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Copy No. process tor; THE PRODUCTION OP AROCLORS,; PYRANOLS, ETC. AT THE ANNISTON AND A|T THE WM. 0. KRUMMRICH PLANT April 1955 ----- f------------------------ E. Mather Distribution List; 1. Mr. J. S. Brough, London 2. Dr. N. B. Dyson, Newport 3. Mr. 0. V. Taylor, Newport 4. Mr. 0. V. Taylor, Newport 5. Mr. W. E. Hamer, Ruabon ^6. Mr. J. P. Stlckley,------------Krummrioh Plant 7. Mr. J. P. Stlckley,-----------St. Louis Library 8. M. C. L. file at Sti Louis 9. Mr. D. B. Hosmer, Aijnlston 10. Spare MONS 045979 TABLE OP CONTENTS TABLE OP 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 OP THE PROCESS CHEMISTRY OP THE PROCESS PHYSICAL AND CHEMICAL DATA PLOW SHEETS PLANT LAY-OUT PROCESS IN DETAIL COtHENTS ON THE PROCESS CONTROL TESTS SPECIFICATIONS AND TEST METHODS: RAW MATERIALS FINISHED PRODUCTS PLANT OPSRATUKl DATA: HAZARDS CAPACITY YIELDS MATERIALS CONSUMPTION SERVICES COSTS EQUIPMENT AMENDMENTS HISTORYJOP THE PROCESS IN MONSANTO OPXRATINO INSTRUCTIONS ACKNOWLEDGEMENT INDEX MONS 045980 INTRODUCTORY NOTE INTRODUCTORY NOTE When the MCC Aroolor process vfae studied in 1947 in preparation for the erection of a plant In Britain, an excellent report "Dept.246: Aroolor Prooeas" Iyles, Soffr4nko and Becker, Septemoer 1946, des cribing the Plant "B" (now th$ Krummrich plant) prooess, was available. Supplementary information was collected Into a report "Notes on the Plant 'B' Manufacturing Prooess for Aroclors" by E. Mather, April 1947, and soon afterwards the report "Notes on the Anniston Aroolor Plant", B. Mather and D. 3. Haveroroft, September, 1947, was written. More Information came to hand from time to time,Including the "Prooess Description for Aroolor, Dept. 246", C. H. Schwartlng, J. P. Neff and J. W. Craves, November 1953, sIbo a revised version of this by Schwartlng and Schwartz, March 15, 1955, and visits were paid to the Anniston and Krummrloh plants for the purpose of revision early In 1955 Haveroroft 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" Iyles, Soffranko and Miller, March 24, 1947. subsequently the MQC report "Process Description for Pyranols and Inerteens", Schwartlng, Neff and Oraves, October 1955, appeared. Numerous researoh 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 replaoe; they were drawn up to give Just the essentials of the prooess work. The present report tw Intended to condense all the process infor mation up to about March 1955, Into the form used for MCL prooess reports. The Pyranol process has been Included in the same report because it dovetails so closely into the Aroolor process, and the writing of a separate report for Pyranols would have Involved a good deal of repetition. HONS 045981 l 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 ohlorlne corresponding to the grade of Aroclor required. The crude ohlorlnatlon product Is usually air-blown to remove dissolved gases, and then either Is sold as orude Aroclor, or It Is worked up Into distilled Aroclor. The distilled product is usually treated with Attapulgus earth. The following table shows tthioh of these steps are Involved lr) making each of the different grades of Aroclors. All the operations are done batchwlse, except that some of the distillation Is done In a semi-continuous manner. MONS 045982 SYNOPSIS OP THE PROpBSS, contd. r-2 SYNOPSIS Grade Diphenyl Crude HB Distilled KB used 0 Chlorine Airblown Distilled Earth Treated Nature of Finished Product 1142 DP 42 ye8 no no 1242 DP 42 yes yes (vao) yes 1148 DP 48 yes no no 1248 DP 48 yes yes (vac) 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 DP 62 yes yes (vao) yeB 1262M is 90* Aroclor 1262 by welg it, 100 Toluene 1168 DP 68 yes no no 1268 DP 68 yea yes (vac) no 1169 " DP"' 1269 1170 1270 1171 1271 2565 4065 4465 5060 ' DP DP DP DP DP 75* DP 25* CHB 60*. DP 40* DHB 60* DP 40* DHB DHB 5460 DHB 69 69 70 70 71 71 65 65 65 60 60 no no no yes,atm.pr. no no no yes, atm.pr. no no no yes, atm.pr yes no no no no no no no no yes no no yes yes, (vac) yes no yea yea, (vac) no no no Dark oil Clear oily liauld Dark oil Yellow oily liquid Dark viscous 11auid Yellow viscous liquid Dark viscous sticky mass Lt.yellow atlckv mass Dark sticky mass Lt.stlcky resir Dark crystal line solid Dark crystallne solid Dark crystal- Flaked Cryst. solid Flaked Flaked Black brittle resin. Black brittle resin Clear lt.yeBow brittle resin Black brittle 'resin Clear It. yellow brittle resin HONS 045983 I -3 SYNOPSIS SYNOPSIS OP THE PROCESS, contd. Aroclors up to and including 1262 are usually spoken of as "liquid Aroclors"; those from 1267 upwards are called "solid Aroolors". 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 chlorlnator, and a special still. MCL research report 416A, 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 53/97/5 February 1954 describes the "topping" of 1254 for a special customer, and 25/11/54 describes the prepar&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 oases 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 Fyranols (Fyroolors, Inerteens, Askarels) Involves at the most only a blending operation to arrive at the compositions as set out in the following table. - MQNS 045904 SYNOPSIS OF TOE PROCESS, contd, I-4 SYNOPSIS Trl Chl.bz. w/vr % Trl-tetra Aroclor Chi. bz. 1254 1260 Tin Tetra phenyl Pyranol 1467 1476 1478 1481 1482 1488 1495 Inerteen PPO- * TOP-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 ~ - Qlycldylphenyl ether 0.20 0.20 MCL Research Pro 5ress report 3470, 51/141/12, June 1952 d scribes certain variants of these. | | _______________ 1 ____________ !____________ 1______ 1_____ Pyr&nols are products for the (American) General Electric Company. Pyroclora are the MCL products corresponding to the Pyranols. Inerteens are made for Westlnghouse. Askarel Is the MCC trade mark. The trichloro-benzene and the trl-tetra chloro are used to Increase the fluidity of the Aroolors 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 glycidyl phenyl ether are "chloride scavengers" as discussed In section VII below. * PPO denotes phenoxy propene oxide. a synonym for glycidyl phenyl ether C,H_-0-CH, 65 * MQNS 045985 II. CHEMISTRY OF THE PROCESS II - 1 CHEMISTRY OF 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-containlng^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 atomlo weights: H - 1.008 C - 12.01 Cl - 35.^55 we have for direct substitution M-.wt. * Cl Compare Diphenyl C12H10 154.20 Trlohlorodiphenyls C^gH^Cl^ 257.54 41.3 Aroclor 1142, 1242 (42*C1) Tetra Penta Haxa Hepta Octa Ennea 12H6C14 291.99 48.6 Aroclor 1148, 1248 (480) Ci2H5C15 326.44 54.3 Aroclor 1154, 1254 (54*) ^12^4^6 360.88 59.0 Aroclor 1160, 1260(60*) C12H3C17 395.33 62.8 Aroolor 1162, 1262 (62*) C^gH^Clg 429.77 66.0 C^HClg 464.22 68. a: 'Aroclor 1168, 1268 (68*) Decachlorodlphenyl c12c1iq Terphenyl ^gH^ 498.67 71.2 Aroclor 1171, 1271 (71*) 230.29 Deoachloroterphenyls C18H4C110 Vndecaohloro C^gH^C!^ 574.76 61.8 Aroclor 5060, 5460 (60*) 609.21 64.0 HONS 045986 T CHEMISTRY OF THE PROCESS, oontd. II - 2 CHEMISTRY OP PROCESS The conditions of chlorination (high temperature^-and local excjsa-^ of chlorine) are such that,for example ,Aroclor^l26JJ containin^60Jt^, of chlorine,corresponding about to Ci2H4C16 will'certainly contain considerable amounts of 01285015, C12H3CI7, etc. Further, there will probably be a very large number of isomers of, for example, C12H4Cl6. This 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 product would not necessarily be identical with Aroclor 1254 made by direct chlorination of diphenyl to 54j< chlorine content. This is of practical importance because partial crystallization of liquid Aroolors, which has ocoured, and which 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 11- section VII, below. Chloride Scavengers. See the discussion of the action of scavengers in Section VII, below, pages 6-. Heat of 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, (1. e. about 20 kg. cal. per g. atom fed in). The heat of evaporation of Aroclcya. Trouton's rule (g. eal/g.mol 21 x B.Pt. *C. abs) gives, for example, for Aroclor 1260 of M.Wt.about 360 and mid B.Pt. about 395*C.(668*abe) 14,028 g. oals. per g mol, or 39 g. cals per gram. HONS 045987 III. PHYSICAL AND CHEMICAL DATA Ill - i Pbys .SeChem. Data Physical Constarts of Diphenyl Compiled by W. P. Metzr.er Date: Pebruary 12, 1943 Corrected: June 22, 19*13 Corrected: Jan. 11, 19**** <) Bellstein V-576 NAME SOURCE DATE Formula Appearance W65 Monocli flic Molecular Weight 154.20 ` Bolling point at 760 mm 255*0. Bolling point at 10.4 mm 118c. Crystallizing point 69.0*0. Melting point 69 *C. Solution point. Specific Gravity at 77/4*C. , 0.9896 Specific Gravity at 20/4*C. 1.041 Refraotlve Index at 77.1*C. D - 1.58822 Viscosity at 100*C. 28.8 Say. Sec. Surface tension at 129.2*0. 29.5 dyne/cm Solubility in water at 60 *C. Insoluble Not#: Piles of W. P. Metzner, St. Louis Chem.Rubber handbook 1941 1942 Chem. Rubber handbook Int.Crlt.Tables 1928 Swann file #137* Swann curves * 1935 1934 Int.Crlt.Tables 1928 Int.Crlt.Tables 1928 Int.Crlt.Tables 1928 Int.Crlt.Tables 1928 Swann Plle#137A 1930 Int.Crlt.Tables 1928 Dow 1943 MQNS 045988 T III. PHYSICAL AND CHEMICAL DATA, oontd. Physical Constanta of Diphenyl, oontd. III - 2 Phys.A Chem. Data NAME SOURCE DATE Viscosity at 70 *C. 31.2 Say. Sec. Swann Pile #137A* 1930 Solubility in Abs. Ale# Ale.at 19.5*0. 