0808 CT-0785 Middle acid tank south of CR on foundation. Made by Goodrich. Dwg. C-825. "Vulcalok" lines - steel tk. 7'0" ID x 8'6", shell 5/16", dished head 5/16", bottom 7/16", 4" outlet for safety plug on bottom. 18" manhole and cover, 5-5" flgd. outlets In head, 5/16" Triflex lining, rubber covered float and card for measuring device. Head with 6 - 1^" couplings for railings. Order B99&3 on 5/19/36, Req. 69966. Chg. out $945.65. South of CR on foundation. Same as 0784 and 0786. CT-0786 West acid tank, same as CT-0784 and 0785. CT"0808 Storage tank and chlorinator with stirrer and gas burner. (Gas fired chlorinator). Made by Kilpatrick and Sons Pdy. Co. Dwg.VA324, Cast Iron, 6' ID x 4'll" deep inside, wall 2" thick, bottom 3" thick and dished in 3". 3" outlet at lower rim. Marked S-459, weight 12,675#. Machining outside of top flange but without holes and machining outlet in rim including drilling and tapping holes. Cost of machine work $56.00. Order B8162 on 4/24/56, Req. 69398, Cost $517.65. On 12' level SW corner Bldg. CR. Drawing C850 gas heater on exit-line. Subsidiary drawings; Pr. relief door on 6'0" Cl storetank Clamp for electric strip heater Vent for Cl tank Shear pin unit -- for drive on agitator Brick setting Drive for stirrer 8'5" x 10'll" steel shell for tank Vent stack for still heater Still heater B-613 B-684 B-686 C-605 F-867 E-888 E-88l B-689 E~886 This gas-heated chlorinator is also called S-0459. The chlorine enters the gas-fired chlorinator through a per forated pipe ring, and there Is a separate inlet pipe- DSW 257519 STLCOPCB4061638 XII. EQUIPMENT LIST, contd. XII - 31 Equipment List CT-0808 Closed Tanks, contd. CT~0808, contd. with a simple open end for use when the perforated pipe becomes choked. The cover carries a wide neck through which material recovered from the monel catch vessel CT01258 can be returned by means of a wide steel funnel. There is another neck, wide enough to admit a sampling bottle also used as a gauging hole. Inlet from #1 chlorinator CT-01285 by a gas-heated gravity line or via pump P-0907 through .lines with H. P. steam tracing. 9" monel duct, with cleaning flanges, rises at 45 from the chlorinator cover, then descends at 45 to the monel gas chamber CT-01258. Prom the monel chamber onwards the ducting to the scrubber is of steel with cleaning flanges. Compressed air connection into the chlorine inlet for clearing (not very successful). Agitator with water cooled stuffing box. Thermo recorder well. Bottom outlet with gas flame heating, to the retort vessels R-026 and R-027 in an adjoining lean-tc building. See Drawing E-867 for the furnace setting, E-881 for the steel casing of the setting E-888 for the drive C-605 for shear pin for drive B-613 for pressure relief door on furnace E-886 for vent stack, P-324 which shows a shallower vessel; the chlorinator pot is similar but is 4'll" deep. The final chlorination to high chlorine content is more easily done in this, separate chlorinator because higher temperatures are needed to keep the charge molten. DSW 257520 STLCOPCB4061639 XII, EQUIPMENT LIST, contd. Closed Tanks, contd, XII- 3? Equipment List CT-0808 - 0852 CT-O808 conttiL Drawings B-684 strip heater B-686 clamp for strip heater B-689 vent stack for furnace have not been requested as they are not of interest. Strip heaters are not now used,, CT-0851 Water condenser made by Heine Boiler Company, Dwg, B485 (Plant A), used as temperature control for Aroclor condenser CT-0770, 12 tubes, 1" OD - 10 GA seamless steel tubing 10'-0" long, 10'.0" overall length of 6" std, pipe shell single pass. Order B8773 on 5/11/36, Req, 69576, Price $98,00, Used on #1 vacuum still. Safety valve on shell, CT-0855 Chlorinator puchased from Leader Iron Works, Size 5' dla, x 161 made up complete including coils, inner shell, and grating, Dwg, E-880 and B-659- Order B-2815 on 2/5/37, Req. 76475 on 1/26/57, chg, out $790.00 on 5/31/37. . East chlorinator, #5 chlorinator. See CT-0744, CT-0848 TCB stg. Tank, Made by Graver, Tank dwg, E 4415 Coil C4412 for steam General E4566 Tank 8" ID x 25'6" long welded, 5/8" shell, 7/16" dished heads, 15-26" and 2-24" dia, manhole openings on top, 2-1" xHy, W, S, pipe coil, 71' approx. Order B5654 on 2/17/57, Req, 76951 on 2/12, Price $920,00 West of CR underground, Pyranol Plant, CT-O852 Raymond 2 stage cyclone dust collector sent to B by Anniston Plant, Each cyclone approx, 20" dia, - 21" str, section 52" depth of cone, steel construction, used with B-0105 In lean-to of building CR, No drawing. DSW 257521 STLCOPCB4061640 * XII. EQUIPMENT LIST, contd. ----------------------------------------- Closed Tanks, contd. XII - 33 . Equipment List CT-O968 n-01164 CT-0968 Scrubber liquor pump tank purchased from Nooter. Dwg. C-4616. Steel vertical Jacketed, size 4*6" ID x 5'6" long with Jacket. Order B15673 on 8/2/37. Req. 81458 on 8/2/37. Price $575.00. CT-01013 #1A scrubber liquor pump tank made by Leader. Dwg. C-4616. Size 4'6" ID x 5'6" vertical, steel, flange quality, all welded. , Jacketed. Order B 4l64 on 4/29/38, Req. 87029 on 3/9/38. Price $582.00 On 38' level SE comer CR. ' CT-01014 Scrubber tank made by Heintz. Dwg. C-4845. Steel 12" dia. std. wrought steel pipe 10'10" high, dished end and other end fitted with.3/4" faced and drilled fig. with 5/8" cover plate. Steel plate, and distributor. Use 5 cu. ft. 1" Cl Raschig rings pkg.5 Order B3933 on 3/4/38, Req. 86921 on 3/4/38. Price $139.00. On top of CT-01013, #1A scrubber. CT-01162 Scrubber tank made by Heintz. Dwg. C5743. Welded steel scrubber, size 12" ID x 5'. Order B19519 on 9/27/39, Req. 1977 on 9/19 Price $102.00. Vent line to CT-0848. (*) CT-OII65 Catch Tank 55 gal. steel drum. For CT-0762. Mate to CT-01164. $11.40. 11/27/39. Chg. out (*) (*) Both CT-01162 and CT-01163 are on vents of CT-01321 and 02621, Pyranel Plant. " CT-01164 Catch Tank. Same as CT-01163. For CT-01162j, Pyranol Plant. DSW 257522 STLCOPCB4061641 XIIo EQUIPMENT LIST, contd0 Closed Tanks, contd. XII - 54 Equipment List CT-01258 - 01279 CT-01258 Monel gas chamber made by Nooter, Dwg. C-5825. 4' dia. x 4' high constructed of Monel, Order B7855 on 4/5/40, Req, 8061 on 5/27/40, Req. 8061 on 5/27/40, . .Chg. out $867,00, On gas exit from fire heated chlorinator. This monel vessel is at the lowest point of the gas exit line from the gas-heated chlorinator. Solid Aroclor which collects in it is removed by hand and returned to the chlorinator with a subsequent batch, CT-01259 Cyclone Tank made by Heintz. Dwg, B5821, 2'6" dia, x 6*7" high constructed of 5/16" steel plate. Order B7545 on 4/27/40, Req, 8062 on 5/27/40, Price $92,00, Hang from roof of Bldg, on 58* level, CT-01259,01279, 01280, 01281, 01282, cyclones on chlorin ator off-gas, follow the scrubbing towers CT-P759 etc. Drain through S, G's to the return seal pipes between towers and circulation tanks. Off-gas to the main leading to the HC1 absorption systems. See drawing B-5821 (This drawing not yet found April 5, 1947) o See drawing B-660, CT-01265 Monel condenser made by Nooter, Dwg, C-6144, 42" dia, x 65" high cone bottom condenser constructed of 5/16 Monel metal welded construction throughout, ` Order B-8564 on 4/9/40, Req, 8198 on 4/1/40, Price $928,00 ' This vessel is obsolete, CT-01279 Cyclone separator made by Nooter Dwg, 5821, 2" dia, x 6'7" high cyclone separator made of steel and welded throughout. Order B15177 on 6/12/40, Req, 10252 on 6/5/40, Chg, out $66,25, For use at CT-0968, DSW 257523 STLCOPCB4061642 XII. EQUIPMENT LIST, contd. Closed Tanks, contd. XII - 35 Equipment List CT-01280 - 01321 CT-01280 Cyclone separator made by Nooter. Dwg. B-5821. 2' dia. x 6'7" high cyclone separator made of steel and welded throughout. Order B13177 on 6/12/4o. Req. 10252 on 6/5/40. Price $66.25/ At CT-O762 east scrubber. CT-01281 Cyclone separator. Same as CT-01279 and 1282. At CT---0759. 2nd from E scrubber. CT-01282 Cyclone separator. Same as CT-01279 - 1280 - 1281. Used at CT-O76O. 3rd from E scrubber. ; CT-01283 Chlorinator made by Leader Iron Works, Inc. Dwg. E6209, 3' x 161 steel vertical chlor. welded const. Order B-14119 on 6/21/40, Req. 10408 on 6/11/40. Price $720.00 East of CT-0833o #4 chlorinator. See CT-0744. CT-01310 #5 Aroclor 1260 Storage Tank made by Leader Iron Works. Dwg. 0-609= Horizontal 10' OD x 26' long on str. shell, incla. coils, etc. Omitted 2 - 3" nozzles changed 18" noz. to 2.4" and added covers for 24" noz. Tanks, coils, coil supports, inside of noz. and manholes and manholes and noz. and inside covers must be sprayed with zinc 0.005" thick followed by a sprayed coat of 0.003" tin. Order B13240 on 6/11/40, Req. 10432 on 6/11/40 Price $2200.00. Underground S of CT-0848. Pump P-0929. CT-01321 Pyranol Mixing Tank made by Nooter. Drawing D6455. 141 OD x 10' high steel tank with 3/8" shell, 1/2" std. knuckle radius heads, entire interior sprayed with min, thickness of .015" tin. ' 42" Quadruplex turbo mixer complete including Turbo adaptor assembly -- off set from centre.1 2 (1) Order B20976 on 9/27/40. Chg. out $2930.00 (2) Order B21762 on 10/8/41, Req. 13664, Cost $740.00 DSW 257524 STLCOPCB4061643 XIIo v EQUIPMENT LIST, contd. Closed Tanks, contd. ' XII - 36 Equipment List CT-01321 01397 CT-01321 contd. Driven by MSC-01288, Motor MOI7180 1^" steam coil, 45 turns, 18" diameter,through the cover. 96OO Imp. gallons. Outdoors. Everdur or galvanized piping. Bronze valves. Bottom outlet to Taber pump P-01540 delivering to filter press F-O159o Capped inlet on cover for Attapulgus Earth. Manlid. Steam coil. Dial thermo. Vent to soda-lime vent box. Heat insulation (gone). CT-01377 Still receiver tank made by Nooter. Dwg. C-795, B-7082, like CT-0771o PA #145. 5'6" x 5'6" Monel metal receiver, complete with cover, coil, etc. Glass wool insulation 2" and finished coat. Order B4137 on 6/27/41, Req. 18315 on 2/17/41. Price $3295.00. NE corner of 12' level platform in Bldg. CR. Is Used'on #2 still S-062. CT-01378 Condenser tank made by Nooter. Dwg. B65I. 12" ID x 5' long .Monel metal. Order B4137 on 10/20/41. Req. 18315 on 2/17/41. Price $650.00 W of CT-01413 on 20'6 level platform. Bldg. CR. Like CT-0770. Used on #2 still. CT-01396 Vacuum scrubber purchased from Combustion Engineering Co. Drawing C-807. 3' ID x 10' high, steel construction including grating and screen. Order B836O on 4/4/41, Req. 19989 on 4/4/41 Price $260.00. N one on 29' platform. Like CT-0753. On #2 still, coke scrubber. CT-01397 Water heat exchanger made by Leader Iron Works. Dwg. B-483. 6" dia. x 10' long, 12 tube. Order B8324 on 4/4/41, Req. 19993, Price $11900 North of CT-0831. On #2 still. Spare. DSW 257525 STLCOPCB4061644 XII,, . EQUIPMENT LIST, contd. Closed Tanks, contd. XII - 37 Equipment List CT-01398 01491 CT-01398 CT-01399 Cooler tank made by Leader. Dwg. B644. 2'6" ID x 3' high steel cooler tank complete with coil. Order B8324 on 4/4/41, Req. 19995. Price $152.00 South one on 291 platform Used on #2 still. Vented. E-6839 and #2 blending tank made by Nooter. Dwg./D-10290, general arrangement. 7' ID x 7' high, complete with coil, agitator, and drive support, zinc and tin lined, seams to be chipped and ground smooth. Order B8325 on 4/4/41, Req. 19990 on 4/4/41 Chg. out $950.00. Driven by M-02170. Middle one of 3, north end of 12' level platform. Vertical bearing for agitator shaft, A-6855. Compare CT-0779. Newport experience shows the need for adequate heating and agitation in blending higher Aroclors. CT-01400 #2 filtrate receiver,made by Nooter. 7' ID x 7' high incl. coil and supporting legs. Inside of tank zinc sprayed, all seams chipped and ground. 1" glass wool insulations 2.\" fin. coat. Order B8323 on 4/4/41, Req. 19992, Price $925.00 West one of 3 north end of 12' level platform, CR. Dwg. C-6863. See CT-O78O. CT-01413 Separator tank made by Heintz Steel. Used on #2 still. Dwg. C6957. 3* ID x 6' high tangential separator with integral vapor pipe complete. Order B10722 on 5/9/41, Req. 20429 on 5/1/41. Chg. out $382.50. North one on 29' level platform Bldg. CR. CT-01432 5th chlorinator. See CT-0744. Nooter. Drawing E6209. CT-01491 Heat exchanger tank made by Leader Iron. Dwg. B483, CABI #217. 6" dia. x 10' long, all steel, 12 tubes Order B21479 on 9/19/41, Req. 24894 on 9/19/41. Chg. out $140.00. Used on #2 vacuum still system. DSW 257526 STLCOPCB4061645 XII. EQUIPMENT LIST, contd. Closed Tanks, contd. XII - J8 Equipment List CT-02086 -02621 CT-02086 Air blowing tank. Like CT-0750- CT-02404 This store tank has been set up outdoors to hold the tri-tetra-chloro benzene mixture, which is bought in rail cars and unloaded by pump P-01111. The tank is a vertical cylindrical vessel 15'0" ID, 20'0" high on straight side with dome top and bottom. Total capacity 20,000 U.S. gallons. It has a bottom outlet, with a strainer box, to pump P-02077 delivering to either of the Pyranol blending tanks. The tank has a Varec depth indicator with stainless steel exposed parts, a vent pipe, a dip pipe for air blowing, an internal steam coil, and external heat insulation. NOTE; Mr. Barbre, 1947, said that a batch tank to hold filtered Pyranols, pending final approval, would be a convenience. CT-02621 An additional blender, CT-02621 has been installed out doors for making Pyranols. It is a vertical cyclindrical steel tank 10'6" ID 23'0" high with flat top and bottom. Total capacity 14,800 U.S. gallons. The bottom slopes 2" to the bottom outlet, which leads through a strainer box to a Taber pump P-02179, delivering to the filter press, P-0172. The tank has a 7? H.P. Lightnin mixer installed hori zontally low down through the straight side, the exposed parts of the mixer being metallized with 0.015" of aluminium. The vessel also has a Varec depth gauge with stainless steel float etc, a vent pipe to a soda lime vent box, an internal steam coil with T.I.C.*item 1-01894,set at 50C. (tin-sprayed thermo well), and external heat insu lation. There is also a dip pipe through which dry air from the Lectrodryer FC-046 can be blownby a hose con nection with Corby coupling to agitate and dry the contents of the tank. Attapulgus earth is introduced through a funnel fitted to an opening (with screw cap) in the top of the tank. DSW 257527 STLCOPCB4061646 XII. EQUIPMENT LIST, contd. XII - 39 Equipment List. Note: In MCC manuals the CT ana OT items of equipment are listed under "T", e. g. Closed Tanks and Open Tanks. DSW 257528 STLCOPCB4061647 -v ' XII. EQUIPMENT LIST, contd. XII - 40 Equipment List D-012 Dryers D-012 Flaker, Devine, 48" dia. x 30" long, drum 5/8" thick, rolled steel, machined and polished. Housing to be of #16 ga. monel. Order B 7578 on 4/14/36, Req. 69124 on 4/14/36, Price $1668,00 quot, 3/17/56. In lean-to on floor on found, of concrete. Driven by M-0827 - 5 HP Wagner motor thru MSC-0659U Jones Speed Reducer. The pan is heated by gas flames. Sketch showing drum side-knife, dip pan and essential dimensions on 48" diam. x 50" long steel drum, monel hood flaker -- drg. B-675* chutes for finished product. Drg. D-518. See drawing B-574. General arrangement, and C-827, weighing truck. Dryer for Attapulgus Earth. In 1946 a vertical steel tank with internal steam coils was installed at the Krummrich plant. It was still the only equipment for drying earth at the Kruminrich plant in 1955* but reliance was placed mainly on supplies drawn from Anniston, With the Krummrich plant dryer, the earth was fed in through a hand-hole in the cover, and withdrawn, as required, by means of a twin damper arrange ment on the wide bottom outlet. See hand sketch sent to MCL April 1947. At Anniston the earth is screened, 20 mesh, then dried in trays about 5" deep, place in an electrically heated cupboard. Each tray contains a weighed amount, so that the correct charge of earth can be put into the treatment tank directly from the dryer. DSW 257529 STLCOPCB4061648 XIIo EQUIPMENT LIST, contd. XII -41 Equipment List Dryers Dryers, contd. Dryer for Attaplugus Earth, contd. In 194-7 at the Krummrich plant the Attapulgus earth was . being dried in a vertical cylindrical steel vessel, with cone bottom, and an internal steam coil. The earth was fed in through a hand hole in the cover and withdrawn as wanted through twin dampers in the bottom. See the sketch sent to MCL with the drawings collected in 19^7- The cover of this dryer had a vapour vent, but there was no positive movement of air through the vessel, and the electrically heated sheif dryer used at Anniston (see page 5 of the report "Notes on the Anniston Aroclor plant" Havercroft and Mather, September 19^7), would appear more likely to give thorough drying. The steam heated dryer was still in use at the Krummrich plant March 51, 195^ The reference of Schwartlng and others, November 12, 1955, page 10, to an electrically heated dryer refers to a still earlier unit which had been abandoned. DSW 257530 STLCOPCB4061649 .v XII, EQUIPMENT LIST, contd, XII - 42 Equipment List F-0106 - 0172 Filters F-0106 ` Steel filter purchased from Nooter. Dwg. C-3775* Size 12" dia. x 3'10-3/4" high. Leg supports, glass wool packing. Order B35H on 2/19/56. Req. 67729 on 2/14/36. Price $36.00 quot. 2/5/56. Formerly used on chlorine gas, but used in 1946 to filter out iron etc. impurities from the HC1 gas coming from other departments through a long steel line . F-0113 Sperry 24" bronze filter press. Cover for electric oven heater for press -- Drg. B-685. Replaced by Sparkler press F-0172. Steel support and pan for Sperry filter B-7121. 