9.98 g./lOOg.solvent Seidell 1941 Solubility in 100# Methanol at 19.5*C. 6.57 g.AOOg. solvent Seidell 1941 Benzene at 27.9*C. 137g./100g.solvent Seidell 1941 Heptane at 26.5*C. Plash point *P. Plre point P. Heat of oombustlon Kg-cal. (15*) Heat of formation 25.1 g./lOOg.solveHt Seidell 235*P. - closed cup Ind. Jc Eng.Chem. 255*P. - open cup 22,882 124*0. Dow 1941 1940 1943 per gm.mol-1504.4 Int.Crit.Tables 1928 Latent heat of fusion Latent heat of vap. at 69.2*0. 28.8 gm-cal.per gm. (53.1 BTO/lb.) Lange Handbook 1937 190.9 Btu.per lb. Swann Pile #137A* 1928 Speciflo heat at 40*C. (solid) J.387 cals/g 1.6l Jouls/gm. / Int.Crit.Tables 1928 Crltioal temperature Crltloal pressure Dissociation constant _ -. - -_ -- Pounds per U.S.gal.at 77* C 8.23 lbs.per gal. Swann Pile #137A 1930 Toxlolty (1) Dr.MoLester,Anniston Plant Report 1997 (2) Peroy May "Chemistry of Synthetic Drugs" 3rd.Ed.p.IS NOTH! Piles of W. P. Metzner,St.Louis. HONS 045989 III. PHYSICAL AND CHEMICAL DATA Ill - 3 Phys.fc Chem. Data 1. Diphenyl Specific Oravlty: 0.992 at 75*C/4*C. The Swann Chemical 'Company bulletin of 1930 gave thermal data on diphenyl Vlecoalty of Diphenyl (from Anniston flies) p. 160 170 180 190 200 220 250 300 350 400 450 482 Centlpplses 1.439 1.309 1.206 1.114 1.034 0.901 0.792 0.57* 0.459 0.37* 0.313 0.283 Specific Heat (from Anniston files) p, 200 300 400 500 600 700 800 900 1000 B.t.U./lb. 0.416 0.470 0.5*7 0.616 O.658 0.679 0.686 O.690 0.696 MOWS 045990 I III.PHYSICAL AMD CHEMICAL DATA, oontd. I. Diphenyl, oontd. III - 4 Chem. Jt Phya. Data Another record gives the following values for liquid diphenyl: c. Sp. Heat cals./gram 100 150 200 250 300 350 400 450 0.360 0.380 0.412 0.460 0.518 0.575 0.610 0.625 Vapour Cp 0,460 250*C. 0,625 450*C. (D. A. Roper, Design Data for Units 4*5) Density of Liquid Diphenyl (from Anniston flies) *C. 75 100 150 200 250 300 350 400 450 0.9885 0.9695 0.9294 - 0.8885 0,8470 0.8010 0.7510 0.6918 O.618O Heat of Vaporization: 65.4 g. oal./g. at 258.5*0. HONS 045991 III. PHYSICAL AMD CHEMICAL DATA, contd. Ill-5 Phys.i Chera. Data 2. Distilled High Boilers Santowax .FI contains about Vft diphenyl 10# ortho terphenyl 46j< meta terphenyl 21j< para terphenyl 22% trl'orthophenylene, quaterphenyls etc. (Anniston Final Report 1942) Upper hold point Lower hold point 137-143*0. Changed ) 137-145*0. 45-60'C. Sept.23/47) " 45-63*C. 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 Oravlty of Crude Santpwax: 140*C. 175 215 300 1.026 1.000 0.98 0.964 (est. from curve of other points). Vlsooslty of Santowax R 155C. 225 32.4 Saybolt Universal Seconds 28.5 , " " " Molten Santowax flows about like water at 25*C. (A.M.Ellenburg's letter January 6, 1949). (Probably 250*C. was intended). Speolflo Heats (estimated) Solid Liquid 0.4 0.5 Latent Heats (estimated) Fusion 63 B. tf. u./lb. Vaporisation 140 B.t-.u./lb. HONS 045992 III. PHYSICAL AND CHEMICAL DATA, oontd. 2. Distilled High Boilers, oontd. Ill-6 Phys. & Chem. Data Santowax R, oontd. Bolling Range: 360-450*0. Flash Pointi Cl.open cup 191*0. Flame Point! Cl.open cup 238*0. Another aocount gives Flash Point 190*C; Flame point 220*C. Values assumed in the design of the Santowax still at Anniston: Specific Heat Heat of Vaporization Visoosity at 250*C. Visooslty at 350*C. 0.5 140 B.t.U./lb. 5 oentlpoises * 2 centlpolses * (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 53 - 55*C. 205 *C. 2% l2*o!) mlxture 240*c- 84.8*C. about 74*C. See also Monsanto Technical Bulletin #P-103> January 4, 1947 issue, for the properties of the separated crude isomers sold. 3. Trlchlorobenzene Dr. Jenltlns, January 27, 1954, refers to Ind. Eng. Chem. 3g. (1947) p. 517 for vapour pressure data, MONS 045993 III. PHYSICAL AMP CHPUCAI DATA, cootd. Ill - 7 Phye. * Cham. Data Aroolora The main characterlatloa of tha Aroolora are given in tha following table; Orad. M. Pt. c. " ' Spaolflo Oravity r... Sp. Or. Vlacoalty oo.ff. Saybolt p.r *0. Seoonda Dlatllllng Range *C. 10 - 90* Pour Hold Point Point c. *C. Softening Point ASTH 1142 1.348 to 1.353 0.0009 65/15.5*0. 1242 1.338 to 1.348 0.0009 50 to 53 65/15.5*0. at 54.5*0. 1148 1.412 to 1.415 0.0009 65A5.5'0. 1248 1.404 to 1.414 0.0009 73 to 80 65/15.5*0. t 54.5*C. 1154 1.500 to 1.510 0.0009S 65/15.5*0. 1254 1160 1.495 t 1,505 3,00093 ,44J to 47.3- 365 to 390 8-12 65/1515*0. t 98.9*0. 1.558 to 1,563 0.0010 90/13.5*0. 1260 1.550 to 1.560 3.0010 7? 49 77 385 to 415 26-34 90/15,5*0, t 98.9*0. 1162 1262 1,58, to 1.587 0.0010 90/15.5*0, 1.572 to 1.583 0.0010 88 to 100 90/15.5*0. at 98.9*0. 1262K 1168 1268 1169 1269 1170 1270 1171 1271 304*0. min. 2565 4065 4465 5060 5460 160 to 210 t 130*0. 145-165 135-160 225-250 285-255 285-300 "66.0 to 72.0 66.0 to 72.0 110.0 to 115.0 100 to 105.5 Saa alao Phoaphate Dlvlalon report 171-102 'Highly chlorinated quater phenyli" aent to Mr. Hamer, Maroh 12, 19*18. MGNS 045994 III. PHYSICAL AMD CHEMICAL DATA, contd. Ill-8 Phys. te Chem. Data Other properties are listed In Seotlon IX, Finished Product Speci fications. MCC Bulletin P-115 gives the following data not Included In either of the foregoing lists: -- Oeneral description of the Aroclors: (non-oxidising, permanently thermoplastic, chemical Inert, will not bum, compatible with most non-hydroxyllc solvents, good electrical properties and fire resistance, adhesive, and non-drying). JEvaporation loss i data, % loss In: 5 hours l6?*C. and 6 hours 100'C. Flash point Fire point Refractive Index. Corrosion data Specific heat f-c. dynes /sq.cm. Surface tension (Aroclor 1254) 25 8o 100 50.3 44.0 42.0 Thermal conductivities Solubility data for many compounds Vapour pressures (semi-log ohart) 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. 3 October 1953, page 477, gives a method of determination of thermal conductivity of liquids in general. MCL Res. Prog. Rpt. 355E, 51/91/3. 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. MQNS 045995 III. PHYSICAL AND CHEMICAL DATA, contd. in-9 fhya.it Chera. Data Vapour pressure curves for some of the Aroclors are given on pages 72 - 75 of the report by Iyles, 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 100*C. were given In a report from the Southern Researoh Institute, Birmingham, Alabama. (Report No. 1, project 526, to MCC February 4, 1954). All these data are shown In logarithmic form on pages III-9aJeb below. Dr. Roebuck, then at Ruabon, in a letter dated June 8, 1953, 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 171-1089, 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 13, and September 17, 1953. A final report under this Job number was promised July 16, 1953. Newport Plant Teohnloal Committee, December, 1953, recommended Investigation Into combustion methods of determining the concentration of Aroclors In air. Mr. Benlgnus, of St. Louis, September, 1953, dlsoussed 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 the Pyranols containing 33j<, or more, of Trlchlorobenzene, the vapour pressure of the Pyranol might be taken as equal to that of TCB alone up to about 150*C. 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 54/16/9, September, 195 4, reports the vlsooslty of Aroclor 2565 from 100 to 130*C. Report 1152, DF 52/26/6, August, 1954, discusses the viscosity, and the vlsooslty Index of a tlntetraphenyl blend of Pyranol. HONS 045996 T .b*. MOMS 045997 i i i - io P h y s .4 Chem VISCOSITY IN CBitIFOISBS a t 130*C iii-n P hy3.& Chem. III-12 Phys.ft Chem. Data III. PHYSICAL AND CHEMICAL DA^A, oontd. Specific Qravlty-temperature data are given on page 11 of MCC Bulletin P-H5 also on pages 13, 14 and 15, of Section III, below. The coefficients of fall of speolfic gravities of the Pyranols with Increasing temperature in the range between 45 and 85*C. are as follows: -- 1467 and 1488 1495 0.001 per 1*C. 0.00285 per 1*C (Lyles, Soffranko It Hiller page 43) MONS 046001 III. PHYSICAL AND CHEMICAL DATA, contd. Specific gravity of Aroclora at Various Temperatures III-13 Chem.St Phya. Data For 1242 Temp. *C. 60 65 70 75 80 85 90 95 100 Sp. Or. 1.347 1.3^4 1.338 1.335 1.332 1.329 1.324 1.319 1.315 Lbs. per Qallon(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 1.394 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 OK 1476 60 65 70 ' 75 60 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 oontd... HONS 046002 III-14 Phys.iChem. Data III. PHYSICAL AND CHEMICAL DATA, contd. Speclflo Oyavlty of Aroclors at Varlyia Temperatures (Sontd.} For Temp. *C. Sp. Or. Lbs. per Qallon(US) 1260 or OS 1462 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 13.21 13.17 13.13 13.09 13.05 13.01 12.96 12.92 12.88 1262 60 65 70 75 80 85 90 95 100 1.604 1.600 1.597 1.593 1.588 1.582 1.577 1.572 1.568 13.40 13.36 13.32 13.28 13.24 13.19 13.15 13.11 13.07 HONS 046003 III. PHYSICAL AMD CHEMICAL D|ATA, oontd. III-16 Phys.4 Chem. Data Solubility Data MCC Bulletin P-115 Includes data- on the compatibility of Aroclors with numerous solvents. MCC report 2949, October 28, 1953, 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 5^60 In Dutch Shell Co.'s Risellaoil. See also the disousslon 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 Ruehrweln, January 1949, states that the solu bility of saygen in 1254 at 25*C. Is about 1 x 10" moles of oxygen per gram of Aroclor. On December 29, 1953, Dr. Gardner enquired for data on the solubility of gases in Aroclor up to 7000 pslg, but MCC could not supply any data. The following MCL Research Reports deal also with questions or compatibility: -- Job 1152, 51/141/20 etc. "Effect of Pyroclors on eleotrlcal wire Insulation"-- softening and loss of break-down strength -- Pyroclors unharmed.. See also under "Caskets" In Section XII, below. Job 1151, DF 53/86/1, September 1953. "3olubillty of methyl anthraquinones etc. In Aroclors". Job 1151, NR 53/97/8 "Solubility of TTP in Aroclor 1248" Also MCC report 2272, "Solubility of Aroclor 5460 In various solvents", Wade, December 19^8. 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 120*C. corresponds to about 85 x 109 at 100*C. (Aroclor 1254 - - MCL Specification 500 x lO^ ohm/om* minimum at 100*C.) MOWS 046005 T HI. PHYSICAL AMD CHEMICAL DATA, contd. III-17 Phya.i Chem. Data M 0 N T A R B (1946 data) Softening Flash Fire Penetration Chlorine Iron Calcium Acidity Irade Point Point Point B50g.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. basic % 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 1CT2 per 5 sees. -- Montar #9 la the residue from the diphenyl process; data on It Included here only for convenience'. No data found on Montar #7. - MOMS 046006 IT-1 HONS 0 4 6 0 0 7 rr-u Flow Sheet Joantities per 100 lbe. of Aroelor 12*2 (150 lbe. of Aroelor 11*2). .Approximate quantities, net bard and fut process Instructions ) (Quantities for other Aroclors may be ea leuIsted In the seme way from the data In Section X below). Stream 13 *6 10 12 13 1* 15 16 17 18 19 20 21 22 23 2* 27 28 29 30 31 32 3* Diphenyl 63.85 Chlorine BC1 92-1 rraee *T.* Trees trees *7.* *7.* Pree^ 6.1 *1.3 *1.3 *0.3 1.0 Trace frees Aroelor Water 5.0 5.0 9*-8 12.2 82.6 108.55 108.55 82.6 60.6 2.0 102.5 2.* 100.1 LOO. 1 0.1 100.0 6.05 Carbon 2.0 2.0 2.0 Attapalgua earth 0.05 0.05 0.05 Urns TOTAL 0.5 0.5 <*) 63-85 92.1 52-* 5.0 *7.* *7.* 9*-8 18.3 123.9 2.0 125-9 120.9 5-0 108.55 108.55 102.5 (#) 0.5 2.9 100.1 0.05 100.15 0.15 100.0 (*) 6.05 () fetal loea from absorption system. (4) lapped at intervals. (x) Total working losses of Aroelor; about 2.5 in the crude stage and 3*55 in the refining stage. HONS 046006 * * *ru MONS 046009 T Flow sheet or EquiQMg^r PyRNOl.S n< INERTEENM **m7 i - V-o in > Th Aroeldr lrr CT-oyfq hv~h #-onf7 F - on* f Pyrftn* it> 6rnd 11#I MUNS 046010 I VII - 25 Comments VII. COMMENTS OH THE PROCESS, contd. List of Reports, contd, MCC RESEARCH PROGRESS REPORTS Job, No. 117-790 Report No. 2673 Use of dilute chlorine December 10, 1951 Date Opples sent to MCL January 30, 1952 117-1987 Method of determination of stability of TCB Munch and Ashworth October 16, 1950 117-1987 part I Infra-red studies, TCB and Pyranol 1467 May 7, 1948 117-2032 Tentative Amendment to Process for TCB, Hubbard and Steahly October 16, 1950 117-4013 Aroclor 5^60 toluene solutions 171-718 2771 Effect of exposure of Aroolors to steel April 27, 1953 171-719 2772 Containers for Aroclor 1242 April 27, 1953 171-1027 A series of reports on minor Inquiries from Sales April 14, 1953 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. MONS 046109 T VII - 26 Comments VII. COMMENTS ON THE PROCESS contd. Llat of Reporta, contd. MCC RESEARCH PROGRESS REPORTS, contd. Job No. Report No, Date Copies sent to MCL 171-1029 2788 Use of Aroolora with aeo. butyl acetate and a aeries of reports on asalstance to fie Aroclor Dept. April 14, 1953 April 27, 1953 etc. 171-1054 A aeries of reports on July 20, 1953 low-temperature dielectrics 171-1075 2887 Mlnpr Investigation for salps; examination of competitive products July 20, 1953 171-1076 Assistance to Aroclor Depertment July 20, 1953 171-1077 2883 Aroclor 5460 from Davis "Tarophen" July 20, 1953 171-1088 288V Differences between Anniston and Krunmrlch Plant8 July 20, 1953 171-1089 2892 Determination of Aroclor concentration In gases June 7, 1954 171-4013 Aroclor 5460 - toluene solutions 171-4019 Customer contacts. MONS 046110 VII. COMMENTS ON THK PROCESS, eontd. VII - 27 Comments List of Reports, contd. HCC RESEARCH PROORESS REPORTS, contd. Job No. Report No. 729-1573 Improve flexibility of operation of Krummrieh plant Semi continuous distillation. Will quicker chlorination give more hlghbollers? Date Copies sent to MCL 729-1664 Series: Maximum production rate with minor changes in equipment; Krummrieh plant. April 27, 1953 etc. MONS 046111 VII - 28 Comments VII. COMMENTS ON THE PROCESS, contd. List of Reports, oontd. MOO CENTRAL RESEARCH REPORTS Report 5*0 January 1949. Studies on Light Stability of Electrloal Resistivity of Aroclor 1254. White and Ruehrweln (Clves data on the solubility of oxygen In the Aroolor) Date sent to MCL HOC REPORTS 1877 Standard Process Report on Aroclor 4465 Ellenburg 2215 Anniston Aroclor Data book Final Report 2272 Solubility of Aroclor 5460 In various solvents. December 1948. 2498 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 3, 1951 HONS 046112 VII. C0MMEMT3 ON THE PROCESS,COntd. List of Reports, eontd. PUBLICATIONS J. Appl. Chem. 3 ' October 1953, page 477 "Method of determination of thermal conductivity" Baxter, Vodden and Davies VII - 29 Comments Am. Soc. Mech. Sng. 58 (1936) p. 719 "Thermal conductivity of Aroclors" Ind. Eng. Chem. 39 (1947) p. 517 "Vapour Pressure of Trichlorobenzene it See also MCL Research Progress Report 1151, 53/58/3, 54/26/13, D? 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, Brlmlngham, Alabama, "Vapour Pressures of Aroclors below 100*C." HONS 046113 VII. COMMENTS ON THE PROCESS. COntd. List of ReportB, contd. WCC BULLETINS "Askarel" Sales bulletin July 2k, 1953 Indirect Heater for Unit Chemical Operations ------------ MeArdle (re-Issued as bulletin P-130) Physical Properties of Arodors P-115 Properties of Aroclors (replaced the foregoing report.) P-128 Aroclor Incombustible Lubricant P-130 Indirect Aroclor Heater for Unit Chemical Operations P-137 Die casting VII - 30 Comments Date sent to MCL September 9, 1953 January 17, 1952 Requested July 7, 1954 January 28, 195: HONS 046114 VII. COMMENTS ON THE PROCESS, contd. List of Reporta, cortd. LONDON CENTRAL ENGINEERING REPORTS Preliminary Report. March 1949. Periodical reports on running-in the Newport Plant. July - November 1951. Pinal Report. , Aroclor Plant ferformance. September 1951. Operating Instructions for Aroclors September 1951 Design Book. Newport Project 41. Chemical Engineering Design. January 1950. MCL REPORT Market Research. N. 0. H. Thomas November 1947. Tentative Process and Analytical Methods February 1951. VII - 31 Comments HONS 046115 VII - 32 Comment s VII. COMMENTS ON THE PROCESS, oontd. List of Reports, oontd. MCL RESEARCH REPORTS Job Mo. 50/175/2 Nov. 50 Electrical testa 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 Sept,52 Capacltator paper. 52/48/1 Sept.52 Literature survey on uses for Aroclors. Final Reports Dec. 52 Alternating current characteristics of Aroclors.. Feb. 53 Jun. 53 Literature Survey of Uses. Electrical Testing Methods. HONS 046116 VII - 33 Comments VII. COMMENTS ON THE PROCESS, Contd. List of Reports, contd. MCL RESEARCH REPORTS, oontd. Job. No. 355E 50/193/1 Nov.50 Examination of TCB samples 51/91/1 Aug.51 Oasket materials. Aroclor 1248 as cooling medium, compared with mineral oil. 416A 52/1/1 Jan.52 Solubility of 4465 and 5460 In white spirit. Removal of green colour. Crystal formation In 1232. 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. 454e 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 Bakellte 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. FR53/58/3 Jun.53 Breakdown strength after earth treatment. Capacitors. Effect of metals on Aroclors. Material for publication. HONS 04611? l_ VII. COMMENTS ON THE PROCESS, Oontd. VII - 34 Comments List of Reports,oontd. MCL RESEARCH REPORTS, oontd. Job No. 1151 DF53/85/4 Nov.53 Blowing of fuses In Aroolors. DF53/86 Sep.53 Anthiqulnone derivatives aa stabilizers. Joint box compound. Storage m Bteel. Activated alumina In refining competitive materials. NR53/97/1 Jul.53 Stability up to 300*C. Crystal deposition In 1232. (Torque con veyors). Blending of 1221 and 1242. Topping of 1254. Puller Earth. Alumina etc. In refining. Solubility of TTP In Aroclor. Determination of Aroclor In Air. Resinous Aroolors. DP54/16/3 Mar.54 Exposure of plastics etc. to Pyroclors. DF54/26/3 Jun.54 SluaieE for hydraulic fluids. Metal exposure. Synthetic rubbers, Oaskets, mixtures of Aroolors with organic phosphates etc. Running tests. Rust Inhibitors added. Resistant paints sought. Burn point. Auto genous Ignition. V.I. Improvers. Material for publication. DP54/kY/l Apr.54 Electrical tests. Montars. Paints for piping etc. Reclamation of aroed Aroolors. Various applications studies. Gaskets. Test cell. Aroclor capacitors. Publications. MONS 046118 VII - 35 Comments VII. COMMENTS ON THB PROCESS, cortd . List of Reports, contd. MCL RESEARCH REPORTS, oontd. Job No. 1152 51/141/20 Jan.53 Teohnioal service. Bffeot on lr.3ulatlon of wire. Examination of arced material. Bffeot of Aroclor on Shellac. 53/60/1 Jvm.53', Effect on Insulation of wire. DF53/85/1 Sep.53 Technical service. Test cell. Effect on insulating materials, processed wood etc. Silicon glass ooated wire. Reclamation of used Pyroclor., DF53/89/5 May 54 Use In polishes. NR53/103/1 Jun.54 Puller'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. Caskets. Test cell. Damage by arcing. Customer's test method corrected. Viscosity of 2565. Resistivity of 1254 against time. Silicone glass fibre etc. Il6l NR54/77/1 Nov.54 Hydrolysis of Aroclors. MONS 046119 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 ko be assimilated Into the Organic Division collection of reports. Work has been done, for example, on the Isolation of the individual chlor-dlphenyls, and on Infra-red analysis of mix tures of chlor-dlphenyls, alBO 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. MONS 046120 T . VIII. CONTROL TESTS. Determination of Stloky and dummy Stages of Aroolors 1168, life, 1170. U7l VIII - 1 Control Teats 1. Shortly after a specific gravity of 1.570 at 100*C. Is passed, the Aroolors 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, oool slightly and test between the thumb and forefinger, while wearing a rubber glove. If the material is stringy it is in the sticky stage. 