3/4" pipe coll for filter catch pan -- A-7156. F-0159 General Electric Filter Press. Serial #6186968, Type FP30. Accessories included, 3 HP motor and 4 compartment drying oven. Form G, Cap, 25/30 gal. per min. Size 12", 20 chambers. Heated and insulated steel cover*with pullies, cable, counter weight and strip heaters, Pyranol plant. Order B18935 on 9/21/393 Req. 1991 on 2/20/39. Chg. out $984.00 on 11/30/39. F-0172 Sparkler filter. Serial 484. Model l8-dl2 all bronze construction with Improved Scavenger plate, plates to be arranged so entire set can be removed. Steam tracing inside the lagging, then a metal shield over all. Steel legs and floor flanges for bolting to floor. Served by pump P-0984. Order B10302 on 4/2/41, Req. 20430 on 4/30/41. Price $830.00 per quot, 3/19/41. On ground floor center of Bldg. CR. Installed for Aroclors, but later transferred to use on Pyranols, Chain hoist, MSC-Ol495 provided for lifting out the nest of plates. * MSC-02108. DSW 257531 STLCOPCB4061650 XIIo EQUIPMENT LIST, contd. XII -45 Equipment List F-0172 - 0259 Filters, contd. F-0172, contd. Samples of filter paper for the Sparkler press F-0172, which was then being used on Aroclors, bought under the reference "#21-l8 Filter paper'1, $2,755 per 100 sheets. Sparkler Mfg. Co. Mundelein, were sent to London, April 9, 1947, F-0258 F-0172 was moved to the Pyranol department and replaced by a 55" Sparkler. See Operating Instructions 8/10/54^, and Mr..Harden's notes of August 1950= Sparkler Filter, 55D-12 cell type,504 Stainless Steel, with jacket for 50 psig. 55" Sparkler press for Aroclors Installed In place of F-0172, F-0172 being used for Pyranols. F-0259 Sweetland, Size 10 RH, 54 leaves. 525 sq.ft. C.I. body, lined with thick nickel. Nickel valves and outlet line, with pump P-01757 Out of use In 1955= (Pyranol plant). DSW 257532 STLCOPCB4061651 XII,, EQUIPMENT LIST, contd. Furnaces XII - 44 Equipment List FC-045 70-045 Gas heftter for No. 1 still. Steel shell 3/16" x 3'9" dia. x 4'10|-" long, lined with insulating fire brick, etc. 1 coil 2" xHy pipe, 12 turns formed into a 2' dla coil with spare blocks and legs. Drawing E-886. Req. 69859 on 5/14/36, Order B9665 on 5/29/56. Used to heat material in S-043, pumped thru coil by P-0595 Vent stack drawing B-689 (could not be found in 1946.) Piping details, drawing C-815, was sent to London April 24, 1947. At plant B in 1946, there were two natural gas burners aimed tangentially into the bottom of each furnace, and there was some evidence of damage due to overheating of the lowest phrt of the coil. The central "dummy" inside the coil was made as a solid cylinder of firebrick and plastic refractory material built up on a circular plate suspended on a central steel lifting bar. Head room and a suspension hook are required over each furnace, for maintenance work. The material from the still is pumped downwards through the coil in the furnace of the new still, but upwards in the old stillo The main reason for this is that this arrangement enables the coil of the deep still to be on the same level as that of the shallow one. At Anniston the material is pumped upwards because this puts the coldest Aroclor in at the bottom where the coil is most in danger of overheating. This can have little advantage, except towards the end of the run, when the temperature spread between the inlet and the outlet is greater. There is a thermo-recorder pocket in the inlet of each coil, and another in the outlet. There are valves on the circulation lines, by which the coil can be sucked empty. See Section VI, page 18. These also help in locating any blockage in the circulation system. DSW 257533 STLCOPCB4061652 . V .' XII. EQUIPMENT LIST, contd. XII - 45 Equipment List FC-045 -066 rarnaces. contd. Ft-045 contd. Mr. Furzey reported, December 5# 1951 that the coils last about 12 months, but may require cleaning every 5 or 4 months to remove plugs. At Newport the still coil is interchangeable with that of the diphenyl department still. A temperature difference recorder controller was installed on the heater coil at Newport, and a COs connection made to the furnace for emergency use. At Anniston there is a 12-point Micromax temperature recorder on the chlorination system, and one for each of the two vacuum stills. FC-046 Electric, Air Drying Furnace purchased from Lectrodryer Corp. Serial 270, Size BWC-250, dual-absorber type. 40# pressure. 440 volts, single phase, 60 cy. 4-8 hours operation. 500 amp. heater on each side thermostati cally controlled, at 270F. See T-014. Order B7403 on 4/14/36, Req. 69119 on 4/14/36. Price $1,350.00 on 6/30/36. Has blower with Motor M-01486 for scavenging. Serves the air-blowing tanks CT-0750 and CT-02086, and the melter CT-O763, in the latter case at pressure enough to blow the charge to the ehlorinator. Brings the dew point of the air to between - 10*F. and + 10F. Lyles, Soffranko and Miller (Pyranol report March 24, 1947, page 60) state that the dry air should be checked twice a month for its moisture content, and that the alumina needs renewal about once a year. FC-066 Steel Heater Furnace for No. 2 still. Drawing 0-3479 Brick lining, coil, burners and stack. S. W. corner of the 20'6" level platform. Bldg. GR. Generally like FC-045. Drawing C-3479 (missing April 1946). DSW257534 STLCOPCB4061653 XIIo .v EQUIPMENT LIST, contd. . XII - 46 Equipment List 1-016 - 044l Instruments 1-016 Taylor Temperature Controller. Drawing D4417, Size 1, #36JR323. Direct acting, self acting, with stdo double seated valve incl. steam strainer. Range 110P. to 170P., Set 122, 25' tubing 3/4" union hub connection placed 7' from bulb end. Order B3443 on 3/10/37, Req. 76979 on 2/15/57 = Chg. out 3/31/31, $76.57. On CT-0848, Pyranol blender. 1-0108 Rotameter Instrument purchased from Economy Equipment Co. Serial #10166. For scrubber TW-0182. No. 6, Pig. 25 bronze with stainless steel float calibrated for max. cap. of 300 gph water. . Order B19959 on 11/10/37, Req. 83079. Price $66.70 1-0204 Poxboro. DP cell. Stainless Steel body. Ni diaphragm. 1-0244 1-0381 TIC, L & N. 2 point Micromax. Range changed to 0-600C. Used to replace MSC-0668. Palmer Supercar Dial Thermometer, 8" cone Mercury actuated. Range 0-150C, 25' stainless steel connecting tubing with adj. clamp, fig. to be located 9' from end of bulb. Order BI8385 on 8/23/40, Req. 12533 on 8/23/40. On 1269 stg. tk. CT-01310. Price $56.50 1-0398 Pulton Sulphon Temperature regulator #931 with 6A bulb and 20* of capillary - Bronze body stainless steel trim,,, to be used on steam at 65# pressure. Range No. 76K-190F, to 250P,, Size 1, press N. G. on CT-0748 diphenyl stg. tk. Order B23310 on 10/28/40, Req. 14583 on 10/28/40. Price $69.05 1-0441 L & N 6 point temperature recorder. Serial #389329, #40352M, Model S, micromax strip chart temperature recorder. Type DC potentiometer - multi point curve printing, record numbered and color dot for each DSW 257535 STLCOPCB4061654 XII. EQUIPMENT LIST, contd. XII - 47 Equipment List 1-0441-01118 Instruments, contd. 1-0441 contd. thermocouple. Time cycle - 50 sec. normal for each point. Order B15260 on 6/18/41, Req. 21072 on 6/17/41. Price $595*00. In second floor control room. Bldg. CR. 1-0^45 Watt hour meter instrument purchased from General Electric. Serial 21-220-745. #85 x 905. Type V5A, 220 to 5 CT use. Order B 9118 on 4/15/41. Req. 20515 on 4/14/41. Chg. out $51.40 on 6/50/41. In cabinet outside E wall Bldg. CR. 1-0507 Palmer Dial Thermometer. CABI #217, Range 0-150cC. in Pyranol Mixing Tank CT-01521. 15 ft. stainless steel special armor flexible tubing plain bulb. Order B20458 on 12/1/41, Req. 24425 on 9/9/41. Chgi out $49.59 on 12/27/41. 1-0855 Bailey Integrating and Recording Plow Steam Flowmeter. Serial #15996r. Order BII589 on 9/25/45, Req. 67905 or. 5/11/45. Price $548.00 In control room E wall. For steam from the 200 lb. main. Supplies the ejectors, the high pressure coils in the air-blowing tanks, and melter. See MSC-0682 for the low pressure steam meter. Taylor Fullscope recording controller on the No. 1 still vacuum system. Chlorine flow recorder controller on No. 5 chlorinator. See also MSC-O665, page 6l. 0668, page 6l. 0675, page 6l. 0682, page 65. 0705, page 65. 1-01118 Foxboro steam flow controller, 0 - 2000 lbs. per hour. DSW 257536 STLCOPCB4061655 XII. EQUIPMENT LIST, contd. . XII - 43 Equipment List 1-01347 - 02045 Instruments, contd. 1-01547 Taylor PR, 2 pen, with alarm and shut off valve. Chlorine lines. 0 - 100 pslg. 1-01894 1-01941 1-02019 1-02045 Taylor Fulscope TI C. 0-150#C. working at 50#C. Tin-sprayed thermo well. On blender CT-02621. Controls Fisher diaphragm valve on steam to coil in CT-02621. Pyranol blender. Fokboro. D.P. cell for chlorine liquid In store tank. Taylor Fulscope LRC. Worthington meter, gallons, well water. See also MSC - 0663 0668 0675 0682 0705 0770 01393 DSW 257537 STLCOPCB4061656 . k " XII. EQUIPMENT LIST, contd. XII - 49 Equipment List L-031 Elevators L-031 Bucket elevator from General Conveyor & Mfg. Co, Drawing E-87O. Lg. to be 22'4-11/16" OA c to c take up shafts and 20'6" casing and head section 3/16" and boot 1/46" belting, 4 ply R covered pinched 10-7/32" for buckets of 4" x 3" chrome steel. Order B10455 on 5/15/56, Req. 70140 on 5/25/56. Price $491.20. Driven by M-0834. Drive drawing B-661. Solid Aroclors (dismantled 1952). See also V44, 45, 46 conveyors from flaker D-012 to elevator L-031, and chain hoist MSC-01495 over the Sparkler filter E-0172, and electric hoist MSC-0655 for solid Aroclors. A chain hoist is used also to lift bags of lime to the still operating platform. DSW 257538 STLCOPCB4061657 v XIIo EQUIPMENT LIST, contd,, XII - 50 Equipment . List M-0790 - 0834 Motors Note; The motors are changed to other duties from time to time, but the following details will serve to indicate the types of motors used. .. H-0790 Westinghouse Motor 3 HP-1750 RPM. Serial 7435 Type CS, sq. cage induction motor, horiz., frame W225, 220/440 V* 3 ph., 60 cy., 8/4 amp., 55 C. temp,,, rise, style 801068Y, class 1, total enclosed, ball bearing. Rec`d. 8/20/35. (#6058-5077) $78.96. On pump P-0346. ` M-O827 Motor 3 HP 1200 RPM from Wagner Electric Co. Serial #1718199, horizontal induction motor, totally enclosed, fan cooled, bail bearing, 3 ph, 60 cy, 220/440 volts, 8.2/4.1 amp., type CPI, frame 254, model W425198. Order B8l84 on 4/23/36, Req. 69376 on 4/23/36. Chg. out $94.16 Also drives V-046 thru second chain on link belt; drives . D-012 flaker thru MSC-0639 speed reducer and chain. . M-0830 Motor 2 HP 1800 purchased from General Electric, Serial HK-1407, Horizontal induction, totally enclosed, fan cooled ball bearing, frame 225, 2HP 1740 RPM, 220/440 volts, 5.61/2.81 amp., type K, 3 ph., 60 cy., model SK-225-A715. Order B8169 on 4/23/36, Req. 69377 on 4/23/36. ' Chg. out $73=84 on 6/30/36. Drives P-O565. ' M-0832 Motor 3 HP 1200 RPM purchased from Wagner Electric. Serial 1714954. Horizontal induction, totally enclosed, fan cooled, ball bearing, 220/440 volts, frame 254, 3 ph., 60 cy,, type CPI, model W42J198, 8.2/4.1 amp. Order B8178 on 4/23/36, Req. 69378 on 4/23/36. Chg. out $94.16 on 6/30/36. On blower B-094. M-0834 Geared head motor 2 HP 1200 RPM purchased from Master Electric Co. Serial HE-975> air Jacketed, totally enclosed, fan cooled, 1140 to 220 RPM single reduction parallel geared head, 220/440 volts, 3 ph., frame 254, type PA, style 47476, 55 cont. rating, 6.2/3.1 amp. Drives L--031. Order B8156 on 4/24/36. Req. 69373. Chg. out $109.14. DSW 257539 STLCOPCB4061658 v - XII. EQUIPMENT LIST, contd. XII - 51 Equipment List M-0835 - 0848 Motors, contd. . M-0835 Reeves vertical motodrive 1^ HP 1800 RPM purchased from Bates Co. Motor serial 1914691, motodrive unit serial MD-1136. Size 4253-E-18, model V 34J223, 3ph, 60 cy., 1.9 amp., frame 224, 4 to 1 speed variation and 50 to 1 gear reduction, hand chain control and chain in place of standard hand wheel. Order B 7376 on 4/14/36, Req. 69123. Charged out $300.96. Drives V-044. M-0836 Reeves vertical motodrive, same as M-0835. Drives V-045. M-0841 Geared head vertical mounted motor 5 HP purchased from Master Electric Co. Serial HE-988. 220/440 volts, 3 ph., 60 cy., totally enclosed, fan cooled, ball bearing, type PA, frame 11230 # 254 DP - 1725 to 80.2 RPM Style 47478 - cont. 55C. Order B 8155 on 4/24/36, Req. 69375 on 4/23/36. Chg. out $211.84 on 6/30. Drives stirrer in blending tank CT-0779. M-0846 Vertical mounted induction motor. 1 HP 1800 purchased from General Electric. Serial EP-2773. Totally enclosed fan cooled, ball bearing, thrust type with ring base and drip cover, 3 ph., 60 cy., 220/440 volts, 1720 RPM. Model 5K204A1550. Frame 204Y. Order B 8175 on 4/23/36, Req. 69371. Chg. out $55.44. Drives P-0573. M-0847 Vertical mounted induction motor 1 Hp 1800 purchased from General Electric Co. Serial EP-2779. Totally enclosed, fan cooled, ball bearing, etc. same as M-0846. Drives P-O909. M-0848 Vertical mounted induction motor 1 HP 1800 purchased from General Electric Co. Serial EP-2777* Totally enclosed, fan cooled, ball bearing, thrust type with ring base and drip cover, 3 ph., 60 cy. 220/440 volts, 1720 RPM, model 5K204A1550, frame 204Y. . Order B8175 on 4/23/36, Req. 69371. Chg. out $55.44 Drives P-0674. DSW 257540 STLCOPCB4061659 XII. v ' EQUIPMENT LIST, contd. XII - 52 Equipment List M-0849 - 0871 Motors, contd. M-0849 Wagner horiz. induction motor 5 HP 1800 Serial #1714562, totally enclosed, fan cooled, ball bearing, type CPI, frame 254, model W-50J195* 5 ph., 60 cy., 220/440 volts 1750 RPM, 12.6/6.5 amp. Order B-8177, Req. 69572, chg. out $97.08 6/50/56 Drives P-O578. On pump P-O578, on No. 2 chlorinator. M-O85O Horizontal Induction Wagner motor 5 HP 1800 Serial 1718576 Same as M-0849 and 0851. Drives P-0579. On pump P-0579 on #5 chlorinator. M-O851 Motor same as M-0849 and 0850. Serial 1718577. M-0853 Vertical mounted induction motor 5 HP 1800 G. E. Makers. Serial FP-1104. Totally enclosed, fan cooled, ball bearing, thrust type with ring base and drip cover, 5 ph., 60 cy., 220/440 volts, 1750 RPM, model 5K225A2450, 8.54/4.27 amp.,frame 225Y, type K. Order B 8174 on 4/25/56, Req. 69567. Chg. out $95.92. Drives P-O585 M-0854 Motor Serial FP-5898 same as M-O852 and 5* on CT-O768. M-O856 Vertical mounted induction motor 5 HP 1800. Made by G. E. Serial FP-2457. Thrust type and drip cover, ring base, class 1, group d, underwriters #5474727. Explosion proof, ball bearing, 1720 RPM, 5 ph., 60 cy., model 5K225A2446, 220/440 volts, 8.42/4.21 amp., frame 225Y, type K Order B8172 on 6/26/56, Req. 69568 on 4/25/56. Chg. out $115.58 on 7/15/56. Drives P-O585. M-0871 Vertical induction motor 5 HP - 1750 RPM from G. E. Serial FP-5177. Totally enclosed, fan cooled, ball bearing, thrust type with ring base and drip cover. 220/440 volts, 15.9/6.95 amp., frame 254 Y, type K, 60 cy., 5 ph., model 5K254B1950. Order B8175 on 4/25/56, Req. 69569. Chg. out $124.21 on 7/51/56. Still pump drive, drives P-0595. DSW 257541 STLCOPCB4061660 ' XII. . EQUIPMENT LIST, contd . XII - 53 Equipment List M-0873 - 0914 Motors, contd0 M-0873 Vertical mounted Induction motor 5 HP - 1750 RPM. Purchased from Go E, Serial FP-3107. 220/440 volt, 60 cy., 5 ph., totally enclosed, fan cooled, ball bearing* thrust type with ring base and drip cover0 Model 5K254B1930, 13.9/6.95 amp., frame 254Y, type K. Order B8176 on 4/23/36, Req. 69370. Chg. out $124.21 on 7/31/36. Drives P-0592 in tank outside. M-0875 Horizontal Induction motor 1 HP 1200 made by G. E. Serial DP-5227, Totally enclosed, fan cooled, 60 cy., 1130 RPM, model 5K204A1036, 220/440 v., 3/45/1.73 amp., frame 204, type K, 3 phase. Order B13188 on 7/2/36, Req. 71152, chg. out 7/21. Drives P-0595. M-O885 Vertical mounted induction motor 1 HP 1800 purchased from Continental Equipment Co. Serial 50498. Totally enclosed, fan cooled, ball bearing, thrust type with ring base and drip cover. 