2. 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 Crystallising pr Hold Points of Aroolors 1168, life', 1170, 1171 !^ 1. After passing the gummy stape 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 200*C. over a gas flame. Agitate with a 0-260*0. thermometer. ~ 2. 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 - s'C. 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 2-2 minutes. If the temperature Increases after this period, then the highest 046121 mqns VIII. CONTROL TESTS, contd Determination of Crystallizing or Hold Points of Aroolors 1166, 1169, 1170, 1171l oontd. VIII-2 Control Tests 6. oontd. temperature attained will bo the hold point. However* If there Is no Increase in temperature, then the point where it held steady Is the hold point. 7. CAUTIONt Wear goggles and asbestos gloves when obtaining sample of the solid Aroclor* In the molten stage. Softening Point tSF) Determination of Aroolors 2565, 4065, 44^5, 5060, 50^5 A8TW Method The sample shall be melted nd stirred thoroughly, to avoid having air bubbles In the mass and then ppm's! into the ring so as to leave an exoess on ooollng. The ring, while being eooled, should rest on a metal plate. After ooollng, the exoess material shall be out off cleanly on top with a slightly heated knife. Fill the 600 0.0. beaker to a depth of 3-1/4" with glycerine at room temperature. Suspend the ring containing the sample and ball In the glycerine so thgt.the lower surface of the ring Is exactly 1" above the bottom of the beaker and the upper surface 2" below the upper surface pf 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 5*0. 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 chlorlnator sample for comparison and make corrections as follows: suppose the S.F. of the standard sample Is 112*0. and d^ops at 110*C., which lndloates too rapid heating* then add 2*C. to the S.P. ef the ohlorlnator sample. It Is Important to follow the setting of the ring and the thermometer as well as the rate of heating. HONS 046122 VIII. CONTROL TESTS, oontd. vni-3 Control Tests Hold Point ' A little more detail of the "hold point" test was given by Mather, November 6, 1948i A portion of the sample Is melted In a Jj" x 1" Pyrex test tube whloh is then closed with a oork carrying a thermometer, and the tube then hung In the neck of an unsllvered Pyrex vacuum vessel whloh in turn hangs In the neok of a wide mouthed glass bottle, formlhg 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 on them to save time In packing the O.K. material. made, The following sample of material In process has been sent to MCL: Distilled untreated Aroclor 1254, June 23, 1949 HONS 01,6123 T IX. SPECIFICATIONS AND TEST METHODS IX - 1 Specifi cations Speciflcatlons_for_BIPWraYI, ipjPHENYL)_(XENENE]_ (Raw Material) Code Mo. 611 Chemical Formula (K) Date: 4-6-51 Molecular Weight: 154,SOP Supersedes Specifications of 8-|6-40 Approved WON TWD NB SMK DBH ATI. PROPERTY Appearance and Color SPECIFICATION Light yellow crystal line Solid METHOD NUMBER 10,252-41 Crystallizing Point 68.7*0., Min. 10,298-40 Distilling Range* First Drop 100)8 (First Drop to Dryness) Dry Point 252.5*0., Min. 1.5*0., Max. 256.5*0., Max. 10,299-40 SAMPLE FOR ANALYSIS - 1 x 16 oz. W. M. Bottle Notes: Above specifications obver 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. Hlgh_BollerSj_ Crude and Distilled. No specificationsj used at the Krummrlch plant as delivered from Anniston. HONS 046124 T IX. SPECIFICATIONS AND TEST METHODS, oontd. IX - 2 Specif1cations Specificatlons_for_TOMJE_ (Raw Material) PROPERTY SPECIFICATIONS METHOD NUMBER Appearance and Colour Clear, practically colour less liquid, 10 APHA max. 11220-52 Sulphur Trace, max. 119-40 Paraffin % 0.5 max. S-529-3 Barrett add wash No. 2 max. 11222-52 Colour of unquenohed Sulphonohlorlde 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. Allphatlcs % 0.10 max. 11,799-52 "Allphatlos" and "paraffins" are defined as being measured by tests 11799 and S-529-3 respectively, rather than In their usual chemical sense. MOMS 046125 IX. SPECIFICATIONS AMD TBST METHODS, oontd. 8peolficfttlon8_for_H2dratea Llme_(Raw Material) PROPERTY SPECIFICATIONS Appearance and Colour Pine white or slightly grey powder, free from lumps or gritty material. Sulphate, as SOs 0 0.30 max. Mg (0H)a 0 0.50 max. Oa COs 0 Ca (OH), 9.0 max. 92.0 min. IX - 3 Specifi cations METHOD NUMBER 10,188-40 10,189-50 10,192-40 10,193-50 10,191-41 Chlorine_Oas_. No specifications. Snlft gas from the chlorine cells appears to be satisfactory. 8pe_olflcatlons_for_At_tapulgus^ Earjth. (Raw Material) The supplier's specification 1st -- Through 800 mesh soreen 95Jt minimum Volatile matter at 950*C. 150 maximum Krummrlch Plant Method No. 12,304 12,305 Deliveries are not tested except that the Bcreen test is occasion ally siade. Moisture content up to, say, 250*0., with a much lower allowance than 150 would appear to be more In line with the requirements of the process. Cliff Char^ No MCC specifications. HONS 046126 IX. SPECIFICATIONS AND TEST METHODS, eontd. IX - 4 Specifi cation SpeclflpatlonB_forjrin-tetrahenjrl_ (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 + 2*C. Colour White Purity 97ft based on th* reactivity of the material with HC1 Condition Pree from fibres, dirt and paper Inorganic Ohlorldes 0.000080J< 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 Xrummrich plant. Material containing 50 ppm ,of Inorganic chlorides is usable, but earlier deliveries, containing perhaps ten times this amount, were purified at the Krummrlch plant as follows: (D. B. Hosmer and C. Barbre, January 1950). 1. Bach container of tln-tetraphenyl received from the Hooker Company Is transferred to a larger Flberpak 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 0.1}0f( 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 ohlorlde content by the regular analytical procedure. If the pilot batch Is found to contain less than 0.00001ft chlo rides, the T.T.P., Is approved for use. If the pilot batch oontalns more than 0.00001j< chlorides, the T.T.P. is set aside for reprocessing. 5. T.T.P.,which is acceptable for use,Is tested again before It Is added to a plant batoh, by making a second pilot batch from HONS 046127 T IX - 5 Specifi cations IX. SPECIPICATIONS AND TEST METHODS, contd. Specifications for Tln-tetraphenyj, contd. 3. contd. the T.T.P. to be used and a sample of Pyranol No. 1468 from the plant batch. Our procedure for purifying T.T.P. consists of washing a monoohlorbenzene solution of contaminated T.T.P. with city water followed by recovery of the T.T.P. by recrystallizatlon. (See report on Job 116-1740 Refining of T.T.P. by L. A. Hertling. 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 Krummrlch plant to Ruabon In January 1950. Speolf1 cations_for_Qlycl^lphenyl jtether^ Phenoxg gropene oxide C6H5.O.CHg.CH.OCH2 Supplier's specification (Shell) Bpoxy content 980 w/w minimum Colour, Hasen Pt. Co. standard 30 max. Sp. Or. 20/20 *C. Total chlorine as Cl' 1.105 - 1.115 4o ppm max. Note; A batch showing 0.680 total chlorine gave bad results In use. Another stunple showed 0.250, but only 0.75 ppm Inorganic chloride. Another again showed 0.850 total chlorine, but only 1.50 ppm Inorganic chlorides. MONS 046128 ' IX. SPECIFICATIONS AND TOST METHODS, contd. IX - 6 Specif1cation Specifications_of Trlchloro benzene^ (Raw Material) (Pyranol 1478 OEC) Specification H 5228222 PROPERTY SPECIFICATIONS METHOD NUMBER Appearance and Colour Colourless mobile liquid APHA 10 max. 10,105-53 Condition Add number Clear 0.014 max. 10,105-53 10,087-53 Sp.Or. 15.5/15.5*0. Inorganic chlorides 1.460 to 1.477 0.000010(< max. 10,106-53 10,195-40 Viscosity, 100*7. SUS 28 - 32 10,086-40 Dleleotric Strength,25*C,,30 K.V. 10,122-40 Refraotlv Index 25*0. 1.5680 to 1.5715 10,125-40 Distillation range 1st drop 5* 50* SOU 205.0 min. 210.0 min. ' 213.0 min. 215.0 max. 10,108-42 Crystallls.. point 10.0*C. max. 10,101-53 Ha0 0.0075J* max. 10,620-41 Corrosion test 6 hours at 210*C. 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 HONS 046129 Specially processed material to make It suitable for electric grades. See also the finished product specifications for Pyranol 1478, page 35 Section IX, below. T ' ' XX. SPECIFICATIONS AND TEST METHODS, contd. IX - 7 Speoification Specl^f^cations_for_Trlretrachlorobanzene blend (Raw Material) Chemical Formula: Mixture Semple 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*0. 1.510-1.522 Acidity (mg. KOH/g.) Moisture (HsO) 0.014, max. 7J> ppm., max. Refractive Index at 25 *C. 1.5775-1.5790 Free Chlorides 0.10 ppm., max. Crystallising Point -15*C., or lower Last Crystal Point 0*C., max. Dleleotrlc Strength at 25*C. 3D KV, min. Distillation Range (ASTM 0-850, Modified) First Drop 2,10*C., min. 50 by Volume 650 by Volume 215*C., min. 228*C., min. 90j( by Volume 255*C., max. 9556 by Volume 2fi5*C., max. Dry Point - 27S*C., max. Corrosion Test, 6 hrs.at 210*C. with bright aluminum foil Change In weight of A1 0.00 Color APHA 100, max. Condition Clear Acidity (mg. KOH/g.) Free Chlorides Q.014, max. Q.10 ppm., max. Chemical Composition Trlchlorobenzene 58.5$, min. 1,2,3,4 Tetrachlorobenzene 26.0-29.00 1,2,4,5 Tetrachlorobenzene 3.OJg max. Pentachlorobenzene 3.50 max. 10,105-53 10,105-53 10,114-53 10,109-53 10,620-53 10,125-53 10,118-53 12,035-53 12,033-53 11,605-54 10,108-52 10,126-53 12,036-53 general Tests (made only on request) Fire Point Cone to Bolling Pt. 10,123-53 Oeneral Information Dleleetrlo Constant Vis3c0o0sictyycalets1, 0100*F0*.C. " 246,8-32~ 5SUaS M,,0NSs 004466113300 IX. SPECIFICATIONS AND TEST METHODS, contd. XX - 8 Specifi cations Comments on Raw Materials Diphenyl See the comments under "Excess Colour", page 10, Section VII, above. Anniston report 1?1-1077 288? 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 seeitiB unnecessary in view of the use of iron as a catalyst in the chlorlnator. Trlchlorobenzene. The Krummrich plant laboratory, February 26, 1951, gave a limited approval of a French sample of trlchlorobenzene sub mitted by MCL. Copies of the following reports, concerning the suitability of trlchlorobenzene supplies have been sent to MCL, May 7, 1948. "A Method of Determining the Stability of Trichloro benzene" 117-1967, Munch and Ashworth, April 25, 1948 "Trlchlorobenzene 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. MONS 046131 T IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 9 Speclfl cations Comments on Raw Materials, cont<). 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 Krummrlch plant around 1948, had shown poor stability, fnd the cause 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 >47* 355B 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 Prodeleo Co. sample 52/19/1 Mar.52 French TTB sample failed on tests but gave passable Pyroclor. 52/1/9 etc.Nov.5t 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 Barth August 23, 1949 Tln-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 Trl chlorobenzene December 13, 1950 Sample 0-4072 of Diphenyl 0-4073 of Santowax R (distilled hlghbollers) 0-4074 of bottohs of diphenyl stlll(cn|de hlghbollers) sent from Anniston to Ruabon October 13, 1947 Repeated as I-146-C] I-l46-B>- - - January 25, 1949 I-i46-dJ MONS 046132 IX. SPECIFICATIONS AND TEST KETHODS, oontd. IX - 10 Speclficat!ons Comments on Raw Materials, oontd. Trlohlorobenze, oontd. A letter from Mr. Ellenbyrg, July 14, 1947, discusses the use of higher grade benzene tor making TCB, also the quality of bought dichlorobenzene used as raw material. A Krummrloh plant report, September 23, 1947, dlBcusses 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. MONS 046133 IX - 11 Specifi cations IX. SPECIFICATIONS AND TEST MEfTHODS, contd. Specifications for Finished Ooojla - Aroclor 1142 Crude, Conmerclal ISSUED DEC 21 tqcj bemitmen? W*. 9. Kr.m1,,jc|1 p,Ml PRODUCT CODC MO. AROCLOR U4g CRUPB, COHMKRCXAL CMKMICAL FORMULA MlXtUFe -- 1 qt. Bottle (Anniston) Kra.:" g 16 os- W.Mlj. BBoottles Twnr. UNCLASSIPIBD SPECIFICATIONS RawUnt.ljaU frarartt specification Appsaranee and Color Specific Qravitjr 25*/l5-5*C Add Ruabar (ag. KOH/g.) brown to black pily liquid 1.384-1-397 0.7, aax. Method Huober Anniston -- 10,084-53 14-49-5* 14-46-54 10,114-53 10,087-53 RESTRICTED SPECIFICATIONS Add Kuaber of the orude, whloh Is stored In non-lacquered aetal con tainers shall be 0.2 ag. XOH/g. aaz. EXTERNAL SPBCIPICATIONS Rons HONS 046134 IX - 12 Specifi cations IX. SPECIFICATIONS AND TEST METHODS. contd. Specifications for Finished Ooo^a - Aroclor 1148 ISSUED APR 3| 195S nuNmi ifM4***#*-- PftOOMCT COOK I 246 Pdopuer flA mm)m JUUlil 10UCT (fMtdtti mmmm) MSTMOO lOtMTITT tALKI tool _104Q-I0-Qi|/ll-0V0Q ?YM OHOMCAU rOHMUL A Mixture CCML JOB MV 11/18/40____________ UNCLASSIFIED SPECIFICATIONS sarsr.--------------------- -------- UN " IMPU AMAWYN4 Sales _ 2i 16 fli. If. . BaUlfin_ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ Routine Tests Sxmzbs Specification ____ Method Number Appenranoe Color Speclflo Oravlty at 65/15.5*C Oily liquid ,, BroWn to black 1.410-1.420 m 10,084 10,084 10,114 ftaRiptgn -- -- 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 stored In non-laoquered metal con tainers shall be 0.2 mg. KOH/g., nax. con MOMS 046135 By.______ ' PI.* IX - 13 Specifi cations IX. SPECIFICATIONS AMD TEST METHODS, contd. Specifications for Finished Qooda - Aroclor 1154 Crude. Commercial PRODUCT COOK HO* 8*6 MKT HOD IOKNTITY 5oo* 10*0-160-04/11-03/09 AROCLOR 115* CRUDE. COMMERCIAL CHIMICAL fOAMULA MlXtUrO lUPtHMOCt PBCIPICATIONS OP MOU WT. ~~ AMPLC POP ANALYSIS __ 1 8 qt. Bottle (Anniston) frflfow-WtH. Bottlaa UNCLASSIFIED SPECIFICATIONS Property Specification Appearance and Color Speolflc Gravity 65*/15.5*C Acid Number (mg. KOH/g.) Brown to black viscous liquid 1.500-1.510 0.7, max. Method Number Anniston WOK -- 10,084-53 14-49-5* 14-1(6-5* 10,114-53 10,087-53 RESTRICTED SPECIFICATIONS Add Number of the orude, which Is stored In non-lacquered natal con tainers shall be 0.2 mg. KOH/g., max. EXTERNAL SPECIFICATIONS None HONS 04613b XX. ISSUEtfiEC 21 1954 - SlMiCAKBS DEPACTKENT Wm. t. Kiurnnutck Plant By--------------------------------------------------- SPECIFICATIONS AND TEST METHODS, oontd. IX - 14 Specifi cations Specifications for Finished Poods - Aroclor 1160 Crude, Commercial cooeUmoT ^46 _ icemtitv 1 com* 1040-.17Q-04/11-03/09 --amw AROCLOR 1160 CROBB, COMMERCIAL CHEMICAL PORMULA . Mixture 1/6/42 (Anniston) wpmnu PSCIPICATIONE OP 1I1l/1L58/340 BEL 1 pt. can (Anniston) AMPLt won 8 x 16 os. W.M. Bottles "" (WBK)-- - UNCLASSIFIED SPKCZPICATIORS Routine Tests Property Specification Appearance and Color Specific Oravltjr 90*/15.5*C Acid Hunter (ag. KOH/gO own to black scous sticky ss 1.558-1-578 0.7, MX. Method Huaber Anniston TOE -------- 10,084-53 14-49-54 14-46-54 10,114-53 10,087-53 RESTRICTED SPECIFICATIONS Add Huaber of the crude, whloh is stored In non-lacquered Mtal con tainers shall be 0.8 ag. KOH/g., aax- EXTERNAL SPECIFICATIONS Rone HONS Q46131 IX - 15 Specifi cations IX. SPECIFICATIONS AMD TEST MBTjHODS, contd. Specifications for Finished floods - Aroclor ll6g ISSUED API; jj i!J5s ' n' * cPAitruEitr P|.,,, | PRODUCT COM 1 | MOTHOD IDCHT1TV 1-- product rm mm) AROCLOR 1162 PMBUCT lOmdMi mmmj J MljBO COO> 1 1040-l80-04/ll-0,3 ' TTPD TTP CHDMCA4. PDOMUL A Mixture sscvr.-------------------------- 11/18/48 UM 'VSBC^dnST' AMPIC|peD AMAtTMf Sales 2 x 16 ox. W. N. Bottles UNCLASSIFIED SPECIFICATIONS flTBMrftf Appearance Color Speolflo Gravity at 0/15.5*C Add No. (mg. KOH/g.) Vlsoous liquid Brown to black 1-577-1.587 0.7. max. Method Number 10,084 10,084 10,114 10,087 RESTRICTED SPECIFICATIONS Aold Number of the orude whleh Is stored In non-lacquered metal con tainers shall be 0.2 mg. KOH/g., max. MONS 046133 IX. SPECIFICATIONS AND TEST METHODS, oontd. IX - 16 Speolfica tions Specifloatlon_for_Crude_SojLld_ArpolOM (Finished Products) 1166 1169 2565 4065 5060 Method Number Appearance and Colour Acid number Hold Point c. A8TM Softening Point c. Oray to black cryst. powder Orey to blaok cryst. powder Black brittle resin Blaok brittle resin Black brittle resin 10,064-40 -- 145 to 165 -- -- 225 to 250 -- 0.3 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 MQNS 046139 IX - 17 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, oontd. Spedflcations for Finished Poods - Montara 3 and 4 PROOUCT COD! MBTHOD fOBMTITT 846 piwoucfrTfS$ mm) HOWTOS 3, AND 4 ISSUED APR U |g55 JMNMMS OCPAflTMtNr * e. KniMMici, p|,,,, CH KMICAl FORMULA Mixture ivTiiiiisirvnsnf IPl4 FOR AMALYSU [mol *t. juts Sales UNCLASSIFIED SPECIFICATIONS jaoJtlne Tests ProPor-y Appearance Specification Biaok solid Montar 3 6405-003-04-03/09 Montar 4 6405-004-04^03/09 Method Number 11,321 GENERAL INFORMATION Phyjlcal ^Properties (typioal values) Montar 3 Softening Point 180-170'C Acidity Slightly basic Chlorine Content 50-52* CaO 5-10* Ps 0.3-0.6* Montar 4 140-200*C Slightly basic 54-56* 5-10* 0.5-1.0* HONS 046140 IX - 18 Specific cations IX. SPECIFICATIONS AND TEST METHODS, oontd. Specifications for Finished Ooodg - Aroolor 1242 (Pyranol 1499) 27 FWOOUCT Zit COOK NO. CMO MKTHOD IOKNTITY _NAMC AROCLOR 12*g (PYRANOL 1499) CHCMICAL FORMULA WlXtllTt /lUPCNttOKI RKCIFICATIONSOF 8 22/41 FtCIAL MFO, Jfti "* 1040-240-04/11-03/09 ISSUED . MOL. WT. -- W- P|M, 3ampli roe ANALYSIS __ x 5 pt. Aaber Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Specification Method Nuaber K2E Anniston Color Condition APHA 100, MX. Clbar 10,084-53 14-44-54 10,084-53 ... Specific Orsvlty at 25/15*5*0 Aoldlty (ag KOH/g.) Moisture (H*0) Refraotlve Index at 25*0 Free Chlorides Pour Point Dielectric Constant 1000 cycles, 100*C Resistivity at 100'C 1.381-1.392 o.bio, mx. 35 PP.. mx. 1.^245-1.6265 0.10 ppm., nax. -l4*C or loner 4.7-4.9 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 14-36-54 500 VDC and 0.1" gap ~ 500 x 10* oha-oa., In. 11,604-54 14-35-54 Corrosion Test, 6 hrs. at 210*C with bright alualnua foil Change In weight or A1 OM 10,126-53 14-55-54 Color APHA 150, aax. Condition Clear Aoldlty (wg KOH/g.) 0.010, MX. Free Chlorides 0.10 ppa., mx. Oeneral Teats (aade only on request) Dleleotrlc Strength at 25*C 35 K.V In. Sulfates None Fire Point Noie Viscosity at 100*F 8tf2C1T97C2 SOOVOS Distillation Range (ASTM D-20, Coorrfrceccttoed) 10< 3322! }`C, aln. 90* y36g*C, mx. 11,605-53 -- 12,169-54 -- 10,123-53 14-28-54 10,086-5A 14-4-52 10,117-54 14-31-54 (ovep) MOMS 076141 IX - 19 Specif1 cations IX. SPECIFICATIONS AND TEST METHODS, eontd. Specifications for Finished Glooms - Aroclor 1242 (Pyranol 1499) eontd. OEWBRAL INFORMATION Specific Heat at 25*C. Coefficient of Expansion (25 - 65*C.) Fixed Chlorine 0.30 0.00068 eo/ec/*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 MONS 046142 f IX - 20 Specifi cations IX. SPECIFICATIONS AND TEST MEOjHODS, contd. Specifications for Finished Qooflg - Aroolor 1248 ISSUED SEP 9 1954 STAMMS IEMITNHT Wm. <3. Krumtfirieh P|n| PRODUCT Oil C COOK NO. -230 _ NtTHOO IOCNTITV code* 1040-260-04/lf-tr5.............................. _____ Arcs 1.9r 1848 chimical rammcA Mixtureimol. wt. --Dielectric tirade Materiel - 5 x 5 pt. Amber Bottles ...crcTT^Vo, a/2g/i ss?'