2.9 amp. 3 ph,, 60 cy., 220/440 v., 1750 RPM, type NCU20. . Ordered for spare. Drives P-0604. Price $48,00. Order B-13196, Req. 71147 on 7/1/36. M-0904 Motor 3 HP - 1200 purchased from Continental Electric' Co. Serial 51704, Totally enclosed, fan cooled, normal starting current, squirrel cage induction motor, 3 ph., 60 cy., 220/440 volts, 1150 RPM, 55 cont. rise, type NP 254, 8.4/4.2 amp. Order B17431 on 9/1/36, Req. 72637> Chg. out $90.40 on 10/24. Drives B-0105 in Bldg. CR. M-0914 Blackmer motor 7i HP 1800 made by Louis Allis. Serial 217543. Totally enclosed, fan cooled, type JX, 3 ph, 60 cy., 220/440 volts, 1750 RPM, frame 284, class 53d, form B, 18.4/9.2 amp. Order B21241 on 10/22/36, Req. 74034, Chg. out $133.12 Drives Naphthalene pump P-0617 for CT-0347. DSW 257542 STLCOPCB4061661 XIIo EQUIPMENT LIST, contd,, XII - 54 Equipment List M-0955 - 01229 Motors, contd. M-0955 Portable "Lightnin-Mixer" 1/4 HP 1725 purchased from Mixing Equipment Co. Mixer Serial 57108, Motor Serial HK-4556. CABI 106/1956. Model C-4, 5" folding monel metal propeller monel shaft, 4/2 amp., 110/220 volts, single phase, 60 cy., class 1, grpup d, explosion proof, underwriters P-519572, extension cord and attachment plug. Order B1540 on 1/19/57, Req. 76212 on 1/18. Chg. out $109.42 on 2/27/57* Used for drum shipments. M-0975 M-O985 Motor 5 HP 1800 purchased from Wagner Electric Co, Serial 1725558, Totally enclosed, fan cooled, ball bearing, induction motor, type CPI, frame 254, model W50J247, 5 ph, 60 cy. 220/440 volts, 12.6/6.5 amp. cont. rating 55 C. Order B2854 on 2/9/57, Req. 76765 on 2/5/57. Cost $95.61. On P-O629. On No, 1 chlorinator pump P-0629. . Wagner Vertical Motor 7i HP - 1800 RPM. Serial #1728961. Totally enclosed, fan cooled, ball bearing, type CP-2, frame 254Y, 440V, 60 cy., 5 ph., 18.4/9,2 amp. 1750 RPM, model W40V145. Order B5525 on 2/12/ 57 and Req, 76927. Chg. out $155.98. Inst, to drive submerged pump in TCB stg. tank CT-0848. On P-0546. M-01229 Vertical mounted induction motor 1 HP 1800 purchased from Louis Allis. Serial 269797. Totally end. fan cooled, ball bearing, thrust type with ring base and drip cover, weatherproof conduit connection box, type IS, frame 204V, class L, form B. 220/440 volts, 5 ph, 60 cy., 5/1-5 amp. cont. 55C., 1750 RPM. Order B5855 on 5/4/58, Req. 86889 on 5/5/58. Chg. out $55-20 on 4/29/58. On pump P-0751. DSW 257543 STLCOPCB4061662 ' XII. .v EQUIPMENT LIST, contd. XII - 55 Equipment List M-01377 - 01575 Motors, contd. M-01377 Go Eo Motor 2 HP - 1800 RPM. Serial MR-89690 Totally enclosed, fan cooled, sq. cage, induction motor, type K, ball bearing, 220/440 V, 60 cy., 3 pho, frame 254, 1760 RPM,-model 5K254B91o 5.44/2.72 amp. Order B15955 on 9/26/38, Req. 91711, Chgo out $75.00. On P-01111. M-01456 Westinghouse horizontal motor 3/4 HP 1200 Serial 4139 Totally enclo fan cooled, low starting current, 440 volts, 3 pho, 60 cy'., ll60 RPM. Type GS, frame 204, 206/1.3 amp., style 1707136.# 55C. rise, Chg. out mach. $41.03 on 12/29/39 Order B17367 on 12/18/39i Req. 1357 on 8/31/39 - on Blower B-0148. M-01469 G. E. Motor 3 HP-1200. Serial #KT-10671. Totally end. fan cooled, model 5K254A1024, frame 254, type K, 220/440V, 3 ph., 60 cy, ' 1165 RPM, 9006/4.53 amp., cent. 55C. rise. Order B18935 on 9/21/39, Req. 1991 on 9/20/39. Chg. out $72.47 on 11/30/39. On gear pump to P-0159. M-01486 M-01501 M-01575 General Electric Motor 1/4 HP 1800, totally end., model 5 KH47AB984, type KH, 110 volts, single phase, 3.4 amp., 55 0 Cont. Order B17923 on 10/L7/59, Req. 1551 on 9/8/39. Cost $24.25. 1 On Lectrodyer PC-046. Replaced by M-OI706. . Motorized car spotter 5 HP 1640 RPM purchased from Link Belt Co. motor serial 307959, spotter serial 5252. 220/440 volts, 60 cy., 5 ph, type IK, frame 225 VY, class 3, form B, 17.2/8.6 amp. 55C. Order B26741 on 12/29/39, Req. 5128 on 12/29/39. Chg. out $375.86. On track 11 at load dock. DSW 257544 STLCOPCB4061663 XII. EQUIPMENT LIST, contd. XII - 56 Equipment List M-01622 - 01660 Motors, contd. M-01622 General Electric motor 7i HP, 3600 RPM, Serial BU7108. Totally enclosed fan cooled, type KF, model 5KF254C25, frame 254, 220/440 v,, 3 ph., 60 cy., 3435 RPM, Drives ML-045. Order B4ll8 on 2/20/40, Req. 6737 on 2/0. Chg. out $114.96. M-01629 Vertical motor 7i HP purchased from Turbo. Made by Westinghouse,, Serial 2640. Totally enclosed, fan cooled, frame 284, class 1, RPM at full load 1735, cont. rating at full load 55C,, rise, 220/440 volts. 3 ph, 60 cy., 18.8/9.4 amp., style 1071192. Order B83.37 on 5/20/40, Req. 8441 on 4/9/40, chg. out $112.66. On MSC-01205. Driving agitator in CT-0808, .final chlorinator. M-OI65O Louis Allis motor HP, serial 258334, 1750 RPM, type JS, frame 254, class 43N, form B, 220/440 v,,, 3 ph, 60 cy., 13/6.5 amp., full load 55C. cont. Order B26263, Req. 85432 on 12/24/37= On Sparkler press pump. M-OI656 Wagner Electric Motor 5 HP 1800 RPM Serial 1758959= Horizontal totally enclosed, fan cooled, ball bearing, less base and pulley, type CPI, frame 254, 220/440 v., 3 ph., 60 cy., 1750 RPM, cont. rating 55CP, model 1E8J247B, 13=2/6.6 amp. Order B12802 on 7/8/40, Req. 10231 on 6/5/40, chg. out $87=92. Drives P-OIO56 Taber Horizontal pump. M-01660 General Electric Motor 1 HP 1800 RPM purchased from Taber Serial GU1902. Totally enclosed, fan cooled, vertical mounted, ball bearing, thrust type, with ring base and drip cover, 3 ph, 60 cy., 220/440 volts, 1720 RPM, model 5K204A1550, frame 204Y, type K, 3=11/1=56 amp., cont. 55C. rise Order B13111 on 6/10/40, Req. on 6/10/40, chg. out $50,19= Drives new Taber sub. pump P-0909= DSW 257545 STLCOPCB4061664 XII EQUIPMENT LIST, contd . XII - 57 Equipment List M-01697- 0177-2 Motors, contdo M-OI697 Motor made by Wagner 1/5 HP, CABI 169, 50" dia. type S-60WS, style 1249-4622 portable circulating fan, single ph,,, 60 cy., 115 volts, complete with guards, T^loor column, and cord, BI6528 on 7/26/40. Req. ' 11797 on 7/26/40, Chg, out $60.58. Used on operating platform near chlorinator, ' M-01706 . M-01718 Vertical mounted induction motor 5 HP 1800 made by G, E, serial JU5498. Totally enclosed, fan cooled, ball bearing, thrust type with ring base, and drip cover, model 5K225A4264, frame 225VY, type K, 220/440 v,, 5 ph,,, 60 cy,, 1750 RPM, 8.54/4,27 amp,, cont. 55C, rise. s' Order B18445 on 8/25/40, Req. 12560 on 8/25/40. Chg. out $92.24 on 10/51/40. On P-0929 Taber. Replaced by M-01501. Louis Allis Motor 7i HP-1800 RPM, Serial 555985. Totally enclosed, fan copied, weatherproof conduit, connection box. Type JX, frame 284, 220/440V, 5 ph.<, 60 cy., 1750 RPM, Class D, form R, 19,6-9.8 amp., full load temp, rise 55C,. trine hours cent. Order B21071 on9/50/40, Req. 15674. .. Chg. out $115.00 on 10/51/40. Drives (Falk Reducer MSC-01288) on Turbo Mixer for CT-01521. . M-01752 Motor 1 HP-1800. Serial 77640. Totally enclosed, ball bearing, squirrel cage, weather proof threaded type connection box, type CS, frame W-204, 220/440 v., 5 ph., 60 cy., .1750 RPM. ' Order B26550 on 12/4/40 and Req. 15856. Chg. out $56,98. On B-O54. M-01772 Lewis Motor 1/2 HP 5600 made by G.- E. Serial J55, CABI 169, totally end., model 5K49BG756A, type K, <55C., 440 v., 5 ph., 5450 RPM, amp. 7. Chg. out $25.00, Req. 16665 on 12/50/40. Use with P-0578 on OT-0640. ' rise DSW 257546 ! STLCOPCB4061665 XII o E SHIPMENT LIST, contdo XII - 58 Equipment List M-01811 - 01995 Motors, contd o M-01811 Louis Allis Motor 2 HP 1800 RPM Serial 585555= Totally enclosed, fan cooled, normal starting current. Cl conduit connection box, less base and pulley,, 220/440 volts, 5 ph., 60 cy., 1750 RPM, type JS, frame 225, class M, form R, code H, 5=6/2.8 amp. Order B4156 on 5/7/^l* Req. 18515 on 2/17/41 Chg. out $65=56 on 6/50/41. . On ground floor N. E. of P-0172 on P-01057= M-01850 Louis Allis Motor 1 HP 1800 RPM Serial 595205 Totally enclosed, fan cooled, ball bearing, 220/440 v., 5 ph=, 60 cy., 1740 RPM, type IS, frame 204, class L, form B, 5.1/1=55 amp. Order B7411 on 5/26/41, Req. 19654 on 5/26/41. Chg. out $56.98. On ground floor. M-OI856 Louis Allis motor 5 HP 1800 RPM Serial 591009. Totally enclosed, fan cooled, vertical flgd. mounted (Cl conduit connection box) normal starting current, 5 ph, 60 cy., 220/440 v., 1750 RPM, type JS, frame 254 VB= class N, form R, code H, 1.5/6.5 amp. full load temp, rise 55C. Order B658O on 5/15/41, Req. 19215 on 5/15/41. Chg. out $109=7^ on 6/50/41. On P-0997 top of S-062. M-01859 Unit heater from Am. Blower Corp. Serial 1959= Order B8956 on 4/11/41 and Req. 20240. Chg. out $48.75= In MSC-01593 = M-01995 Motor 1/5 HP 1800 RPM made by G. E. Explosion Proof, class 1, group d, underwriters No. FA552-094. Totally enclosed, fan cooled, ball bearing, type K, frame 45A, model 5K45AC1024A, temp, rise 55C. trine rating cont., 440 v., 5 ph, 60 cy, 1725 RPM, 55 amp. Order B4625 on 2/21/41, Req. 18520 on 7/21/41. Chg. out $29=75 on 9/50/41. On P-01054. DSW 257547 STLCOPCB4061666 XII. -1 ' EQUIPMENT LIST, contd. XII - 59 Equipment List M-02170 - 0514 Motors, contd. M-02170 Geared head motor 5 HP 1800 RPM. Made by Master Elec. Serial PD-9. Parallel, air jacketed, fan cooled, totally enclosed, frame # 254, 80 RPM on mixer shaft, barrel mounting for vertical operation, style 105545, 220/440 v., 5 ph., 60 cy., 1725 RPM, type PA, amp. 13/6.5> 3 ph, trine hours cont. PLTR 55C. Order B5580 on 4/8/42, Req. 50060 on 2/10/42. Chg. out $259.25. On CT-01599, #2 blender. M-02175 M-02877 M-05133 Office Pan. Drives P-01111 at loading dock - 5 HP* Drives P-01540. M-04592 Drives Side entering agitator in #2 mix tank CT-02621. M-04691 Drives P-02077 at TTCB storage. M-04817 Exhaust fan - located in pyranol press room. M-04025 Drives P-02077. M-0514 Drives P-02251. DSW 257548 STLCOPCB4061667 .v XII. EQUIPMENT LIST, contd. xii - 6o Equipment List ML-045 Mills ML-045 "Helix-Seal" impact mill purchased from Williams P. C. & Pul. Co. Serial #9394. Size #1. Less drive pulley-Driven at 5500 RPM thru V belt drive furnished by Monsanto. Order B2371 on 2/1/37- Req. 76578. Price $420.00. West lean-to. Hand fed. For solid Aroclors. Dismantled 1952. DSW 257549 STLCOPCB4061668 ' .v ` XII. EQUIPMENT LIST, contd. XII - 6l Equipment List MSC-0639 - 0675 Miscellaneous Equipment MSC-0639 Speed reducer made by W. A. Jones Foundry, Serial 85957, #105DW, assembly #1, style 4, 56 to 1 ratio, low speed shaft to be 7i" instead of 4" extension. Order B8242 on 4/24/36, Req. 69409 on 4/24/36, Price $156.00 Driven by M-O827, drives D-012. CR, lean-to.t. MSC-0655 Shepard Electric Liftabout Hoist. Serial 36306. 440 volts, AC, 3 ph, 60 cy., single speed control with motor drive trolley. Hoist speed 18' per min., lift 19'. Hoist motor 3 HP. Travel motor 3/4 HP. Order E7405 on 4/14/36, Req. 69120. Chg. out $906.70. MSC-0663 Multiple temperature recorder 40112-291 Micromax Model S strip chart, 2 prints, surface panel $300.00. Made by Leeds and Northrup, Serial 276758* Order B9975 on 5/19/36, Req. 69970. In lean-to. Bldg. CR. MSC-0668 MSC-0675 L & N Temp. Recorder made by Leeds and Northrup. Dwg. B-666, Serial 276807. (1) #40354-291 Micromax model S strip chart, multiple temp, recorder, 4 point. (Multiple colored dots instead of numbers on print wheel). Surface panel mounting $465.00. (2) Extra for high contact for operating alarm $20.00 Order B9976 on 5/19/36, Req. 69969, Chg. out $491.82. South wall, west instrument. Bldg. CR.(See note on next pg.) Replaced by 1-0244. Temperature Recorder purchased from Leeds and Northrup. Serial 276784. #40353-291 Micromax, model S, strip chart multiple point temperature recorder for 3 prints. (Multi-colored dots instead of numbers on print wheel.) Surface panel mounting $400.00. Extra for high contact for operating alarm, $20.00. 3 thermocouples to fit wheels. Our Dwg. B-666. Order B9977 on 5/19/36, Req. 69968, Chg. out $324.05. South wall, east instrument. Bldg. CR. (See note on top of next page.) DSW 257550 STLCOPCB4061669 XII. -v ' EQUIPMENT LIST, contd. XII - 62 - Equipment List MSC-0668 - 0676 Miscellaneous Equipment, contd. MSC-0668 -0675 Note: . Record the following temperatures: Batch temperatures in chlorinators: CT-0744 0745 0853 01283 0808 Goods temperature in diphenyl store tank CT-0748 Coil inlet temperature on the stills S-043 and 062. " outlet " " " " "" Vapour temperature entering the condenser. Goods temperature in receiver. Goods temperature in blending tank, CT-0779. Goods temperature in finished product receiver,CT-O78O. Drawing B-666 shows thermo-couple wells. Drawing B-6868 shows monel thermo-couple wells as used in distilled Aroclors. MCS-O676 Gas Electric Water Cooler for drinking water. Made by G. E. Compressor 6541356, cabinet 6600807. Model RM-51, pressure type, 110 v., single phase, 60 cy. Order B14045 on 7/14/36, Req. 71432. . Chg. out 7/31/31, $176.00. On 12' level. Bldg. CR. SW 257551 STLCOPCB4061670 XII. EQUIPMENT LIST, contd. XII - 63 Equipment List MSC-0681 - -75^ Miscellaneous Equipment, contd. MSC-0681 Rail truck purchased from Nutting Truck Company. Dwg. C-827. Welded construction, wheels equipped with Hyatt Roller Bearings. Used as weigh truck for still pots on SC-095. Includes track. Order B11134 on 6/3/36, Req. B70395. In lean-to Bldg. CR. MSC-0682 Brown mech. flowmeter. Serial 115969. Recording and integrating steam at 65# ga. press. Dry sat. orifice monel in 4" std. horiz. line, (used on 80 lb. main). Max. flow 4000#/hr. Model 2221-x40. 2 lgs. 25' of copper tubing and connectors - Monometer valves. Elec, clock for 110 v - 60 cy. Order B14604 on 7/22/36, Req. 71548 on 7/20,, chg. out $280.00 MSC-0705 Palmer Industrial Thermometer CABI #89 #249 - 45 reclining industrial therm. 12" scale, steel separable socket - 30" long with 1" std. pipe thread. Range 0-200C. No nickel plating, case painted reg. lacquer. Order BI8261, chg. out $28.05 on 10/31/36. On Buffer tank CT-0750. MSC-0718 Lab and Office of Dept. CABI #89 - 1936. 20' x 10' x 10' high includes partition and elec, lights on NW corner of CR. MSC-0725 Laboratory testing equipment. See reports on G. E. testing. MSC-0734 . Electric drying oven. CABI 89-1936. Cat. 7764, 3 heat oven with one shelf and 9525 thermometer for. 110 v., AC current. Belongs to the Pyranol Dept. Order B23080 on 11/16/36, Req. 74628. Chg. out $26.60. DSW 257552 STLCOPCB4061671 . . .V ' XII. EQUIPMENT LIST, contd. XII - 64 Equipment List MSC-076O - 0903 Miscellaneous Equipment, contd. MSC-O76O Vacuum jet made by Worthington. #2^ JPD-S std. 3 stage steam jet. ejector with 2nd stage condensing and fitted with jet type intercooler. Jet to be Cl bronze nozzles, heads, monel nozzles. Order B7404 on 4/14/36, Req. 69211 on 4/l4. Chg. out $796.00 on 6/30/36. ~ N of MSC-01392 Bldg. CR. Ejectors MSC-O76O, 01392, and 01686 are in a row running north and south in the building, and they are inter connected so that the centre one can serve as a spare ' for either of the other two, to serve the vacuum stills S-043 and 062. Cast iron bodies with monel jets. Karbate ejectors were to be tried. (Anniston were using ejectors with two stages of Karbate jets, then a wet condenser, and then two more Karbate stages.) Faulty behaviour, due to erosion or corrosion, or to wet or dirty steam, is very objectionable as allowing water to get back into the goods. Karbate units have to be very carefully supported to prevent strains from the pipe lines. More recently procelain units have been installed at the Krummrich plant. MSC-0770 Super Tank Gauge made by Varec. Fig. 68, Gastight. Use on tank according to B/P E-4366, Monsanto Drawing. All material to be standard, aluminum float, stainless steel tape and float guide wires. Order B3569 on 2/16/37> Req. 77035* Chg. out $174.80. On CT-0848. TCB store tank. MSC-0903 Steel cabinet made by Medart. CABI #139. 1 unit 48" wide and 24" deep x 6'3" high 9" ledge,bin fronts, dividers and 2 doors on lower part with lock. Order B3013 on 2/18/38, Req. 86579 on 2/17/58. Chg. out $50.51. ' DSW 257553 STLCOPCB4061672 XII. v ' EQUIPMENT LIST, contd. XII - 65 Equipment List MSC-0971 - 01592 Miscellaneous Equipment, contd. MSC-0971 10 steel box lockers made by Medart. CABI 139. Olive green steel arranged 2 wide x 5 high. Complete with locks, 2 keys for each lock x 3 master keys common to . all. Lockers 12 x 12 x 15" deep. Order B15781 on 9/23/58, Req. 91603 on 9/21/38. Cost $25.75. MSC-01061 Two loading ramps made by Monsanto. For one ton chlorine cylinders, using I-beam supports and concrete footings with I--beam rails. East side, outside Bldg. CR. MSC-01094 Drying Oven purchased from G. E. Used with F-0159-in the Pyranol plant. 