& -t `3 * 16 01 UNCLASSIFIED SPECIFICATIONS Bautin? Twte CSBiZ Appeerenoe end Color SBgPigqfUw Method Number Colorless to light yel -- 10,084-53 green liquid; APHA 100, Condition Specific Orevlty 65/15.5'C Add Number (mg. KOH/gram) Moisture (H0) Viscosity at 54.4*C (SUS) Clear 10,084-53 1.405-1.415 10,114-53 0.010 mg., max. 10,087-53 35 ppm, max. 10,620-53 73-80 seconds 10,086-53 Pyranol 1498) shall Refractive Index at 25 "C Inorganic (free) Chlorides Pour Point Dleleotrle Constant at 100*C - 1000 epa Resistivity at 100*C, ohm-cm x 10* minimum at 500 V-DC, o.l "Oap" 1.6285-1.6305 O.lo ppm, max. 0*C, max. 4.5-4.7 $00 10,125-53 10,11 8-53 10,,11115! -53 1` 1,60018-54 11,607-54 Oorroalon Stability Teat 10,126-53 (After a sample containing one gi>am of aluminum roll, 0.003" thick, la heated for 6 hours at 210*C with Aroolor, the aluminum must not show oorroalon by ehange of appearance or weight and the sample shall oonform to the following requirements) Corrosion of Aluminum Poll None MONS 046143 10,126-53 (over) T IX - 21 Specif1 Caliwnb IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Ooofe - Aroclor 1248, contd. The Aroolor 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 10,087-53 10,118-53 10.084-55 10.084-53 General Tests (for Dielectric Grade Material only - to be run on request): Sulfates Distilling Range (corrected for stem and barometric pressure): 100 Distilled by weight 900 Distilled by weight None 345*0., min. 385*C., max. 12,169-51 10,117-54 Fire Point, *C., min Dleleotrlo Strength at 25*C. None to Bolling Point 10,123-53 35 KV, min 10,605-53 RESTRICTED SPECIFICATIONS None EXTERNAL SPECIFICATIONS None HONS 046144 IX - 22 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Poods - Aroclor 1254 (Pyranol 1476) ROOUCT COOK NO. 27 246 METMOO IOKNTITY ------- iooV 1040-280-04/11-03/09 -____ AROCLOR 1234 (F7RAN0L 1476) CHEMICAL FORMULA HlltUM lOFIFtSDtt O /tsn /k 1 SPECIFICATIONS OF 9/27/31 **CIAJOLB _ mol. wt. ISSUED FEB 14 1955 STAHIAMS UPUTMiNr s. Kranmrich Plant y----------- ------------------ analyms 3 x 5 Pt. Amber Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Prope^y Specification Method Number m Anniston Color APHA 100, max. 10,084-53 14-44-54 Condition Clear 10,084-53 Specific Gravity at 65/15.5*0 1.495-1-505 10,114-53 lA-49-54 Acidity (ipg KOH/g.) Moisture (HaO) 0.010, wax. 35 Ppm., ax. 10,087-53 14-42-54 10,62c-53 14-53-54 Refractive Index at 25*C Free Chlorides Pour Point 1.6370-1.6390 0.10 ppm., max. 7-12"C 10,125-53 13-34-54 10,118-53 1.4-48-54 10,115-53 14-47-54 Dleleotrlc Constant 1000 cycles, loo'c ~ 4.15-4.35 11,608-54 14-36-54 Resistivity at 100C 500 VDC and 0.1" gap 500 x 10* ohm-em. , min. 11,604-54 14-35-54 Corrosion Test, 6 hrs. at 210* C with bright aluminum foil Change in weight of A1 0.0% 10,126-53 14-55-54 Color APHA 150, max. Condition Clear Acidity (ng KOH/g.) 0.010, max. Pree Chlorides 0.10 ppm., max. Oeneral Tests (made only on reauest) Dielectric Strength at 25*C 35 K.V., min. Sulfates None Fire Point None Viscosity at 210*F 44-48 SUS Distillation Range (ASTM D-20, Corrected) 10S< 366-378`c 50* 372-3o3*C 90% 383-396 C 11,605-53 12,169-54 ... 10,123-53 14-28-54 10,086-54 14-4-52 10,117-54 14-31-54 MONS 046145 (over) f ' XX. SPECIFICATIONS AND TEST METHODS, contd. IX - 23 Speclflcations Specifications for Finished Qocx)b - Aroclor 1254 (Pyranol 1476). contd. QENBRAL INFORMATION Specific Heat at 85*C. Coefficient of Expansion (85-65*0) Fixed Chlorine 0.87 0.00066 cc/cc*C. 5^.5 - 55.5ft EXTERNAL SPECIFICATIONS Gornell-Dublller Resistivity at 100*C. (500 VDC and 0.1" gap) 1500 x 109 ohm - cm 11,604-54 14-35-54 Paint Customers Specific Gravity at 65/15.5*C. 1.495-1.505 Acidity (mg KOH/i.) 0.010, max. 10,114-53 14-49-54 10,087-53 14-42-54 Color APHA 100, max. 10,084-53 14-44-54 Moisture (HaO) 35 ppm., max. 10,620-53 14-53-54 Viscosity at 810*F. 44-48 SUS 10,086-54 14-4-52 Flash Point None 10,183-53 14-28-54 NOTE) Mr. Harden, August 1950, reporting on his visit to the Anniston plant, gave a r\jn of test results on Aroclor 1354. HONS 046146 IX - 24 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Poo^a - Aroolor 1260 (Pyranol 1482) . 27 MKTMOO IOBNT1TV coos* 1040-290-04/11-03/09 SAMI------ AROCLOR 1260 (PTRAIOL 1482), CHBMICAL FORMULA .--JtUrtVHfr_________________________ _ tURBRtKDKt 0/o*T/kl toSCI A 1CAT10 Nt OO.O/Cf/41 t**CIAL y* JAM mm~ ISSUED FEB 14 1955 mmm depaaimihi Wm. 6. Kniimritli PImI By.-.- -......... 3 x 5 Pt. Anber Bottles UNCLASSIFIED SPECIFICATIONS BftWtlM Itltt gfl.g,ing,fltlCT Color Condition Spoolfle Oravlty at 90/15.5*0 Aoldlty (ng KOH/g.) Noloturo IfiaO) Vlseoslty at 210*F ApBA 150. MUt Clear 1.555-1.566 0.014, mx. 35 ppn>> mx. 72-70 SUS Wethod Kuwbar USE 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 10,086-54 14-4-52 Tba Aroolor 1260 Dielectric Orade Haterlal (as Pyranol 1482) shall meet the following addltloMl speolfloatlons: Refrsotlve Index at 25*C 1.6455-1.6470 Free Chlorides Pour Point 0.10 ppn., mx 25f34*C Distillation Range (ASTN D-20, Corrected) 100 by weight . 500 by weight i-404*C 900 by weight i-4ao*c Corrosion Test, 6 hrs. at 210*C with bright alunlnun foil Change In weight of A1 Color Condition Aoldlty Cm KOH/g.) Free Chlorides 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 HONS 046147 (over) IX - 25 Speclfl cations IX. SPECIFICATIONS AND TEST MBlBftDS, contd. Specifications for Finished Poods,- Aroclor 1260 (pyranol 1488) contd. Osneral Tests (made only on request) Dielectric Strength at 50*C. Resistivity at 100*C. 500 VDC and 0.1" gap Fire Point ' Fixed Chlorine 30 K.V min. 500 x 109 ohm-cm.,mln. 350*C., min. 59.H - 60.55* 11.605-53 -- 11.607-53 14-35-5^ 10.123-53 14-28-54 10,088-53 14-13-54 OSNERAL INFORMATION Dielectric Constant 1000 cycles, 100*C. Evaporation Loss after 6 hours at 100*C. Stability test - after 30 days at 100*C. In glass sealed in air. 3.6 - 3.8 11,608-54 14-36-54 0.2*. max. 10,116-53 14-32-54 No liberation of chlprlne or chlorides HONS 04614b [ IX - <tb Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished OoodB| - Aroclor 1262 PMWCT CODB ,* TMOO IODNTITV 246 product fTM* mm) L AROCLOR 1262 p noduct (Ummtt mm) . ISSUED apr j, 5 JJANMm KfHiIHUiT ,, * *'"*">*k Piut | 1040-300-04/11-03 TVPO TVPI CNflMCAL PODMUIA Mixture kmmiBii iPifcior Qian joo no UMPI^ POD ANAkVMI 8/gg/4l__________ 16 an*:------------------------- Ull Sales Bottles_________________ UNCLASSIFIED SPECIFICATIONS Routine Tests ferncter Appearanoe Color Specific Gravity at 90/15.5*C ~ Add No. (mg. KOH/g.) Vlsooslty at 210*F Specification Viscous liquid APHA 150. max. 1.577-1.587 0.014, max. 8$-100 sus Method Number 10,084 10,084 10,114 10,087 10,086 amerA-. iBtsmflan Pour Point (ASTM) Distilling Range Total Chlorine Speclflo Gravity t ooeff (85-130'C) 35-38C 390-425*0 61.5-62.5# 0,00i/*c MONS 046149,, l T IX - 27 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Ooodq - Aroclor 1260 - 10% Toluol l rmiwti i BTrrraw mm/ PROOUC*T m?JLL?60"10*TQLUQL TYR 1WTV ISSUED APR U 1955 STJMaMJ IEPART MINI Vn A *._____ _ . 11/18/40 Mixture -- 5BT5T ------------- Ml AMR^C FOR AMALY** Sales g X 16 02. W, M. Bottles________________________ UNCLASSIFIED SPECIFICATIONS BgMtelW frrcptrty Appearance Color Composition: Aroolor lg60 Toluol - Specification Sjyrupy liquid Amber 90.5-89.5* 9.5-10.5* Method Number 10,08* 10,08* 10,194 OENBRAL INFORMATION fliysloal Properties - Aroclor lgjSo Spaolflo Gravity at 90/15.5*0 Speolflo Gravity t coaff. (75-lj0*c) .Ehyslcal Properties - Toluol Specific Gravity at 15.5/15.5*0 Speolflo Gravity t ooeff. (l5-30*C) Haraloal Properties - 1260 Toluol Mix Speolflo Gravity at *0/15.5*0 1.555-1.566 0.00l/"C 0.870 0.00089/*C MONS 046150 1. *75-1.*95 ISSUED APR ] j joee . S5m"M KMfclfcJr S- P|,,,, IX. SPECIFICATIONS AND TEST MBnfODS. oonttU IX - 26 Specifloatlona Spaolfloatlona for Finished 0ood| - Aroclor 1262 - log Toluol Boutina Teata Proparty Appearance Color Conposltlon: Aroolor 1262 Toluol jmW&maa Syrupy liquid Aabar $0.5-89.50 $.5-10.50 IWtr io,OSS 10,084 10,194 OEKERAL IRPORNATION Phyaloal Propartla - Aroolor_:f.262 Spaolflo Gravity at 90/15-5*0 Spaolflo Gravity t coeff. (85el30*C) Phyaloal Prooertlaa - Toluol Spaolflo Gravity at 15-5/15-5*0 Spaolflo Gravity t ooaff. Ph-valoal Prooartlaa - 1262 Tolpol Mix Spaolflo Oraylty at 40/15,5*0 1.577-1.58? o.ooi/*c O.870 0.00089/*C 1.497-1.516 HONS 046151 T IX - 29 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd, Specifications for Finished Ooodp - Aroclor 1254 - 10* Secondary Butyl Acetate PRODUCT COD> 21)6 PRODUCT fTHtitR MtTHOD IDOMTItV hi- K"mmnck P|,,,, itt.ii eooi 1040-285-04/11-05 TTPt product (dmgtiimmj " " ttpc ' ' ja0gMR; 125*1 - 10* SECONDARY BUTYL ACETATE Mixture Mot. tr. Non *OOM. JDO NO. VM AMUR POP AMALTftO Sales 2 x 16 oe. W. M. Bottles UNCLASSIFIED SPECIFICATIONS AND INFORMATION " SgaUm Proparty Color Conposltlon: ^ Aroclor 1254 Secondary Butyl Aoatat* Qsnaral Inforation gg?gt/a.9f^gn APHA 200, max. 90.0- 91.0* 9.0- 10.0* Method Nunber 12,215-54 12,208-54 Speolflo Gravity of Aroolor 125*) at 65/15.5*0 Speclflo Oravlty of Secondary Butyl Aeetate at 25/15.5*0 Speelflo Gravity Range of Mixture at 29/15>5*C 1.495"1.505 (ohanges 0.00095/*C 0.866 1.425-1.449 HONS 046152 t 1 n. SMcmcATioig Specifics^TM- fQT- TffifT MWIffW eontd. "<* - Kitllltd SQllfl iTOfilora Appearance and Colour 1268 shlta to yellow crystalline ponder Hold Point *C. 135 to 160 1269 shite to grey or light yello* crystalline powder i 285 to 255 1270 shite crystalline powder 285 to 300 1271 prectlcally shite tight fluffy powder IX - 30 Speci fl ea tlcns M65 5*6o clear light yellow brittle resin 1.5 VTA (aax.) clear light yellow brittle realm 2.0 IPA (wax.) Method Ho. 10,084-40 10,127-40 Acid Ho. g. HaOH/g. (us. ) Colour, 5ft la toleana (m.) Moisture % (ax.) 0.05 80 APIA 30 APBA 0.50 0.035 0.05 10,087-40 10,579-41 10,577-41 Melting Point (in), 30* 10,578-41 Foreign Odour Hone to pasa 10,510-40 Total Chlorine % 69.5 to 70.5 59-0 to 60.6 10,088-40 Softening Point *6. 