4 compartment electric drying oven with 115-230 volt heating elements. 3 HP motor. Order B18955 on 9/21/59, Req. 1991 on 9/20/39. MSC-01191 Metal Desk and Stool. Desk 36-5/32" wide, 42" high front, 54" high back, 31" deep. Stool 30" high. Order B5169 on 3/4/40, Req. 7148 on 2/29/40. MSC-01205 Speed reducer made by Falk. Serial M0127-928. Size 28DZX, RPM 1750 to 180, ratio 9.7. Order B8337 on 5/20/40, Req. 8941 on 4/9/40. Chg. out $169.94. Driven by M-01629 on CT-O808. MSC-01288 Falk Motor Reducer 7i HP. Serial M0131-842. #44DZX, output speed 1750 to 41.9 RPM, service factor l-j, ratio 41.9. Order B21071 on 9/50/40, Req. 13674 on 9/50/40. Chg. out $341.94 on 10/31/40. On CT-01321, Pyranol blender. MSC-01592 Worthington vacuum jet 3 stage. North of MSC-0760. Same as MSC-01686. Type 9-10-11. DSW 257554 STLCOPCB4061673 ^ XII. EQUIPMENT LIST, contd. XII - 66 Equipment List MSC-01595 - 02108 Miscellaneous Equipment, contd. MSC-01595 Control Room. Drawing C-9646. Structural steel, floor plate. Bldg, tile 12 x 12 x 3. Pyrobar roof, door and Instrument panel for 1-0441. MSC-01495 i ton Peerless hoist and trolley. Model C, 11' lift. Model J trolley. Order B17508 on 8/6/41, Req. 23095 on 8/6/41. Chg. out $72.74 on 11/27/41. Used to remove plates of filter P-0172 for cleaning. MSC-01686 #2-| Worthington 3 stage vacuum jet. Type 9-10-11. North of MSC-01392. Same as MSC-01392. MSC-01699 Lockers (4) made by Medart. CABI 152,1959. 2 only 15 x 18 x 60 dark green, #14 and #15. 2 only 15 x 15 x 36 double tier. #12 and #13. Order B3439 on 3/8/39. MSC-01877 Canvas tent for tank car. Approx. 7' dia. x 7' high with swing boom, to raise and lower tent into a wooden box along west wall of CS. To be located at load dock at track #11, SW corner CS. Also elec, light in tent, order B20696 on 9/7/^5, Req. 48441. on 9/V^5. MSC-01879 South dock, wood, muriatic loading. Also swing plank and wood decking. On track 11 west of CS. 5' x 5'6". 19^5. MSC-01916 North load dock made of steel with swing plank. 5' x 7' long, 9'6" high. 5x5 angle columns with 6" channels to support steel decking. l" pipe railings. North of MSC-01879. SW of CS on track 11. 1956. MSC-02071 Stoneware sink. MSC-02108 Steel Hood and Duct. 2! x 4' counter balanced with 6" dia. steel duct to outside of Bldg. Hood located over P-0159 G. E. Filter Press. DSW 257555 STLCOPCB4061674 k v XII. EQUIPMENT LIST, contd. XII - 67 Equipment List MSC-02426 - 04442 Miscellaneous Equipment, contd,, MSC-02426 Ducts, hoods, dampers. MSC-05417 Air cond. unit. MSG-05523 Vac. ejector. Worthington, Porcelain, Karbate. 10" Porcelain condenser. 10 lb. hr. air at 2 mm cbs. 150 psig steam. 65F,, well water. MSC-03611 Duct and hood. MSC-03689 Haveg sink. 4' 8" x 19" x 18". MSC-03706 Water cooler. Drinking water. MSC-03741 MSC-03835 MSC-04018 1/2 T chain hoist above F-0172. ] 'L 1/2 T chain hoist - #2 mix tankj _,. Pyranoi plant Work bench MSC-04109 Lightnin mixer (only - not motor) HP side entering metallized with 0.015" Al. See CT-02621. MSC-04132 Water cooler. MSC-04442 Hand hoist. Heaters for plant office and for instrument and control Gas supply and metering. room. Water hose with steam mixing jet for cleaning the floor. Desks. Clothes lockers. Test bench. Phone. Clock. Framed instructions for special pieces of equipment. Drinking water supply. First aid cabinet. Fire alarm & extinguishers.Sprinklers installed in all Hose connections for casual gas heating. rooms. Waste cans. Used water collection. Lighting. DSW 257556 STLCOPCB4061675 XII - 68 Equipment List 0T-0640 - 0751 XII. EQUIPMENT LIST, contd. Open Tanks 0T-0640 Drum, 110 gal. ICC5, CABI #217-1941. With float valve on city water line. Connect 5 GPM pump P-0578. To pump from drum through rotometer to acid absorption system. Black Iron $18.50 as trans from Dept. 560. Seal cans for barometric legs of the ejectors. MSC-O76O, -01292, -01685. On the ground floor. 0T-0751 Steel vessel 4'0" I.D. x 6'0" high, for city water, to conform to state law. . DSW 257557 STLCOPCB4061676 XII. v ' ' EQUIPMENT LIST, contd. XII - 69 Equipment List P-0546-0575 Pumps Note: The pumps are changed around from one duty to another, in the course of ordinary maintenance work, but the details given below will serve to show what type of pump is used for any given duty. Oversized pumps may be used in some cases to diminish the number of types re quired in the department. . P-0546 Swaby Submerged Pump made up 11/18/29. Size #l|-, Cast Iron. On CT-0848. In TCB store tank, CT-0848. P-0578 Chas. Lewis pump Serial 4597, Type BA-481, cast iron vertically split shell cent. pump. Cl bed plate connected with flex, coupling, direct to 1/4 HP 5600 RPM motor. GE M-0466, 5 gal. PM - 55' head, 5450 RPM. Order B695 on 1/15/51. Price $68.00 incl,motor, M-01772. Boosts city water to HC1 absorber. P-0427 Horizontal cast iron pump HP Monsanto Design. Direct connected, cold rolled steel shaft, includes base, coupling and c guard. P-O565 Blackmer pump. Serial 197055, type PA-50L bronze rotary pump, bronze lining, bronze steam jacketed heads, monel shaft. Cl base, I.65 sp. gr., temp. 550 to 500F. - 50 gal. Order B-8170 on 4/25/56. Chg. out $155.45 on 6/50/56. Distillate transfer pump. P-0571 P-0573 Oberdorfer gear pump for filter press. Motor M-OI65O. Vertical submerged centrifugal pump purchased from The Engineering Equipment Co. Serial 55007, Size L-OB with l" inlet and 1" outlet. Compare P-0604, which is a Taber pump on #4 scrubber CT-0759. P-0574 Ditto. P-0575 Taber submerged pump. Serial 55009. Order B7517 on 4/16/56. Req. 9161. Chg. out $177.80 on 6/50. Direct to vertical M-0848 in CT-O756 on #1 scrubber. Same as P-0575 and 0574. DSW 257558 STLCOPCB4061677 XII. EQUIPMENT LIST, contd. XII - 7 0 Equipment List P-0578 - 0580 Pumps, contd. P-O578 Taber horizontal centrifugal pump. Serial 33040. Type L-2, 2-|" inlet 2" outlet connections. Semi-steel with monel shaft and water jacketed stuffing boxes. Bed plate ready to receive motor. 20' static head, rate 80 g.p.m'. 1.5 sp. gr. at 500P. Uses M-0849. On #2 chlorinator, CT-0744. Order B8237 on 4/24/36, Req. 69401. Chg. out $152.92 on 6/30. There are four pumps P-0578, 0579> 0629 and 0907, one for each main chlorinator. Liquor in from chlorinator bottom outlet and out back to the chlorinator. The charge can be pumped, if necessary, from one chlorinator to another, or to the air-blowing vessels CT-0750 and CT-2086. No. 1 chlorinator can be emptied by gravity to the gas-fired chlorinator CT-0808, and there is also a pump line for the same service (disused). The charge from No. 1 chlorinator can be pumped directly to No. 1 vacuum still S-043. There is a line by which partly chlorinated diphenyl can be pumped from a chlorinator to any scrubbing tank, CT-0759, -0760, -0761 or 01014. There is a sampling cock on each pump delivery, with a small box to hold the used sample material, and to deliver it back to the pump intake. P-0579 Taber horizontal centrifugal pump. Serial 33041. Same as 0578-80. For middle chlorinator CT-0744, uses M-0850. On #3 chlorinator CT-0833. P-O58O Taber horizontal centrifugal pump. Serial 33042. Same as 0578-79. From blow tank CT-0750. Uses M-O85I. DSW 257559 STLCOPCB4061678 XII. EQUIPMENT LIST, contd. XII - 71 Equipment List P-0582 - 0593 Pumps, contd. P-O582 Taber vert, submerged centrifugal phmp.'- Serial , 35048. , Pig. 1940, size C-3, 2^" inlet, 2" outlet connections, bronze except shaft which is monel metal. 11'6" length of column pipe. Spare pump for underground tanks. Order B7514 on 4/16/36, Req. 69158. Chg. out $409.20. Direct to M-O852. Same as P-O583 and 0584. Used in Arocior 1260 store tank. Submerged pump in CT-O768 TCB store. P-O583 Taber vert. subm. cent. pump. Serial 33049. In CT-O769, direct to M-0853. Same as P-0582-0584. Arocior storage. P-0584 P-O585 Taber vert. sub. cent. pump. Serial 33050. In CT-O768, 1254 store tank, direct to M-0854. Same as P-O582 and 0583. Taber vert. sub. cent. pump. Serial 33069, Dwg, A387, Type C-3, fig. 1940, 2" inlet and outlet. Cl body, renewable, bronze bearings, bronze impellor mounted on nickel steel shaft. Length 11'6", sump cover plate, cap. 50 gal. p.m., 60' static head, sp. gr. 1.18 at temp. l65-170P. Driven by M-O856. in CT-0748, Diphenl store tank. Order B7518 on 4/16/36, Req. 69162. Chg. out $257.62. P-0592 P-0593 Taber vert. sub. cent. pump. Serial 33113* type C-3, Pig. 1940, 2" inlet and outlet. All Iron construction on nickel steel shaft length 11'6". Cqp. 50 g.p.m., 60' static head, sp. gr. 1.368 at 70 to 90P. In CT-0749f driven by M-0873. Order B7516 on 4/16/36. Req. 69160, chg. out $255.41. * general service and diphenyl tank. , Taber vert. sub. cent. pump. Serial 33111. Type L-2, fig. 1940, 2^" inlet and 2" outlet, casing, yoke, impellor made of steel shaft nickel steel, column supporting intermediate bearing, wrought iron. Length 7'9". DSW 257560 STLCOPCB4061679 XII, EQUIPMENT LIST, contd. XII - 72 Equipment List P-0595 - 0629 Pumps, contd. P-0595 contd. Cap. 75 GPM, static head 15', sp.gr. 1.8 at temp. 700F. Driven by M-O87I. On Number 1 still. Order B7515 on 4/16/56, Req. 69159. Chg. out $582.91. In still S-045. Same as P-0574. Sump plate. Drawing A-495. P-0594 Spare motor same as P-0595. Serial 55112. Driven by M-0872. P-0595 Oberdorfer gear pump. Serial 2855. #7AXZ unloader pump, all bronze gear type. 10-15 GPM at 20# pressure. Used to circulate Aroclor on No. 1 still cooling system. Order B15188 on 7/2/56, Req. 71152. Cost $78.80. . P-0604 Vert. sub. cent. pump. Taber. Serial 55207, Size L-OB, l" inlet and 1" outlet. All iron const., open impellor on nickel steel shaft. Same as P-0575-4 and 5. In CT-0754. Order B15195 on 7/2/56, Req. 71148 on 7/1/56. On #5 scrubber, CT-O76I. P-0615 Blackmer Pump Serial #201747. Size 502, 50 gallon per min. right hand rotary gear pump. Bronze with bronze liner and monel shaft. Steam jacketed heads. Order B20818 on 10/16/56. Req. 75912 on 10/16/56 Chg. out $148.27 on 11/50 Direct to 5 HP 1800 M-01449. On filter press F-0159. P-0617 Blackmer pump. Serial 201902. Size 100L, all iron, jacketed right hand pump, base plate for motor, and flex, coupling, direct connected (M-0914). Order B21241 on 10/22/56, Req. 74054. Chg. out $145.20. Spare pump, P-0629 Taber horiz. cent. pump. Serial 55708. Type L-2, 2^" inlet and 2" outlet. Size 105. Order B2855 on 2/9/57. Req. 76766 on 2/5/57. Chg. out $152.52. Direct to M-0975. On No. 1 chlorinator. DSW 257561 STLCOPCB4061680 XII. EQUIPMENT LIST, contd. Pumps, contd. XII- 75 Equipment List P-0674 - 0984 P-0674 On #1A scrubber, CT-01015> driven by motor M-0848 on No. 1 chlorinator. P-0731 Taber sub. cent. pump. Serial 84722, Size L-OB, l" inlet and 1" outlet. Order B5854 on 3/4/38, Req. 86891 on 3/3/38. Chg. out $174.25. . In CT-01013. P-0907 Taber horiz. cent. pump. Serial 36622. Size 103, type L-2, 2-j?" inlet and 2" outlet connections, semi-steel through out with monel shaft and water jacketed stuffing boxes, with bed plate ready to receive motor, 20' static head, rate 80 GPM, 1.5 sp. gr. at 500P. Order B12801 on 6/5/40, Req. 10250 on 6/5/40. Chg. out $155.28, driven by M-OI656 to circulate liquor for chlorinator CT-01285> #4 chlorinator. P-0909 Taber sub. pump. Serial 36676. Size L-OB with l" Inlet and 1" outlet, all iron const., open Impeller on nickel steel shaft. Order B13110 on 6/10/40. Req. 10366 on 6/10/40. Chg. out $193.75. On CT-O968 scrubber liq. tank. Also on CT-O76O. P-O929 Taber sub. pump. Serial 36853. Size C-3, fig. 1940, vertical 2^" inlet and 2" outlet. Bronze except shaft to be monel metal, lg. of col. pipe 11'6". Order B18442 on 8/25/40. Req. 12559 on 8/25/40. Chg. out $404.59. On stg. tank CT-01510. Driven by M-OI706. P-0952 Roper cast iron pump. RIBI #169. Size 1" rotary, geared, complete with base, gears, pinion, big stand and adapter plate for motor mounting. P-0984 Roper pump. All iron series "0" rotary pump for 15 GPM. 1.6 sp. gr. 50' head pump, spiral gears pkgd. stuffing box with non-graphitic white asbestos pkg. built in by-pass and complete with base, drive gears. Order B4ll8 on 2/17/41, Req. 18522 on 2/17/41. For filter in CR; On Sparkler filter F-0172. Replaced by P-0571. SW 257562 STLCOPCB4061681 XII. EQUIPMENT LIST, contd. XII - 74 Equipment List P-0997 - 01258 Pumps, contd. P-0997 Taber vert. sub. pump. Serial 57682. Type CL4, 2\" inlet and 2" discharge for 75 GPM against 25' head. Pump of dynamo steel with wrought iron pipe column and nickel steel shaft, water cooled, stuffing box. Order B6579 on 5/15/41. Req. 19214 on 5/15/41. Chg. out $446.55. In S-O62. Driven by M-OI856. Shaft has two intermediate C.I. bearings. P-01057 Blackmer pump. Serial 246058. 5WG5202 bronze, size 51L with base and relief valve. Still receiver to blender. Order B16097 on 7/21/41. Req. 22429 on 7/21/41. Chg. out $177.56. On gr. fl. NE of P-0172. P-01054 . Pump made by Weil. Serial 15152. Type DSI, size 1". Uses city water. Order B4625 on 2/21/41. Req. 18520 on 2/21/41. Cost $65.00. On TW-0221. Driven by M-01995. P-OIO56 Taber horiz. cent. pump. Serial 58518. Type L-2, size 105, 2\" Inlet 2" outlet complete with base. Order B19730 on 9/5/41, req. 24125 on 9/2/41. Chg. out $157.44 on 4/51/44. On #4 chlorinator CT-01285. P-01111 Blackmer Pump Serial 249115. #5 OL all iron steam jacketed pump with Cl base plate and gear drive ready to receive our 5 HP 1800 RPM motor size 511. Order B16549 on 7/25/41, Req. 22597. Chg.out $105.05. Driven by M-02877. For discharging rail tanks. P-01258 Blackmer pump. Serial 269500, Size 1202-50. Fig. 5205 complete with relief valve. No base. #2 still receiver to blending tanks. Order B29505 on 1/28/45. Req. 40512 on 12/50/42. Chg. out $154.65. Bronze. DSW 257563 STLCOPCB4061682 v XII. EQUIPMENT LIST, contd. XII - 75 Equipment List P-01277 - 02251 Pumps, contd. P-0I277 Taber vert. sub. cent. pump. Serial 40890. Type CL-4, 2^" inlet, 2" outlet, size 584. Pump to be dynamo steel with wrought iron pipe, column cap. of pump 75 GPM at 25' head for liquid 1.8 sp. gr. Order B8875 on 7/12/45, Req. 45713 on 4/16/45. Chg. out $454.00 on 12/27/45. At S-062 Spare. Same as P-0997. #2 still pump (spare). P-01509 2" Taber pump. 80 GPM. 150 ft. TDH. Shaft. Flexible coupling. M-05014. S. G. 1.5 500F. Steel with monel P-01540 G. E. Filter pump - N. W. comer of lean-to. Taber pump 504 stainless steel, 2" suction, l|-" discharge. Located indoors. Pumps from old Pyranol blender CT-01521 to filter presses. P-01757 On Sweetland filter F-0259. Now used on F-0258. 504 stainless steel 2", 100 gpm. Motor M-05718. P-02052 2" Taber. Semi-steel, monel shaft, water jacketed stuffing box. 1.5 S. G.,500F. P-02077 P-02078 Blackmer pump, from TTCB store to blenders. Bronze lined, with monel shaft. N.W. of Bldg. CR. Taber 5" x 2^" 150 gpm. 80 ft. head. Horizontal impeller. P-02179 Taber Pump from new blender CT-02621 to filters. Motor M-04025. P-02251 Viking pump on Aroclor mixers. M-0514. Pyranol plant. DSW 257564 STLCOPCB4061683 XII. EQIPMENT LIST, contd. XII - 76 Equipment List Pumps, contd. Note : London Engineering Dept. Final Report on the start-up of the Newport Aroclor plant states that Hamworthy pumps were not found satisfactory in use. Good jacketing is needed. There was trouble from corrosion of core plugs in some pumps, leading to leakage of steam into the goods. Steel end covers were used later. The same reports discuss the difficulties encountered with the still pump, which was located in a small secondary vessel, below the vacuum still. DSW 257565 STLCOPCB4061684 XII. EQUIPMENT LIST, contd. XII - 77 Equipment List R-026 - 027 Retorts R-026 Aroclor 1269 Retort assembled and erected by Monsanto. Pots from Nooter. $516.00 for 4. Jacket from Graver. Req. B69906. Burners from Surface Combustion. Req. 69374. Burners - gas fired. ' Jacket, steel, firebrick lined, holding 3'0" OD x 3'8" lg. over dished bottom still pot with cover. Equipped with 2 gas burners and stack. Still pot 1/2" fire box steel,removable so residue can be dumped. R-027 Aroclor 1269 Retort - Same as R-026. Drawings: B-646 E-865 B-374 C-830 C-821 Retort. Setting. General arrangement of solid Aroclor plant. Gas heater for discharge line. Platform for retorts. Mr. Soffranko In 1947 commented that the retorts would be better with thicker bottoms than shown In drawing B-646, and that spare retorts should be held. DSW 257566 STLCOPCB4061685 XII. EQUIPMENT LIST, contd. XII - 78 Equipment List S-045 Stills S-045 No. 1 Vacuum still purchased from Graver. Plant A Drawing C-809. Size 6' dia. x 5'6" long on straight side, 1/2" shell, dished head 5/8" supporting brackets 60# Hydro press test. Order B-7705 on 4/17/56, Req. 69225, Chg. out $556.00 on 2nd floor, 12' level. S-045, No. 1 still, at the Krummrich plant, is of the shallower type, like the Anniston stills, and like them it has a vertical vapour pipe (with Hagan separator inside the still), leading to the top of a vertical condenser, CT-0770, whereas No. 2 still is of the deeper type, and has a cyclone, CT-01415 in place of the vertical vapour pipe and the separator. The cyclone returns a considerable amount of darkish liquid,through a Sight glass,to a return line going nearly to the bottom of the still body. Mr.Purzey, December 11, 1951 reported that the cyclone gave better coloured distillate than did the Hagan separator. Anniston, January 1950, reported satisfactory performance of their Hagan separators. Newport have the internal Hagan separator. In a report dated March 51, 1952, Mr. Dalton of the Krummrich plant mentions a modification to the Hagan separator at the Krummrich plant. The Aroclor colour was better after the change, but it was not certain that the alteration really caused the improvement. There is no attempt at fractionation, and the condensing systems were planned to give the lowest pressure drop attainable, consistent with removal of coloured entrainment particles. The deeper pattern of still S-062 was chosen to give more disengagement space for vapour, but it does not appear to have given any better coloured distillate, and it has the disadvantage of requiring a longer shaft etc. for the submerged pump. The condenser on No. 1 still delivers to receiver CT-0771 DSW 257567 STLCOPCB4061686 XII. EQUIPMENT LIST, contd. XII - 79 Equipment List S-043 Stills, contd. S-04J contd. No. 2 still has heat exchanger CT-01491, head tank CT-01398 with gravity flow (of cooling water only) to condenser CT-01578. CT-01398 has an internal coil (not used) and there is no temperature control instrument . The distillate goes to receiver CT-01377. The temperature of the distillate is roughly controlled by hand adjustment of the flow of water from CT-01398 to the condenser CT-01378. The Newport vacuum still was provided with a subsidiary vessel, located at a lower level than the main vessel, and containing the submerged pump. With this arrangement, it was hoped to diminish the liability of cavitation of the pump, and to permit the use of a much shorter shaft for the pump impellor. The arrangement, however, was unsatisfactory, largely because the pump gland was exposed to hot liquid Aroclor (See the London Engineering Dept. Final Report on the start-up of the Newport plant). Numerous different gland packings were tried, the gland was given a lantern ring, fed with liquid Aroclor etc= etc., but finally a long vertical steam Jacketed pipe was fitted on top of the secondary vessel, to carry the ,, stuffing box above the level of the charge in the main still. This location also put the driving motor into cooler surroundings, and the new arrangement has been made to work satisfactorily, though it brought back the troubles of the long shaft. In the pump assembly, the pump is hung from a manlid on the still cover, on k wide pipe down the centre of which the pump shaft runs. The delivery pipe from the pump runs independently up through the same manlid on the cover of the still (welded through). Differential expansion may distort the alignment of the parts, and may DSW 257568 STLCOPCB4061687 XII. EQUIPMENT LIST, contd. XII - 80 Equipment List Stills, contd. S-04J contd. displace the Impeller axially within its casing. Another trouble which appeared was that air leaking in through the gland could travel down the central pipe around the shaft and cause cavitation in the pump. The remedy for this is to have holes in the pipe,communicating with the main vapour space in the vessel. The stuffing box is water cooled; the bearings inside the still may give trouble, this clearance must be just right. Carbon bushings have shown some promise. It has to be remembered that the charge contains a fair amount of solid (lime) etc. which might lodge to some extent In the still instead of flowing to the secondary vessel. The internal bearings are lubricated by Aroclor bled off the pump delivery line, but they may become choked by the solid matter in the charge. See also the description of the Anniston still and pump ' on pages 20-, Section VI,.above, and comments on the distillation process, pages 4-, Section VII. Prom the bottom of the condenser at the Krummrich plant, the distillate passes through a jacketed line to a jacketed sight glass with sampling fitting, and so to one of the receivers CT-0771 or CT-01377. There Is a ring of gas burners around each condenser exit, to deal with the heavier Aroclors, but the burners are not much used. Condenser CT-0770 can be cooled by Aroclor circulated by pump P-0595 through the condenser shell space then through heat exchanger, CT-0831 (cooled with well water) and through a sight glass to head tank CT-O766, and so back to the pump. This system Is alternative to the cooling by-distilled water used on this condenser, but it has gone out of use since the Krummrich plant gave up the production of the higher Aroclors. DSW 257569 STLCOPCB4061688 XII. EQUIPMENT LIST, contd. XII - 8l Equipment List Stills, contd. S-04-5 contd. There is a steam and water coil in.the head tank to keep the Aroclor at around 110-120C. There is a Taylor Fullscope temperature controller 1-0510 controlling a valve on the steam inlet to the coil. This Aroclor cooling is more convenient for higher Aroclors, but the water system is preferred for the lower Aroclors. The system normally works at about atmospheric pressure though the vent (on the top of heat exchanger CT-0831 is usually kept closed, and there is a pop valve at the same point). The sketch on page XII - 82 will serve to show the arrange ment and to indicate certain minor features not described above. Each still has a bottom outlet which will completely entity the still, also an outlet at about the same level of the top of the bottom dish, which will leave about 80 U.S. gallons of bottoms in the still. Both deliver to open topped cans on small wheeled "dollies" under a hood ventilated by suction fan B-0148. Rising stem gate valves are used on these outlets and gas flames are freely used to heat them for seme time before the still is to be tapped. Bottom outlet also to emergency tank CT-0749* but this vessel is now used as extra storage for diphenyl. The deeper still has a thermo well obliquely through the yrirfe wall, about 7'6" below the cover, but this well was not in use May 1955. Each still body has a BS &B relief disc of AlPb, 8" diameter, vacuum supported, calibrated to rupture at 25 psig. The receivers do not have relief discs. DSW 257570 STLCOPCB4061689 COOLING SYSTEM XII - 62 AROCLOR Equipment List CONOE NSE R5. pio-^i~t "B* July, iqso. r^xJni HC * at CT-OllO To TTo^ 3P deck I P-0915- I use h P HC Hso Connection N*i-rtvrn vulva T7 TIC P Sv T"*n*indicator* T*<nf>. indiC con^jr Purnfn PrMtu<e rlKK ve-Vg ______________ 'XU dcc.<c aa (CTT-0-O7O7177 Roughly to cq|. v - I foot DSW 257571 l'*' deck STLCOPCB4061690  .* XII. EQUIPMENT LIST, contd. XII - 82a EquipmentList S-045 S-045, contd. Drawings. B 485 A 495 Water-cooled condenser on No. 1 still] /CT-0851 1/ -01597 Sump plate for submerged pump JM -01491 I S-045 B 644 B 651 B 662 Head tank for cooling medium --------------------- CT-01598 Tubular condenser --------------------------------------- /cT-0770 L -01578 Vapour exit pipe ------------------------------------------------S-042 C 795 Receiver ---------------------------------------------------------- CT-0771 C-807 Coke tower-------------------------------------------------------- CT-0755 . C 809 No. 1 Still -------------------------------------------------------- S-042 C 815 Piping of vacuum still - FC-045,CT-0770,-01577 C 864 like B 485, on No. 2 still -----------------------------S-062 C 6942 Piping diagram. No. 2 still---------------------- S-062 C 6945 Piping diagram. No. 2 still---------------------- S-062 D 6944 No. 2 still -------------------------------------------------------- S-062 E 6952 General layout No. 2 still------------------------- S-062 D 6955 General layout. No. 2 still with cyclone, receiver, and coke scrubbers. D 6957 Cyclone on No. 2 still ----------------------------------S-062 B 7082 Monel condenser on No. 2 still --------------- CT-01578 DSW 257572 STLCOPCB4061691 .' XII. EQUIPMENT LIST, contd. XII - 82b Equipment List S-062 -0459 Stills, contd. S-062 #2 Vacuum still purchased from Nooter. Serial #52. Dwg. D-6944, 6' ID x 11'10" str. shell, internal pipes, etc. Std. dished heads. Glass wool insulation 3" with 1/2" finish coat. Order B10730 on 5/12/41, Req. 20421 on 4/28/41. Chg. out $950.00. Suspended between 20'6" and 12' platform in CR. S-0459 is another number for C-O808, gas fired chlorinator. DSW 257573 STLCOPCB4061692 ' . v ' XITo EQUIPMENT LIST, contd. XII - 8^ Equipment: List SC-094 - 0246 Scales SC-094 Howe Portable Scale #822, Serial 1363205, all iron platform 30^" x 30^". Cap, 1500 lb. Order B9986 on 5/20/36, Req. 69955, Pyranol Plant. SC-098 Howe scale. Serial 1364566, #1420 Skeleton type, ball bearing, dormant scale, cap. 2500# with double beams. Platform 46 x 38. All metal incl. steel shaft. Order B14351 on 7/20/36. Req. 71556 on 7/17/56. Price $213.85. sc-0100 Scale purchased from The Exact Weight Scale Company, Serial 39992. Style 1226, cap. 200# on ratio of 10 to 1. Dial with Indicator travel 12-g-" under wgt, and ove wgt. Fitted with bag holder for 100 to 200# bags. All on swinging rack. Order B17906 on 9/9/56. Req. 72843. Chg. out $289.41. In lean-to near V-044 and V-045. SC-0246 1000 lbs. capacity, Pyranol Plant. DSW 257574 STLCOPCB4061693 . " " XII. EQUIPMENT LIST, contd. XII- 84 Equipment List T-014 Transformer T-014 Transformer made by Westinghouse. Serial 530335 200 KVA, type SK, now used 440 volt primary 110/220 volt secondary. On the heater of the Lectrodryer PC-046. Cost $10.00. Outside SW corner Bldg. CR. Also used formerly for strip heaters in the still receivers, etc. DSW 257575 STLCOPCB4061694 V. - XII. EQUIPMENT LIST, contd. XII - 85 Equipment List TW-0166 - 0312 Towers TW-0166 Fused Silica Tower purchased from Amercel Co0 Inc. 1 "U" bend trap. 12 absorbers sections B/P Gill 8" ID x 6'6" C to center. Order B8l6l, Req. 69399. Same as TW-OI65. Regarded as obsolete design. TW-0182 Scrubbing HC1 tower made by Haveg. Drawing C-4705. "41" std. 2'6" dia. 10'2" deep, 5/8" thick walls x 3/4" thick bottom, machined dished head, and connecting material, 2" thick Haveg drilled plate with necessary supports 4-3", 1-8" and 1-10" std. Haveg nipple type outlets with figs. Order B20284 on 10/5/37, Req. 83234 on 10/5/37. Chg, out $668.58 on 12/31/37. On 38' level steel struct, south side of CR. TW-0206 Scrubbing Tower purchased from Nooter. Drawing B-5815 support, drawing C-58l4 tower. 17-18" ID x 8' welded steel const', .tower, welded steel scrubber support for tower. Order B7346 on 3/27/40. Req. 8063 on 3/27/40. Chg. out $277.00 on 4/30/40. Above CT-O756, scrubber by pump tank. TW-0221 HC1 absorption tower purchased from Fan Steel Metallurgical Corp. Serial 955-1941. Drawing D-4300 foreign. PA #147. Type AL-400. The tower, fittings and piping made of Karbate. Gas line of Haveg. Cap, to produce 205 Baume HC1 at 4620# per hour. Order B4625 on 2/21/41. Req. 18520 on 2/21/41. Chg. out $5321.13 on 8/21/41. On steel struct. S of CR. Schwarting and others "Process Description --- For Aroclors", November 12, 1953, state that the Fansteel off-gas ab sorbers are constructed of Haveg 60, and have Tantalum heat exchange surfaces. TW-0312 Absorption tower. Fansteel AL-300. Haveg 60 parts. Tantalum tubes, (some tantalum parts salvaged from an older unit,, ) DSW 257576 STLCOPCB4061695 .v ' XII. DRAWING LIST XII - 86 Drawing List Note; Some of the earlier drawings were made at the JPQ plant, and the later ones at the Krummrich plant,, As the two plants have inde pendent numbering systems it is necessary to specify which plant is concerned. The drawings marked "A" in column'2 on the following pages are from the JPQ plant, whereas those marked "B" are from the Krummrich plant. . In column 3, on the following pages, the letter "L" indicates that prints of drawings were sent to Mr. Cooper, London, by air mail, April 24, 1947. "S" indicates that prints of drawings were sent to Mr. Cooper, London, by surface mail, April 24, 1947. "N" indicates that the drawings in question do not appear to be of interest to MCL. "M" indicates that the drawings were not available April 23, 1947. "F" indicates that the drawings were found July 28, 1950, and that prints were sent to Mr. Buis, London. DSW 257577 STLCOPCB4061696 ,, . XII. EQUIPMENT LIST, contd. XII - 86 a Equipment List V-044 - o46 Conveyors V-044 V-045 V-046 Screw conveyor made by Essmueller MF^CoJo. Drawing C-816. Size 6", 6'8J" trough length with outlet at each end. Cover of galvanized iron. Cl trough ends with zinc and tin sprayed. Req. 69909. On bottom CT-0764 - North Conveyor. From stg. bin to bagging scale and back to bobt of elevator, driven by M-0835. Layout - E-877. Flow Sheet - B-640 Screw conveyor made by Essmueller MF Co. Drwg, C-816. Size 6", 6'8-|" trough length with outlet at each end cover of galv. iron. Cl trough ends with zinc and tin sprayed. Req. 69909. On bottom of CT-O765 south conveyor. From storage bin to bagging scale and back to boot of elevator, driven by M-O836. Screw conveyor made by Essmueller MF Co. Drawing C-8l6. Same as V-044 and 045. From flaker discharge to elevator boot. Driven by chain on M-O827. All these were part of the equipment for Solid Aroclors: dismantled in '' 1952 . DSW 257578 STLCOPCB4061697 XII. _* DRAWING LIST XII - 87 Drawing List Drawing Number A-324 ** A LS Title Equipment Number Gas-heated chlorination pot(see E-888) CT-O808 E-3^6 M Muriatic treatment vessel CT-0861 P-352 N Fractionating column(not Aroclor plant) P-370 A L S General Layout Layout P-373 F-37^ A L S Ducts for process fumes,solid Aroclors D-012 etc. A L S Layout, solid Aroclors Layout P-375 N Structural steel F-376 N Steel and foundation P-380 N Electrical layout F-381 N Electrical conduits F-382 N Lighting P-383 N Service lines F-38^ N Foundation details P-385 N Structural steel. Muriatic tower F-386 A L S Piping layout Piping P-389 . N Electrical details F-391* A-459 N Gen. arrt. HC1 absorption A L S Bearing for blender shaft CT-0779 * * See note on page 86 in this section. - DSW 257579 STLCOPCB4061698 XII. DRAWING LIST, contd. XII - 88 Drawing List Drawing Number * * Title Equipment Number B-483 A-493 A-501 A LS A' L S N Water-cooled condenser for vac.still CT-0831 r CT-01307 Sump plate for submerged pump in vac. r CT-01491 still _ S-043 Lead-lined tray for HC1 absorber C-502B M Sand filter for muriatic acid D-512 D-518 A L S Storage hopper for solid Aroclor A L S Chute for Aroclor flake ^CT-0764-\ \CT-076y D-012 C-605 D-609 A L S Shear pin on drive of gas-heated chlorinator B M Store tanks CT-0808 CT-0748 CT-0749 CT-0768 CT-0769 CT-01310 B-615 A L S Relief door gas-fired chlorinator furnace CT-0808 B-640 A L S Plow sheet B-643 N Separator, not installed Plow sheet B-644 A L S Cooler on vac. still system CT-O766 CT-01398 B-645 A L S Cyclone on solid Aroclor plant CT-0751 B-646 B-651 A. L S Still pots for solid Aroclor A L S Heat exchanger on vacuum still ' R-026 R-027 CT-0770 CT-01378 See note on page 86 in this section. DSW 257580 STLCOPCB4061699 _ . XII. DRAWING LIST, contd. XII - 89 Drawing List Drawing * Number * Title Equipment Number B-653 A L S Stack for solid Aroclor plant CT-0751 B-654- A L S Support for st.ack CT-0751 B-658 N Floor gratings B-659 B-660 A L S Chlorine inlet A L S Cyclone - not identified CT-0745 CT-0833 B-661 A L S Elevator drive, solid Aroclors L-031 B-662 A L S Vacuum still vapour pipe S-042 B-665 A N Supports for vent line scrubber B-664 A N Vac. still furnace vent pipe CT-0762 S-042 B-666 A L S Thermocouple wells B-675 B-684 B-685 B-686 B-689 C-795 A L S Hood, etc. of flaker A obsol Strip heater clamp for chlorinator ete A obsol Heater for Sperry press ete A N Vent stack N Vent stack A L S Vacuum still receiver C-798 A L S CaCl2 breather D-102 CT-O808 F-0172 FC-045 FC-045 CT-0771 CT-01377 CT-0762 C-799 C-800 A L S Diphenyl head tank A L S Scrubber liquor tank CT-0767 CT-0754 CT-0755 