100.0 to 105.5 10,085-40 lacoelty Saybolt Seconds at t. Crystallinity Hr. Harden, August 1950. reporting on his visit to the Anniston plant, gave a run of test results on 5^60 160 to 210 130* 10,086-40 10,089-40 MONS 046153 IX - 31 Specifi cations IX. SPECIFICATIONS AND TEST METHODS, contd. Specifications for Finished Ooody - 60# Aroclor 1260 - 40j& Trlchlorobenzene (Pyranol 1467) ISSUED jan 28 1955 STANDARDS DPA'T' ENT ss?k A-gA6 bbs?v _r=______ __ ;*oLo? ifi52=is>2=ii^ Kr................. ___ 60* AROCLOR 1260 - 40# TRICftLOROBBNZBHB (PYRAHOL 1467) Chemloal Formula -______Mixture ________Mol. Wt. ---------- Supersedes Special Speolfioatlon of 8-27-541 Mfg. Job Samples for ------ Analysis 3 x 5 pt. amber bottles UNCLASSIFIED SPECIFICATIONS Property Specification Method Number Color APHA 150, max. Condition Clear Speolflo Gravity at T.56O-I.568 15-5/15.5*C Acidity (mg KOH/g.) .0X4, max. Moisture (Hto) 0 ppm., max. Refractive Index at 25*C Free Chlorides ~ Dielectric Strength Resistivity at 100'C 500 VDC and O.l" gap Vlsooslty at 100*F !.6137-1.6147 .10 ppm., max. 5 K7, min. 5020-56x S1O0S* ohm-cm., min. Pour Point +32 0, max. Tin Tetraphenyl 6.115-0.135# by wt. Distillation Range: (ASTM D-20, Corrected) Flrat Drop 600*C, max. Below 270*C 40#, max. 90# by wt. 595-415*0 Corrosion Test, 6 hrs. at 210*C with bright aluminum foil Change in weight of A1 0.0# Color APHA 200, max. Condition Clear Aoldlty (mg KOH/g.) 6.014, max. Free Chlorides 5.0 ppm., max. 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 10,117-511 10,126-53 MONS 046154 IX - 32 Specifi cations IX. SPECIFICATIONS AMD TEST METHODS, eontd. Specifications for Finished Poods - 600 Aroclor 1260 - 400 Trlchlorobenzene (Pyranol 1467).'contd. OKNERAI. TESTS (made only on request) Dielectric Constant 1000 cycles, 100*C. Fixed Chlorine Fire Point 3.7-4.0 59.10 i*ln. None to Bolling Point 10,608-54 10,088-53 10,123-53 Aro Formed Combustible Oases 1.00, Max. Electrical Stability (Aged 96 hours at 100'C.oovered Jar, 150 air). Decrease In resistivity 100 max. 10,71110,121-54 Analysis of each 10 ml. fraction of a fractional distillation Chlorlne/llydrogen Ratio* Arc Formed Combustlble\ '1, min. Oases )^*1.$0 max. OKHERAL INFORMATION Dielectric Constant ~ 1000 cyoles, 25*C. 4.0 - 4.3 Inerteen PPO-TCB has the same specification as Pyranol 1467, but it oontalna 0.200 of glyeldyl phenyl ether Instead of 0.1250 of tlntetraphenyl. The fire point Is reported every time for Inerteen PPO-TCB. HONS 046155 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 33 Specifi cations Speciflcatlona for Plnlahed Poods- 45< Aroclor 1260 55< Trl-Tetrachlorobensene Blend (Pyranol 1470) ISSUED jan 1355 PRODUCT coot no. A-246 vNOTMO toiNTiT rr . , STAKBARBS BtPARTMlNT W. G. KiwMirich Pitnk tAI.lt cooc ,l0A5|SQA r ,1,1A0-1,,1-t0o--.3 , - 45* AROCLOR 1260 - 55* TR3|-TKTRACHLOROBBHZBWg BLEW? (PYRANOL 1470) CH1MICAL FO MAUL A Mixture MOL. wt. ~~ IUFIMCOII SPECIFIC ATIONt OF New toteiAL __ NFO. JOO-,____ irra,:8" 3 5 pt. Awbor Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Prppmy Color APHA 150, wax. Condition Clear Specific Gravity at 1.563-1.571 15.5/15;5*C , 4 Acidity (ng KOH/g.) 0.014, wax. Moisture (HcO) 30 ppw., wax. Refractive Index at 25*C 1.6075-1>6085 Tree Chlorides 0.10 ppw., wax. Dielectric Strength at 25*C 35 K.V., nln. Resistivity at 100*C, 500 100 x 10* ohn-ca., Bln. VDC and 0.1n gap Viscosity at 100*F~ 41-45 SUS Pour Point -44*C, aax. Tin Tetraphenyl 0.115-0.135< by wt. Distillation Range: (ASTM D- 20, Corrected) First Drop 210*C, Bln. 550 by volune 240-256'C 55)< by voluae 290-330*C 65J< by voIusm 385-400*C 90* by volune 395-415*0 Corrosion Teat. 6 hrs. at 210*C with bright alcualnun foil Change In weight of A1 0.0# Color APHA 200, aax. Condition . Clear Acidity (sig KOH/g.) 0.014, nax. 'Free Chlorides 5.0 ppn., aax. Method Nusiber 10,084-53 10,084-53 10,114-53 10,087-53 10,620-53 10,126-53 10,118-53 11,605-53 10,604-64 10,086-54 10,115-53 11,533-53 10,117-54 10,126-53 (over) HONS 046156 I XX - 34 Specifi cations IX, SPECIFICATIONS AMD TEST METHODS, contd. Specifications for Finished Poods - 450 Aroclor 1260 550 Trl-Tetrachlorobenzene Blenft (Pyranol 1V70). contd. GENERAL TESTS (made only on request) XM CD 1 ro Dielectric Constant 1000 cyoles, 100*C. 10,608-54 Fixed Chlorine 60.0 - 61.0 10,088-53 Fire Point Hone to Bolling Point 10,123-53 Arc Formed Combustible Oases 1.00 max. Electrloal Stability (Aged 96 hours at 100*C. covered Jar, 15X air) Decrease In Resistivity 100, max. 10,71110,121-54 GENERAL INFORMATION Dleleotrlo Constant 1000 cycles, 25 *C. 4.5 - 4.9 Inerteen PPO - TTCB has the same specification as Pyranol 1470, but it contains 0.200 of glycldyl phenyl ether instead of 0.1250 of tintetraphenyl. mons 046157 IX - 35 Specifi cations IX, SPECIFICATIONS AMP TEST METHODS, contd. Specifications for Finished Qoo^b - Trlchlorobenzene (Pyranol 1478) eeoouCT _ csetHO. J-223.. VSff 8510-000-05-03 TRICHLORQBEHZBKB (PYRANOL 1478) CHEMICAL FORMULA Mixture* ISSUED JAN Z3 1955 ------ SUNBMBS 9EPARTMEMT m Vn. G. Kruinmnch Plant --w--------------------------- - tpcctUiriMcaMtoIDntlor foi//0c7l//mkl RtCIAL . MFO. JOB. :yruvt:" 3 5 Pt. Amber Bottles UNCLASSIFIED SPECIFICATIONS Jute. csucz Specification Color APHA 15. aax. Condition Clear Speclflo Gravity at 1.460-1.477 15.5/15;5*C Aoldlty (ag KOH/g.) Q.014, mi Moisture (h*0) Refractive Index at 25 C Free Chlorides Crystallising Point Dielectric Strength at 25*C op*.. i.5680-1. 5715 Cj.10 ppa. lto'C, aa: 30 K.V. . Distillation Range: (ASTM D850, Modified. (Corrected for Stea and Baroaeurlc Pressure) First Drop 05*0. aln. 5)1 by voluaw , sl0*c. am. 5Op by volusie 313*C. aln. 9Op by voluae 315*C, aln. Corrosion Test. 6 hrs. at 210*C with bright alualnua foil Change In weight of A1 Color q.op APHA 200, Condition ., Clear Aoldlty (ag KOH/g.) Free Chlorides 0.014, aai 9.10 ppa., foihgfl. Hjfflbg 10,105-53 10,105-53 10,114-53 10.109-52 10,620-53 10,125-53 10.110-53 10,107-53 11,605-54 10,126-53 ailBRAL TESTS (aade only on request) Fire Point Fixed Chlorine OENKRAL INFORMATION Dleleotrlo Constant 1000 cyolea, 100*C. Sons to Bolling Point B.5P, aln. 10,12: 10,081 53 3.8 - 4.3 MUNS 046158 Vlsooslty at 100*C. 28 - 32 SUS This Is a mixture.of.the.various Isomers of Trlchlorobenzene plus ` ' ISSUED jan 28 1955 STMMIIJ DEPARTMENT Wm. 0. Krwmmrich PIm* By-- ___ IX. SPECIFICATIONS AND TEST METHODS, oontd. IX - 36 Specif!- C&tionS Speclfi.oatl.ong for Finished Qojxla - 75< Aroclor 1254 25B Trlchlorobenzene (Pyranol 1481) PRODUCT ah/ COOK NO. Arg^P MCTHOO IPKMTITV --> . BALKS a*a aa n n av CODS 1050-120-11-03 75% AROCLOR 125* - 25* TR^CHLORCBEWZEWE (PTRAHOL 1*81) CHIMICAL FORMULA WlXtUTB MOL. WT. -- sotctiUncPAIRTStOKNDstlos J,,toMiaS.AjICoIAL t-- _ SAANMAPLLKY.MSOi_N__ _3 x _5 p.t^ A. m.ber _Bo. t.tl_es -- - -- -- --'' r ' " --........-- UNCLASSIFIED SPECIFICATIONS Routine Teeta Proper Specification Method Number Color Condition Specific Qravlty at 15.5A5;5*C . Aoldlty (mg KDH/g.) Moisture (H8o) Refractive Index at 25*C Free Chlorides Dielectric Constant 1000 cycles, 100*c Resistivity at 100*C, 500 VDC and 0.1" gap - Viscosity at 100*F Pour Point Corrosion Test, 6 hrs. at 210*C with bright alnsilnum foil Change In weight Color Condition ,, Acidity (mg KOH/g.) Free Chlorides APHA 150, max. Clear 1.525-1.535 10,084-53 10,084-53 10,114-53 0.010, max. 35 ppm., max. 1.6205-1.6215 0.10 ppm., max. 4.1-4.6 100 x 10s ohm-cm., min. 10,087-53 10,620-53 10,125-53 10,118-53 10,608-54 10,604-54 70-82 SUS -15*0 or lower 10,086-54 10,115-53 10,126-53 O.Ojt APBA 200, max. Clear 0.010, max. 0.10 ppm., max. (MINERAL TESTS (made only on Pequest) Fire Point Distillation Range: 1st Drop Below 270*0 90X , None to Bolling Point (ASTM D-JO, Corrected) 205*C, min. 259, max. 380-395*0 10,123-! 10,117-! GENERAL INFORMATION MCNS 046159 Fixed Chlorine 55.5#, min. f IX - 57 Specif1* cations IX. SPECIFICATIONS AND TEST METHODS, contd. ------------------------------------------------------* LS.S.^ JlJt< 6 195* tJ*mm OciA,,,m Specifications for Finished Poods - 60$ Aroclor 126^. 