CT-0756 * * See note on page/in this section. DSW 257581 STLCOPCB4061700 XII. DRAWING LIST, contd. XII - 90 Drawing List Drawing Number * - * - Title Equipment Number C-804 C-807 A N Hot water collection tank A L S Coke scrubber CT-0752 CT-0753 CT-01396 C-809 C-810 A L S #1 vacuum still A L S Melt tank for high boilers etc. S-043 CT-O762 C-815 A L S Piping of vacuum still . FC-045 CT-O77O CT-01378 C-816 A L S Aroclor conveyor V-044 C-818 A . L S Chlorine vapourizer ' CT-0743 .C-821 N Platform for still pots R-026, R-027 C-822 A L S Chlorinator relief connection CT-0744 C-825 A L S Muriatic acid store tanks C-827 A L S Weighing truck, solid Aroclor plant CT-0784 CT-O785 CT-O786 CT-0795 MSC-0681 C-829 N List of motors C-830 P-838 A L S Gas-heater for discharge of gas-heated CT-0808 chlorinator N 18" fractionating column, not in Aroclor plant C-847 N Holder for strip heater CT-0771 * * See note on page 86 in this section. DSW 257582 STLCOPCB4061701 XII. DRAWING LIST, contd. XII - 91 Drawing List Drawing Number C-848 E-876 E-862 E-863 C-864 E-865 E-867 E-870 E-877 E-880 E-881 E-886 ** Title " Equipment Number N Holder for strip heater CT-0771 N Floor grating L S #1 Blending tank and #1 Filtrate receiver CT-0779 CT-0780 L S Buffer tank (air blowing tank) CT-0750 A M Heat exchanger for #2 vacuum still (see drawing B-483) S-062 A L S Setting for stills for solid Aroclor R-026, R-027 A L S Setting for fireheated chlorinator CT-0808 N Conveyor for Aroclor flake L-031 L S Conveyor for Aroclor flake (layout) V-044 A L S Chlorinator CT-0744 CT-0745 CT-0833 A L S Shell for gas-fired chlorinator furnace CT-0808 L S Shell for above and brick setting S-043 'F-045 E-888 E-889 E-896 D-978 L S Drive for gas-fired chlorinator N HC1 absorption tower N Floor grating, HC1 tower B L S Diphenyl store tank CT-0808 CT-0347 * See the note on page 86 in this section. DSW 257583 STLCOPCB4061702 XII. DRAWING LIST, contd. Drawing Number -- ** Title C-1117 B N Foundation of D-978 D-2076 B L S Turbo agitator for blending tank D-2077 B L S Stator for above C-2479 B M Heating furnace for coil of #2 vacuum still C-3775 B L S Filter for HC1 gas Dt4253, B L S Muriatic tank D-4500 M Fansteel drawing HC1 absorber E-4366 B F M Varec. Gauge on Pyranol mixer E-4413 B L S T.C.B. Store tanks D-4459 B L S Rubber-lined treatment tank with; agitator C-4616 B L S Scrubber liquor pump tank E-4679 N Obsolete, Layout for HC1 absorber E-4689 N Obsolete, Piping of HC1 absorber C-4705 B L S Haveg tower (obsolete) for HC1 abs,, C-4845 B L S Scrubber liquor tank E-C57H M Goodrich rubber-lined tanks C-5745 B L S Scrubber in Pyranol plant C-5814 B L S Obsolete, HC1 tower XII - 92 Drawing List Equipment Number CT-0779 CT-0779 FC-066 F-0106 CT-01260 ' CT-01321 CT-0861 CT-0968 CT-01013 TW-0182 CT-0104 CT-01575 CT-01162 TW-0206 See the note on page 86 in this section. DSW 257584 r STLCOPCB4061703 XII. DRAWING LIST, contd. XII - 93 Drawing List Drawing * * Number Title Equipment Number B-5815 B N Obsolete, HC1 tower support B-5821 F Cyclone CT-01259 CT-01279 CT-01280 CT-01282 C-5825 B L S Monel gas chamber on fireheated chlorination system CT-01258 C-6144 B M F Monel condenser CT-01263 E-6209 B L S Chlorinator CT-0744 CT-01282 D-6455 B L S Pyranol mixer CT-01321 E-6858 B L S Assembly of blending tank CT-0779 CT-01299 A-6853 B-6868 N Agitator in blending tank N Thermocouple wells CT-01399 C-6863 B L S Filtrate receiver CT-01400 E-6941 N Platform of still C-6942 B L S Piping diagram for #2 vac. still S-062 C-6943 B L S Monel piping diagram for #2 vac.still S-062 D-6944 B L S #2 Vac. Still D-6945 Exhaust System,mentioned on p.XII-6. D-6946 M F Control room S-062 S-062 E-6952 B L S General layout #2 still S-062 See the note on page 86 j_n this section. DSW 257585 STLCOPCB4061704 XII. DRAWING LIST, contd. Drawing List * * Title D-6956 B L S General layout #2 still C-6957 B L S Cyclone on #2 vac. still B-7082 B L S Monel condenser #2 vac. still B-7121 N Support for Sperry press A-7156 N Pipe coil under Sperry press A-8855 M Bearing for blending tank (See drg. A-'459) D-10292 B L S Piping of air blowing tank Hand B L S Dryer for Attapulgus Earth sketch (See corresp. file Mar. 25/^7) XII - 9U Drawing List 1 Equipment Number S-062 S-062 S-062 P-0113 P-0113 Anniston Drawings 9C-8000 90-82^5 Layout of chlorinators| #2 Aroclor still \ to MCL, June 7 J 19^6 0-6856*1 Detail of chlorinator ] ^ ,,,,,, ,, , (Swan Chem. ica_l C_ o.)V JV to MCL March 1! 19^7 See the note on page 86 of this section. DSW 257586 STLCOPCB4061705 XIV. HISTORY OP THE PROCESS IN MONSANTO. XIV - 1 History of the Process In the years 1927 - 1928, the Swann Chemical Company developed a procecc for making diphenyl, but as the expected demand for it did not continue, other outlets were sought for the diphenyl. Aroclors were produced in the laboratory in 1929, and as they showed good electrical properties, fire resistance, and general inertness, the General Electric Company became interested, and developed the use of Aroclors in transformers and capacitators. A plant was installed to produce 3000 lbs./day at Anniston. In 1955 Monsanto acquired the Swann Company, so gaining access to their Aroclor patents. As the demand for Aroclors increased, additional production equipment was installed, located at the Monsanto Illinois factory (then plant "B" and now called the Krummrich plant). This equipment came on stream in September 1956. The Krummrich plant site was chose partly because of the availa bility of chlorine there, but when chlorine consumption overtook the production, and chlorine had to be purchased, proximity to the diphenyl production at Anniston had more weight, and additional capacity, largely designed on the plant "B" model, was installed at Anniston in 1941. - By 1946 both plants had doubled their capacity, to give a t<5tal production capacity approaching 2 million pounds a month. About 1954 chlorine cells were installed at Anniston. The Newport plant was designed, mainly on Krummrich plant inform ation, but to a less extent on Anniston information, under Newport Project No. 12 of the London Central Engineering Department. Chlorination started at Newport in June 1951> Mr. Clegorn from Anniston spending some time at Newport to assist in starting the diphenyl and Aroclor plants there. The first production of Pyranol by MCC was in 1956, when Pyranol 1488 was made for the General Electric Company, the blending being done at first in rail tanks. Pyranol 1495 was made in July 1958. The use of tin-tetraphenyl started in 1944, since when the main production has been of 1467 (TCB - 1260 mixture plus tin-tetraphenyl). DSW 257587 STLCOPCB4061706 .v .- ' XV. OPERATING INSTRUCTIONS. XV - 1 Operating Instructions Operating instructions were given in the report of Lyles, Soffranko and Becker, November 1947, pages 84 - and a revised version was put out by the Krummrich Plant Standards Department, August 10, 1954, (copy sent to Newport, May 25, 1955). Points calling for special mention are: -- 1. Care in melting diphenyl received in cars. The first move is to melt a hole, from the surface, down to the bottom of the tank to prevent development of pressure from the heat of the tank coil or Jacket. 2. Usual rail track routine in handling cars. 5. Exclusion of rain etc. 4. Proper use of tracing on pipe lines'. Lines to be blown clear after use where necessary. 5. Tank vents and overflow lines to be maintained above the melting point of diphenyl 6. Charges in the diphenyl measuring tank to be kept hot. 7. Fire precautions in handling diphenyl, toluene, and butyl acetate and mixtures containing them. ' 8. Chlorinator charges kept as cool as possible, and not circu lated in the early stage of chlorination. 9. Watch inlet pressure on chlorine line to chlorinator. 10. Care in emptying chlorinators not to suck back the scrubber charge. 11. Keep chlorinator charge out of the chlorine feed line. 12. Watch gravity and temperature of scrubber for indication of poor absorption of chlorine in the chlorinators. DSW 257588 STLCOPCB4061707 XV. OPERATING INSTRUCTIONS, contd. XV - 2 Operating Instructions 13. Control air-blowing temperature to suit the Aroclor being handled. 14. Check dryness of air from Lectrodryer at proper intervals. 15. Guard against burning or coking the still coils. 16. The usual care in lighting gas furnaces. 17. Care in dealing with hot material tapped from the stills. 18. Cleanliness in handling finished Aroclors. 19. With higher Aroclors take special care against blockage of lines. 20. Safety precautions as discussed under "Hazards", Section XI, above. Pyranols Operating Instructions relating specifically to the Krummrich plant are given on pages 33- of the report "Dept. A-246 Pyranol Process", Lyles, Soffranko and Miller, March 24, 1947, ^6opy..#8 sent to MCL October 15, 1947). ' Points mentioned are: 1. Checking the moisture content of incoming cars of trichloro benzene. Air blowing at about 50C. to remove excess moisture. 2. Sampling of materials at various stages for submission to General Electric Company. 3. Exclusion of moisture, HC1 fume and dirt. 4. As a working rule, in adjusting blends of TCB with Aroclor 1260., 1 part of 1260 added to 80 parts of the blend will raise the Sp. Gr. about 0.001 and the refractive index about 0.0001.' DSW 257589 STLCOPCB4061708 XV. OPERATING INSTRUCTIONS, contd. XV - 3 Operating Instructions Pyranols, contd. 5. Blends containing tin-tetraphenyl are to be warm (about 80C.) when filtered, otherwise some TTP may come out of solution. 6. Waterproof cloth over the domes of the filtered rail tanks to exclude moisture and dirt while travelling. 7. Avoidance of delay in dealing with samples because of the numerous testing stages required. DSW 257590 STLCOPCB4061709 Acknowledgment ACKNOWLEDGMENT To Mr. J. Soffranko who was In charge of the Krummrich plant Aroclor Dept, in 1947, and to the foreman, Mr. Errol Smith. The report "Dept. 246, Aroclor Process" by Lyles, Soffranko and Becker, November 6, 1946 was of very great help in assembling information for the Newport project, also the companion report "Dept. A-246, Pyranol Process" Lyles, Soffranko and Miller, March 24, 1947. The reports by Schwarting and others, 1955 and 1954, have been used in the present revision of the process details. Acknowledgment is due also to other Krummrich plant people who helped then and later. Dr. E. E. Hardy was of great help at Anniston in 1947 in explaining the process and locating information. To Messrs. Ellenburg and Wood for guidance around the Anniston plant, and to Messrs. Baker and Dunlop for analytical information. Mr. Clegorn was very helpful during a visit in March 1955. DSW 257591 STLCOPCB4061710 Index Page 1 INDEX ACETONE, SOLUBILITY TEST ON AROCLORS DISCUSSED....................... VII-11 Acid number, conversion of KOH figure Into NaOH figure -- IX-65 KOH v. NaOH values ---------------------------------------------------- IX-40 Acid number, test methods---------------------------------------------- IX-62-, IX-128 Acknowledgment ------------------------------------------------------------------------- Section XVT Agricultural uses of Aroclors --------------------------------------------------- VTI-21 Air-blowing of chlorination product ---------------------------------------- VI-15- comments on--------------------VII-4 Air blowing tanks, etc. ---------------------------------------------------------------XII-17a Air, dry air needed in unloading-------------------------------------------------- VI-55 Air dryer --------------------------------------------------------------------------------------------- XII-45 Analytical Methods, see "Specifications & Test Methods" and --- ----------------- "Control Tests" Anthraquinone derivatives, as stabilizers inAroclors ------ VII-9 reportmentioned VTI-54 determination of----------------------------VII-9 APHA--------------------------------------------------------------------------------------------see "Colour" Appearance ------------------------------------------------------------------------------- see "Colour" Applications of Products -------------------------------- VII-18-, VII-50, XI-5 literature survey mentioned ----- VII-52 Aroclors, advantages of----------------------------------------------------------------- VII-19 as animal repellants ------------------------------------------------------ XI-5 are complex mixtures ------------------------------------------------------ II-2 blending of to give intermediate Aroclor ------------VII-11 butyl acetate blends ------------------------ see "Butyl Acetate" causes of high chloride content------------------------------ VII-15- changing production from one grade to another - VI-15 ---------------------------- VI-25 colour troubles ----------------------------------------------------------- VII-10- crystallization troubles--------------------------- VII-11-, VII-2 damaged by heating in iron------------------------------------------ VTI-7 effect of metals on ----------- VI-54, VII-1, VII-7, XII-1 isomer ratios v. chlorination conditions ----------- VII-5 need for tin etc. lining in store vessels --------- VT-55 physical and chemical properties ---------------------------- III-7 (solid) crystallization point method -------------------- IX-87 solid, distillation ---------------------------------------------------- VI-24- solid, manufacture discontinued ------------------------------------ V-2 solid, process details ------------------------------------------------ VI-7- solid, specifications --------------------------------- IX-16, IX-50 specifications for ---------------------------- IX-11-, IX-26- DSW 257592 STLCOPCB4061711 Index Page 2 Aroclor,toluene blends ------------------------------------------------------------------- VII-7 test method ---------------------------------------- IX-88- unstable Impurities in ------------------------------------ II-1, VII-16 viscosity index is high------------------------------------------------ VII-19 see also finished products Askarels ---------------------------------------------------------------------------------------------- 1-4 bulletin---------------- VII-30 Attapulgus earth, alternative materials unsatisfactory -- VII-7 dosage of-------------------------------------------------------------VI-27 dryer ---------------------------------------------------------------XII-40- drying of ------- ---------------------------------- VI-27, VII-7 removes T.T.P. ----------------------------------------------- VII-7 sample sent toMCL---------------------------------------------- IX-9 specification ---------------------------------------------------- IX-3 BATCH RECORDS see "Operating Records" Benzene, sample sent to MCL---------------------------------- -------------------------- IX-9 Biphenyl ------------------------------------------------------------------------------- see "Diphenyl" Blending, of Aroclors with butyl acetate IX-40 of Aroclors with toluene VI-29- of different Aroclors, product not necessarily equivalent'to product of direct chlorination II-2,VII-11 for Pyranols ------------------------------------------------------------------- VI-32- Blending Tanks ------------------------------------------------------------------- XII-28-, etc. Blowers --------------------------------------------------------------------------- ----------------------- XII-6 Boiling point range------------- ----------------------------- see "Distilling range" Buildings --------------------------------------------------------------------- see "Plant layout" Bulletins on application of products ------------- see "Applications" Butyl acetate - Aroclor blends, test methods ----------- IX-175- Butyl acetate blends, mentioned------------------------------------------------------IX-40 precautions in handling--------------------------- IX-40 colour of blends with Aroclors(test method)IX-178 quality of------------------------------------------------------------------- IX-10 specification for-----------------------------------------------------IX-29 CAPACITY OP PLANT------------------------------------------------------------------------------------X-lCarbon, no specification ----------------------------------------------------------------- IX-3 Catalyst --------------------------------------------------------------------- see "Iron turnings" Cereclors ---------------------------------------------------------------------------------------------- IX-183 Changing from one Aroclor to another ----------------------VI-13, VI-25Chemical reactions withAroclors ------------------------------------------------ VII-21 DSW 257593 STLCOPCB4061712 Index Page 3 Chemistry of the Process ------------------------------------------------------ Section II see also "Comments on the Process" Chemistry of action of chloride scavengers ------------------------- IX-182 Chloride scavengers ----------------------------------------------------- see "Scavengers" Chlorides in tintetraphenyl, test method ---------------------------- IX-133- Chloride test in boiler water---------------------------------------------------- IX-107a General Electric --------------- see "General Electric" Chlorination, batch data-------------------------------------------------------------- -------VI-5 chart of % CI2 v. lb. CI2 to finish------------- VI-49 chemistry of---------------------------------------- *----- II-2, VII-3 comments on ------------------------------------------------------------ VTI-1- contlnuous, discussed-------------------------- VTI-2 no circulation of chargeat first------------------------ VI-6 process In detail---------------------------------------------------- VI-4 ' purging of gas Inlet line-------------------------------------- VT-6a rate of ---------------------------- see "Chlorine flow rates" record charts-----------------------------------------------------------VI-37- unstable byeproducts mentioned --------- II-l, VII-16 Chlorinator for solid Aroclors ------------------------------------------------ XII-30- Chlorinators --------------------------------------------------------------------------- XII-7- etc. inlet fitting-------------------------------------------------------------VII-2 Chlorine consumption figures ------------- see "Production standards" determination, total chlorine --------------- IX-52-, IX-64 - General Electric method, see ----------- "General Electric" distributors --------------------------------------------------------- XII-9, VII-2 flow rates ---------------------------------------------------- r----------------------VII-1 handling of----------------------------------------------------------------------- VI-2- comments on---------------------------------------------------VII-2 metering etc. ----------------------------------------------------- VT-3-, VI-6a- no specification------------------------------------------------------------------- IX-3 quality, comments --------------------------------------------------------------- IX-8 use of snift gas etc. --------------------- VI-2, VII-2 Chlorphenols in Aroclors --------------------------------------------------------------- VII-10 mentioned------------------------------------------------ IX-8 Cliff-Char ----------------------------------------------------------------------------- see "Carbon" Closed Tanks ------------------------------------------------- XII-7- Cocks, choice of -------------------------------------------------------------------------- XII-5 Coke scrubbers ----------------------------------------------------------------- see "Scrubbers" Colour, see also --------------------------------------------------- "Electrophotometer" test methods, Aroclor1271 (solid) ---------------------------- IX-101 Aroclors 1270 and 1271 intoluenesolution IX-100,-103a Aroclors ------------------------------------------------------------------------- IX-57- DSW 257594 STLCOPCB4061713 Index Page 4 Colour, diphenyl --------------------------------------------------------------------------------- ix-93 general (APHA)----------------------------- -------------------------------IX-47- (Hazen)------------------------------------------------------------ -- IX-153 Pyranols ------ IX-57- Comments on the Process ---------------------------------------------- ---------Section VTI Compatibility data (Aroclor) -------------------------------------- III-16 Competitive products -------------------------------------------- IX-183 Consumption figures ------------------------------------------------------ see "Cost data" ---------------------------- -------------------------- --- "Plow Sheets" -------------------------------------------- ------------"Yield figures" Control tests, in blending Pyranols------------- -------------- ---------- VI-32- Control tests------------- ---------------------------------------------- --------------- Section VTII Conversion factors------------------------------------------------------ -------------------- IX-12b Conveyors------------------------------ -------------- ---------------------------------------------XII-86 a Corrosion test--------------- --------------------- ------------ see "General Electric" Cost data---------------------------------- -------------------------------------------- see Section X Cost sheets ---------------- X-27- Crystallization In Aroclors, see "Aroclors, crystallization trouble" Crystallizing point test method, Aroclor----- ----- IX-87 control test method----- VIII-1- dlphenyl------------------------ IX-94 glycidyl phenyl ether--------IX-161 tri-tetrachlorobenzene IX-I67 Crystal structure, test method for Aroclor 1271----------------- IX-103a Cyclones, on chlorinators----------------------------------------------------------------- VI-9- on stills-------------- XII-78 DENSITY ----------------------------------------------------------- -- see "Specific gravity" Design Reports -------------------------------------------- ------------------------------------- VII-31 Dibutyl diphenyl tin, as a scavenger ------------------------ VII-8, VII-22 Dielectric constand and power factor. test method --------- IX-144- Dielectric strength, test method ----- ----------------------------------- IX-135Diphenyl, comments on quality ------- ---- ------------------------------------------- IX-8 Diphenyl handling -------------------------------------- ------------------------------------- VT-1- Diphenyl measuring tank -------------------------- ------------------------------------- XII-25 Diphenyl, phys. and chem. properties --- --------------------------------- III-l- sample sent to MCL --------------- ------------------------------------------- IX-9 specification -------------------------- --------------------------- IX-l test method (colour) ----------- ............... IX-93 Distillation ------------------------------------------------ .................... VI-14 comments on ------------------------ ............................................ VII-4- DSW 257595 STLCOPCB4061714 Index Page 5 Distillation, of solid Aroclors ------------------------------------------------ VI-24record charts ----------------------------------- ----------------- -- VI-40seml-continuous ---------------------------------------------- -- vi-21use of moderate vacuum ---------------------------------- VI-23 Distilled high boilers------------- -------- see High boilers, distilledDistilling Range, Test Method, Aroclors etc. ---------------------- IX-74- diphenyl ---------------------------------- IX-95 general----- --------------- ------------IX-41glycidyl phenyl ether --- IX-162 trichlorobenzene etc. -<-- IX-70 tri-tetra chlorobenzene IX-168Distribution list ----------------------- ------------------------------------- see title page Drawing list ------------------------------------------------------------------------------------- XII-86see also the drawings listed under many of the items in the equipment list in Section XII Dryer ---------------------------------------------------- --------------------------- see "Air dryer" Dryer for Attapulgus earth -------------------------- see Attapulgus earth Du Pont viscosity method (Parlln) ^-------------------------------------------- IX-179 EARTH------------- ------------------------------------------ ------------ -- see Attapulgus earth Earth treatment of Aroclors ------------------------ ------------ see "Treatment" Effect of metals on Aroclors----- ------------------ -------------- see "Aroclors" Ejectors---------------------------------------------------- ---------- ---------------- VI-23, XII-64 Electrical grades of materials ----------------- --------------------------------- VII-7 Electrical properties of Aroclors III-8, HI-16, VII-32, VII-17 Electrical stability, test method ------------ --------------------------- ix-8l Electrical test apparatus, cleaning of-- ---------------------------------ix-154 Electrical test methods ------------------------------- ---------- VTI-32-,IX-155 - comments on ------- ---------- -r---------------- IX-183 Electrical uses for Aroclors --------------------- -------------- VII-20, VII-21 Electrophotometer, operation of --------------- -- ---------------------- IX-106b- Elevators------- ;------- -----------------------------------------'-- ----------------------- XII-49 Emergency measures ------------------------------------------ ------------------------------- VI-57 Equipment List--------------------------- ----------------------- ---------------- -- section XII general note ----------------------- ----------------------------------- XU-1 Evaporation loss data (Aroclors) ------------- ---- --------------------- - hi-8 FENCHLOR ---------------- ------------------------------ ---------------------------------------- IX-183 Filters--------------- -------------------------- ---------- -------------- -------------- ------------ XII-42Filtration of Aroclors, after earth treatment ----- VI-27-, VI-33 DSW 257596 STLCOPCB4061715 Finished Products, causes of defects ------chlorine contents ------comments on quality----listed ---------------------------phys. and chem. prop, spec, and test methods see------------------------------------ Fire Hazards -----------------------------Fire point, test method --Flaker ---------------------------------------Flaking of solid Aroclors - Flash point, test method ----Flow meter for chlorine, see Flow Sheets -------------------------------Fume exhaust system --------------- Index Page 6 ....................... -- V1I-9---------------------------- xx-i -------------------------- VII-9---------------------- 1-2, 1-4 ----------- ---------------- III-7------------------- Section IX ---------------------- Aroclors -------------------- Montars ---------------------- Pyranols ---------------------------- XI-6 ------------------------ IX-82-------------------------- XII-40 -------------------------- VI-24 -------------------------- IX-82Chlorine flow rates" -"Chlorine metering" ------------------- Section IV ------------ see "Blowers" GASKETS----------- ----------------------------------------------------------------- ------------ ----XII-2attacked by TCB blends ---------------------------------------------------- VII-17 for drums--------------------------------------------------------------------------------- VI-34 to resist Aroclors------------------------------------------------------------ VII-19 General Electric Test Methods, comments on ----------- VII-12-, IX-40 -------------------------- IX-l80- corrosion test :----------------------- IX-85 inorganic chlorides test -IX-77 sampling------------------- VI-32-, IX-40 Glycidyl phenyl ether, chemical nature of -------------------------------------- 1-4 chloride content of------------------------------VII-8 determination of in Inerteens -- IX-165hazards in handling of -------------------- IX-l6l. specifications -------------------------------------- IX-5 test methods ---------------------------------------- IX-l6l- HAZARDS --------------------------------------------------see.also ------------------------------ Hazen colour determination method HC1, --------------------------------------------------------Heat of Evaporation ---------------------Heat of reaction -------------------------------- Section XI ----- "Emergency measures" ------------ IX-153 see "hydrogen chloride" ------------------------------------ II-2 -------------------------------------II-2 DSW 257597 STLCOPCB4061716 Index Page 7 High boilers, distilled, phys. and chem. prop. ------------- 111-5handling of---------------------------------------------------------------VI-1no specification------------------------------------------------------ IX-1 samples sent to MCL------------------------------------------------ IX-9 see also-------------------------------------------------------- "Santowax" History of the Process --------------------- --------------------------------Section XIV' Hold point ----------------------------------------------- see "Crystallizing point" Hydraulic fluids ---------------------------------------- ;---------------------------------- VTI-20 see also under "Research reports" VII-53 etc. Hydrogen chloride, absorbers ---------------------------------------------------- XII-85 absorption, Anniston ------------------------------- VII-11cooling & scrubbing VI-9->VI-11equipment is outdoors,etc. V-2 process in detail ------------- VT-11- see also ---------------------------------- "Muriatic acid" INERTEENS --------- -------------- ------------------------------------ - -- --.............. 1-4 Inorganic chloride test --------------------------------see "General Electric" Instruments ----------------------------------------------------------------- -------------------- XII-46- Introductory Note ---------------------------------------------------- - see front of book Inventory, daily ------------------------------------------------------ ------------------------VI-46a monthly------------------------------------------------------------ VI-47-, VI-50 Iron, determination of in Aroclors etc. ------- -------------- IX-84 general method ----------------- ---------------------- IX-91- Iron turnings, preparation of ---------------------------- --...................- VII-1 wastage of in use ------------------- ------------------------ VII-1 Isomeric ratio, Aroclors -------------------------------------- ---------------------- VII-3 tri-tetra chlorobenzene ------- -------------------- IX-169- JOINTING AND PACKINGS ---------------------------------------------------- see "Gaskets" LABOUR REQUIREMENTS---------------------------------------- ---------------------- X-2, X-l6 Lay-out of plant ------------------------------------------------------------------------------- V-lLectrodryer ---------------------------------------------------------------------see Air dryer Lime (hydrated), addition of-------------------------------------- VI-16, VI-22 specification ---------------------------------------------------- IX-3 Loss on heating at 100C., test method----------------------------------IX-73 DSW 257598 STLCOPCB4061717 Index Page 8 MARKET RESEARCH REPORT (MCL) (reference) --------------------------- VII-31 Melting point test method, Aroclor 1271 - --------- ------------ IX-103 general ------------- ........... -................. IX-50see also--------- " Crystallizing point" Melt tank for Santowax ------------------------------------- -------------- VI-2, XII-24 Mill for solid Aroclors------------------------------------ .......................... -- XII-60 Miscellaneous Equipment-------------------------------------------------------------- XII-61Moisture ----------------------------------------------------------------------------------- see "Water" Montars, mentioned--------------- ------------------- ------ ---- --------------------h ^TW3 phys. properties ---------------------------------------------------------- III-17 softening point test method --------- -------------- ,---------- DC-59 specification--------- ---------------------------- ----------------------------- IX-17 test methods---------------------------------------- ----------- IX-59, IX-111 use in chlorine cells suggested --------------------------- VII-21 uses, electrical ------------------------------------------------ VII-20, -21 Monthly reports --------------------------------------------------------------------------------------X-7- see also -------------------------------- "Inventory, monthly" Motors ----------------------------------------------------------------------------------------------- XII-50Muriatic acid, carbon treatment of ------------- ---------------------- :--VI-11- batch records------------- VT-45 Muriatic acid, specification ------------------------------------------------------ IX-39 see also ------------------------------------ "Hydrogen chloride" NOMENCLATURE 1-2 ODOUR, TEST METHOD, AROCLOR 1270 ----------------- ------------------ IX-99 general ---------------------------- -------------------------- IX-56 Off-gas-------------------------------------------------------------see "Hydrogen chloride" Open Tanks --------------------------------------------------------------- ------------------------ XII-68 Operating Data ------------------------------------------------------- ----------------- Section X Operating Instructions, abstract of ----------- -------------------------- XV-1- report mentioned-- ------------------------ VII-31 Operating Records ------------------------------------------------ ------------- ............VI-36 Outline of Process ---------------------------------------------- ------- see "Synopsis" PACKING ---------------------------------- -------------------------------------------------------VI-34see also "Effects of metals" Packings for pump glands---------------------------------------------------- XII-2 to 4 Parlln viscosity method --------------------------------------------------------------- IX-179 Parr bomb--------------------------------------------------------------------------- see "Chlorine" DSW 257599 STLCOPCB4061718 Index Page 9 Patent Position --------------------------- ------------------------ --------------- VII-8, VII-22 Phenoxy propene oxide ---------------------------- see "Glycidyl phenyl ether" Physical and Chemical Data---------------- ------------------------------------ Section III see also----------------- ---"Specifications" Pipe lines, note on------------------------------------------------------------- XII-1 Plant lay-out ------------------------------------------------------------------------------------------- V-l- Plant Records ----- ----- ------------------------------------- see "Process records" Plasticizers----------- ------------------- IX-183 Plasticizers, use of Aroclors------------------------------------------------ --- VII-21 P.P.O. (phenoxy propene oxide) --------- see "Glycidyl phenyl ether" Power factor, test method--------------- IX-144- Practice figures------------------------------------------------------- X-37 Previous reports on the process ------------------------------------------------ VII-23- Previous reports, see also "Introductory Notes" at front of book Process, for the different Aroclors---------------------------------------------------1-2 in detail -------------------------------------------------------------------- Section VI records --- ------------------------------------------------ ---- -------------- VI-36- reports ------------------------- -------------------- -- see "Previous reports" see also ------------------ --------------- ------------------------------------- Section X Production standards ---------------------------------------------------- X-4, X-38, X-ll- --------------- --------------- see also "Practice figures" Production summaries ------------------------ X-17- Publl cations------------------------------------------------------------------------------------------- VII-29 -------------------------------- see also "Bulletins" and "Reports" Pumps------------------ XII-69- Pyralene----------------------------------------------------------------------------------- ------------ IX-183 Pyranols, batch record sheet---------------------------------------------- VI-46 comments on blending of---------------------------------------------------- VII-7 listed------------------------------------------------------------------------------------------1-4 specifications --------- ------------------------ IX-18-, IX-31, IX-36- sp. gr.-temp. data-------------------- III-12 test method for T.C.B.content --------------------------------- IX-106- Pyroclors------------- --------- ---------------------------------------------- ---------------------------- 1-3 QUENCHING OP STILL BOTTOMS ----------------------------- ------------------------- -- VI-18 RAW MATERIALS, testing of bulks before blending for Pyranols ------------------------------------------------------------ VI-32 Receivers for vacuum stills ------------------------------VI-15-/VI-21, XII-27 Record Sheets ---------------------------------------------------- see "Operating Records" DSW 257600 STLCOPCB4061719 Index Page 10 Refractive Index Test Method, Aroclors etc. ------------------------- IX-84a general------------------------------------ IX-157- glycidyl phenyl ether ------- IX-163 Reports (previous) process ----------------------------------------------------------VII-23- research---------- --------------------------------------------- VII-25- Re search reports------------------ VII-25- Reslstant paints and drum lacquers (Aroclor) ------------------------ VI-35 Resistivity, Aroclors ----------------------------------------------------------------------- III-16 test method--------------- ------------------------------------------ - IX-141- Retorts for solid Aroclors --------------------------------------------------- XII-77 Ring and ball test method------------------------ *--- see "Softening point" SAFETY see "Hazards" Samples sent to MCL, raw materials ------------------------------------------------ IX-9 finished products ------------------------------------ IX-183 Sampling procedure, Aroclors etc. ----------- VI-28, VII-14, IX-108- Santowax, melt tank for----------- ------------------------------------------- VI-2, XII-24 sample sent to MCL------------------------------------------------------------ IX-9 Santowax R, phys. and chemical properties-------------------------------111-5- Scale of Working----------------------- --------------------- see "Capacity of Plant" Scavengers for chlorides, addition of --------------------------------- VI-33 alternatives ---------------------- VII-8, VII-22 chemistry of ------------------------------------ IX-182 comments on------------------------- ---------------VII-8 effect of on chloride test --------- VI-33 patent position ----------- -- VII-8, VII-22 removed by earth treatment VI-33,VII-7 Scavengers,! see also----- -------------------------- -------- -"Dlbutyl diphenyl tin" ----- -----------------------------------"Glycidyl phenyl ether" -------------------------------------------------- "tin tetraphenyl" Scrubber liquor, changes in density of -------------------------- VI-7, VI-10 inventory factors -------------------------------------------- VI-53 Scrubbers on off-gas ----- ------------------------------------------------------- XII-22- etc. handling of ------------------------------------ VI-6, VI-10- Scrubbers on vacuum stills---------------------------------------------- XII-19 etc. comments on ----------------------------- VTI-4- impregnation of ------------- VII-4- Scrubbing of- off-gas, comments on ------------------------------------------------ VII-3 Services, requirements of ---------------------------------------------------- X-12a, X-39 Snift gas --------------------------------------------------------------------------- see "Chlorine" Softening point, method of determination, control test-- VIII-2- Aroclors and Montars----------- -- IV-59 DSW 257601 STLCOPCB4061720 Index . V- Page 11 Softening points, of Aroclors (charts) -------------------------------- III-10- of Montars (table)--------------------------------------- III-17 Solid Aroclors------------------------------------------------------ see "Aroclors, solid" Solubility data (Aroclors)--------------------------------------------------------------III-16 Solubility of gases in Aroclors-------------------------------------------------- III-16 Specifications ------------------------------- --------------------------------------------- Section IX Specific gravity, test method. Aroclors -------------------------------- IX-71- general method -------------------- IX-96- glycidyl phenyl ether------- IX-164 trichlorobenzene ---------------- IX-69 Specific gravity vs. chlorine content (Aroclors)chart------ III-15 vs. lbs. chlorine and % chlorine content (Aroclors) chart ------------- VI-48 vs. temperature (Aroclors) --------------------- III-12- Stability test -------------------------------------------------- see "General Electric" Stability test method (TCB) test method--------------------------------IX-120- Stabilization of TCB---------------------------------- -------------------------------------- IX-10 Stabilizers for Aroclors-----------------------------------------------------------------VII-9 Stills see "Vacuum stills" Sulphates, test method in Pyranols etc. -------------------------------- IX-174 Synopsis of Process --------------------------------------------------------------------------- 1-1- TABEE OF CONTENTS------------------------------------------------------ see front of book Tanks, closed ------------------------------------------------------------------------------------- XII-7- open-------------------------------------------------- -------------------------------------- XII-68 Terphenyls, phys. and chem. prop. ---------------------------------------------- III-6 see also------------------------"High boilers" and "Santowax" Test methods, MCL report mentioned-------------------------------------------- VII-31 ------------------------------------ Section IX see also----------------------------------------------------"Control tests" Thermal data----------------------------------------------------------------------------------------------II-2 Tin tetraphenyl, chemistry of action -------------------------------------- VII-14 ~ crystallizes out fromAroclors------------------ VII-8 ' determination of inPyranols ---------------------- IX-129 effect of on chloride test------------- IX-l8l, -182 mentioned------------------------------------------------------------------- 1-4 patent position -------------------------------- VII-8, VII-22 removed by Attapulgus earth ------- VTI-7> VII-15 sample sent to MCL---------------------------------------------- IX-9 specification -------------------------------------------------- IX-4- test methods ---------------------------------- IX-132- use of--------------------------------------------------------------------- VI-33 DSW 257602 STLCOPCB4061721 Index Page 12 Toluene blends, specifications for ------------------------------------------ IX-27- specification----------------------------------------------------------------------------- IX-2 Towers ------------------------------------------------------------------------------------------------- XII-85 Toxicity ----------- ------------------------------------------------------------------- VII-19, XI-1- literature review mentioned ---------------------------------------- VII-29 references------------------------------------------------------------------------------- III-2 warning on labels -------------------------------------------------------------- VI-34 "Treatment" of distilled Aroclors --------------------------------- VI-27- comments on -------------------- VII-6- see also"Attapulgus earth" Trichlorobenzene, quality of, comments on ----------------------------- IX-8- discussion of---------------------------- IX-8- phys. and chem, properties--------------------------III-6 sample sent to MCL-------------------------------------------- IX-9 solvent effect ---------------------------------------------- VII-17 specification for raw material--------------------IX-6 finishedproduct -------- IX-35 test methods------------ --------------- IX-68- Tri-tetrachlorobenzene, cheaper than trichloro -------------------- IX-40 isomeric ratio -------------------------------- IX-168- speclfication of --------------------------------- IX-7 test methods ------------------------------------ IX-I67- use of------------------------------------------------------ VII-8 Turbidity,test method----------------------------------------------------------------------IX-159- ' see also under-------------------------------------- "Colour" UNSTABLE BYE-PRODUCTS OP CHLORINATION--------------------------II-l, VII-16 Uses for products -------------------------------- see applications of products Utilities ----------------------------------------------------------------------------- see "Services" VACUUM STILL HEATING COILS ------------------------------------------------ XII-44- etc. sketch -------------------------------------------- VI-20a Vacuum stills --------------------------------------------------------------------------------- XII-78- discussion of --------------------------------------------------- VII-5- operation of ---------------------------------------------------------- VI-14- Valves, choice of--------------------------------------------------------------------------------- XII-5 Vapotester --------------------------------------------------------------------------------------------- XI-6- Vapourizer for chlorine--------------------------------------------------VT-2- Vapour pressures of Aroclors ---------------------------------------------------- 111-8- curves --------------------------------------III-9a- at low temperatures (report mentioned)----------- VII-29 DSW 257603 STLCOPCB4061722 Index Page 13 Vegetation, effect of Aroclors on------------------------------------------------ XI-5 Viscosities of Aroclors---------------------------------------- ---------------------- III-8- ' charts -------------------------------------------- III-10- Viscosity, conversion graph ------------------------------------- ----------------IX-6lb general test method---------------------------- IX-112- Parlin method (Du Pont)-------------------- IX-179 test method------------------------------------------------- ----------------- IX-6la- WATER, TEST METHOD, IN AROCLORS ETC. --IX-65-, IX-102, IX-104for traces -------------------------------------------------IX-65- Weighing scales -------------------------------------------------------------------------------- XII-83 Welfare----------- ------------------------------------------------------------------------- -- Section XI XENENE------------------------------------------------------------------------- ------see "Diphenyl" YIELD FIGURES -------------------------------------------------------------- X-15 computation of----------------------------- X-3- standard----------------------------------------------------------------------- X-ll- DSW 257604 STLCOPCB4061723 AROCLCR PROCESS 313 Cl I ?T I Of TABLE OF CORTOTS PART I - Synopsis of Process II - Reactions And Stoichiometry III - Flow Diagrams (a) Materials (b) Equipment IV - Equipment List V - Specifications (a) Crude Materials (b) Finished Products (c) By-Products VI - Process In Detail Comments on Process VII - Operating Instructions In Ua (a) Emergencies (b) Operating Instructions (c) Explanation of Record Sheets (d) Special Operating Instructions {) Utility Failures (f) Health and Safety VIII - Hazards & Means to Safeguard Men-Material and Equipment XX - Method Used to Take Inventory & Evaluate Materials on Hand X - Cost Factors XI - Status of Process Development DSW 257605 XII - History of Manufacture by Monsanto *1 PAGE 4 7 9 10 11 14 48 49 51 36 57 67 82 83 84 108 115 127 130 132 13* 158 161 166 STLCOPCB4061724 PART I SYNOPSIS CP PROCESS DSW 257606 STLCOPCB4061725 OoWtJ I'M i-OFrfTis Aroclor 1260 From Storage TCB From Storage TTCB From Storage Aroclor 1254 SPARKLER FILTER BRONZE 2' I.D. X 2 1/2' SPARKLER FILTER BRONZE 2' I.D. X 2 1/2* SPARKLER FILTER 304 S.S. 3'6" I.D. x 3' FVranol 146' Pyranol 1470 Ptranol I486 Tnerteen FFO-TCB Inerteew FFO-TTCB Ptranol K8 I DSW 257607 PYRANOLS DEPT A-246 W.G.K. PLANT SEPT. 20,1957 810.90 STLCOPCB4061726 DlPHtNTVU Storage-] DIPHENYL MEA3URIN0 TANK STEEL 650 SAL. Vent | m UR BLOW TANKS (2) STEEL. 2000 OAL. WITH 00 OPM PUMP CHLORINATORS (5) STEEL, 850 OAL., 20 FT* EXTERNAL COOLINO AREA, 200 FT* JACKET COOLINO AREA, WITH 1' I.D. X 10'10" 0FF-0A3 SCRUBBER 2' I.D. X 6'T" CYCLONE SCRUBBER, 650 OAL.SCRUB LTdlOH TK.A'ao PPM POMP 3 O 'Ho1 M Ofi* Gab *~To Deft. l7,f-2/5, or 257 3v i--Air 2. FUME SCRUBBER 8" HAVSO \ DUAL AIR DRYER, ACTIVATED ALUMINA '-To Sewer ' J l VACUUM 3TIL-L, BATCH, 3TEEL, 2500 OAL. 100 FT* COI L AREA ? VACUUM STILL, SEMI AUTOMATIC, STEEL 1000 OAL., 44 FT* COIL AREA 4i flONTAR *3 >- AND *-* PIONTAR ^4 - STEAM CONDENSER (2) glKEL 31* FT* BACH TI I I I I TANGENTIAL SEPARATOR 3' I.D. X 6 i 1 1 I i [ i DI3TILLED WATER TANK(2) STEEL, 110 OAL. GRAVITY CIRCULATION AROCLOR CONDENSERS (2) MONtL, 47.J FT* BACH 1 l 1 1 ----- ....J CENTRIPIX SPARKLER PILTER 304 S.S. 3'6" X 3' ^3 Stage Steam Jet Ejector Toluene- Attapulgus Earth! CONS SCRUBBERS (2) STEEL 530 OAL. ( )still receivers 2 MONEL 1000 OAL. BLEND TANKS (2) ZINC (0.005") AND TIN (0.003") SPRAYED, 2100 OAL., BRONZE AOITATOR WITH 504 S.3. 100 OPM PUMP RECEIVERS (2) ZINC (0.005") AND TIN (0.003") SPRAYED 2100 OAL. DSW 257608 JAroclor Storag AROCLORS DEPT. 24S W.G.K PLANT SEPT. 19J967 811.00 STLCOPCB4061727 BATES LABEL NOS. DSW 257609 through 257719 NOT USED STLCOPCB4061728