6' 40$ Trl chlorobenzene" p/,B( PRODUCT TYRO PYRANOL 1488 PRODUCT (Ctoirtfi *mm) 1 tyro 60$ AROCLOR 1260 - 40$ TRICHLOROBENZENE 6MKMCA4. FORMULA ' PRODUCT CODS A-246 MRTHOD lORNYITY 1050-130-11-01 1 6 u 1 Mixture or 8/27Al rccMk jam m. uoc Sales in|m tor amaltsio |3 X s i>t. Amber Bottles UNCLASSIFIED SPECIFICATIONS Routine Tests Property Specification Method Number Color APHA 150, max. 10,084-53 Condition Specific Oravlty at . Clear 1.560-1.568 10,084-53 10.114-53 15-5/l5;5'C , Aoldlty (m KOH/g. Moisture (H*0) 0.014, max. 35 ppm., max. 10,087-53 10,620-53 Refractive Index at 25"C 1.6137-1.6147 10,125-53 Free Chlorides Dielectric Strength at 25*C 0.10 ppm., max. 35 KV, min. 10,118-53 11,605-53 Resistivity at 100"C 100 x 10 ohm-cm., min. 10,604-54 500 VDC and 0.1" gaf Viscosity at 100"F 52-56 SUS 10,086-54 Pour Point -32 C, max. Distillation Range (ASTM D-20, corrected) 10.115-53 10,117-54 First Drop 200C, min. Below 270`c 40$, max. 90$ by wt. 395-4l5C Corrosion Test, 6 hrs. at 210*ti with bright aluminum foil Change In weight of A1 0.0$ 10,126-53 Color APHA 200, max. Condition Clear Aoldlty (mg. KOH/g.) Free Chlorides 0.014, max. O.l ppm., max. HONS 046160 general Tests (Made only on request) Dleleotrlo Constant 1000 oycles, 100"c Fire Point Fixed Chlorine Arc Formed Combustible Oases 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- IX - 38 Specif1' cations IX. SPECIFICATIONS AND TEST METHODS, oontd. Specifications for Finished Oocfds - 600 Aroclor 1260 400 Trlchlorobenzene, contd. Slectrloal Stability (aged 96 hours at 100*C., covered Jar, 150 air) Decrease In Resistivity 100, max. 10,121 EXTERNAL SPECIFICATIONS Wagner Eleotrlo Company Power Factor (60 at 100*C.) 30, max. Resistivity at 100*C. 500 VDC and .0.1" gap . >000 x 109 ohm-cm itln. 11,608 11,607 General Information Dielectric Constant 1000 Cycles, 25*C. - 4.0 - 4.3 HONS 046161 IX. SPECIFICATIONS AMD TEST METHODS, contd. IX - 39 Specifi cations Finished Products Specl_flcatlons_ror_Murlatl Ac:ld^20_B^._(American2 Commercial^ PROPERTY Appearance and Colour Turbidity Sulphates as h2so4* ASaOs t Assay (HC1) % (max.) (max.) (min.) SPECIFICATION Method No. Colourless to light yfllow liquid 1.5 NPA max. Practically clear 10,070-40 10,071-40 0.01 0.0001 31.45 10,073-40 10,074-40 10,072-40 HONS 046162  ' IX. SPECIFICATIONS AMP TEST METHODS, contd. IX - 40 Specif1cations and Test Methods Finished Product Specifications and Test Methods. Close cooperation with the General Electric Company has cleared up oertaln misunderstandings about the specifications and test methods for eleotrlcal grade materials, a[nd 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 nqt always been changed to suit, and suoh points have now been corrected. There had also been confusion between "corrected" and "uncorreqted" temperatures In the distillation range test. 0. E.'s main plant blend their o*fn Pyranols from MCC Aroclor, and purchased ohlorobenzenes, but MC<) do the blending for G. E.'s Canadian and Meat Coast plants, and for 0 E.'s licensees. 0. E. still receive advance samples of components intended for their use, and samples of finished blends before despatch, though they are ooming 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 a. B. and Vestlnghous* 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 trl-tetrachlorobenzene Is largely replacing the triohlorobenzene. This Is a change originated by O.E. mainly on grounds of cost. Reoently a blend of Aroclor with secondary butyl acetate has come Into use (not for electrical purposes). Mhlle the butylaoetate Is being handled, the same fire precautions are observed as with toluene. The butyl acetate mixtures are rngde In the finished Aroclor vessels CT-0780 and CT-01400. MONS 046163 T IX. SPECIFICATIONS AMP TEST METHODS, oontd. IX - 41 Test Methods 10,006-54 Date: 8-9-54 By: 8MK:H0H Material: OeneRal Method Test: Distilling Range Method No. 10,006-54 WOK Q.M. No. 1 The distillation test method as \>sed by WOK 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: - The flask shall bf the Standard Barrett Benzol Flask of 200-ml. oapaolty. For testing materials boiling above 100*C. the flask will be covered with a layer of asbestos paper, cutting Into the latter a circular bole li Inches In diameter, with the center of the hole coincident with the bottom of the flask, and leaving the glass completely bare. The sldearm Is not covered. Two reotangular silts are afso out In the asbestos covering the neck of the flask, one bn each side of the neck, and the center of each looated 90* from a vertical plane bisecting the sldearm of the flask. The Rectangular slits shall be 5/8" 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 hole* are out In the asbestos covering the bulb of the flask, one on each efde, eaoh 1-1/2" In diameter, and the center of each looated |Ln the center of the side of the flask bulb. These enable observation of the dry point to be made. For testing materials boillhg below, or Including, 100'C., 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 sllghly smaller diameter them the thermometer to be used, and employing aj 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. Oently MONS 046164 IX. SPECIFICATIONS AMD TEST METHODS, contd. IX - 42 Test Methods 10,006-54 Oeneral Method, Distilling Range^ Method No. 10,006-54, oontd. Increase the hole-size with a rat-tall 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. Tor materials boiling below, or Including, 100*0., the tube will be cooled In a trough filled with Ice-water mixture having a temperature of less than 5*0. (measured) throughout the distillation. The trough will be filled so that the entire length of glass In the trough Is covered. Tor materials boiling 100-200*C., 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. Tor materials boiling above 200*C., 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; - The receiver shall be either a standard 100-mi. graduated Pyrex cylinder, op one of the formed type distillation receivers. These are made up specially and are graduated fr.-ir. 0-10 ml. and 90-100 ml. In D.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. Tne formed receivers are used for mateplals normally liquid at room, temperatunas. The standard 100 ml. Pyrex cylinders are used for materials which crystallize at room temperatures or above. B.. Heat Source: - Only the Bunpen 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. MONS 046165 . IX. SPECIFICATIONS AMD TEST I^THODS, contd. IX - 43 Test Methods 10,006-54 Oeneral Method, Distilling Ranpe, 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 UBed, It shhll 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 0.1*C. anjd are capable of being read to 0.05*C. Select, If possible, a thermometer which will Indicate the anticipated range desired tin Its upper two-thirds of graduation, so as to prevent the cork or flask from Interfering with readings. The usual accurate thermometer will be Bcaled 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: -- 'Correction - (No. of degree graduations exposed)(Temp.diff.ln*)(0.00158) 4 The exposed graduations aim read from the top of the cork. The temperature difference Is ithe reading of the thermometer minus the temperature of the stem midway of the exposed mercury oolumn as taken by an auxiliary thermometer. The correction shall be added. 0. Transite Boards: - The tra|nslte board used should be ca. 6" square, 3/1(5" thick and shall have a hole with a diameter corresponding to the following: Materials boiling below 1Q0*C. 100-150*0. 150-2C|0*C. 200-290*0. 250-3C(0*C. above 30jO*C. i" diameter hole 1" diameter hole li" diameter hole 2' ; diameter hole 2j" diameter hole 2i" diameter hole MONS 046166 f . . XX. SPECIFICATIONS AND TEST METHODS, contd. ix-n Test Methods 10,006-5** Oensral Method, Distilling Range. Method Mo. 10,006-54, oontd. The flasks shall not be set 'directly on the transits 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 transits board. This provides a better seal, to prevent the flame from touching the sides of the flask and super heating the vapours. H. Manipulation! - Swab out the condenser with a piece of dry doth 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 sldeam. 2. Seat the cork and thermc|meter, which Is at room temperature. In the neck of the flash, adjusting the thermometer so that the top of the expansion bulb, or the top of the mpper expansion bulb. If there are two. Is level with the bottom of the sldearm of the fljask. Be sure the thermometer b.i'i is In the center of the heck of the flask, and not inclined to the side. 3. Clamp the flask in place on the asbestos sheet, wnl.-h rests on a transits board having the proper hole-size previously designated. _ 4. Connect the flask to the condenser in such a manner that the sldearm 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 oondenser tube without further draining or drying. 6. Plaoe water, loe-and^ater, 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 boll. 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 flapk. MQNS 040167 T . . IX. 3PBCIPI0ATI0H3 AMP TEST METHODS, oontd. IX - 45 Test Methods 10,006-54 general Method, Plstllllng Range, Method No. 10,006-54. oontd. 6. 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 Bidearm 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, whloh allows the thermometer time to reach the proper temperature. 10. Repeat once more, and wfyen this Is accomplished, restore the burner to position 4nd quickly adjust the flame height to that whloh 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 tike condenser tube into the receiver; 1 ml-. 3 ml., 5. 10, 20, 30, 40, 56, 60, 70, 80, 90, and then In 1 ml. Intervals <fn UP 60 the dry point. The dry point temperature Is retd at the Instant the last drop of liquid material is vapourized from the bottom of the flask. At this same tlite, the burner Is turned off. Any distillation showing lets than 96 ml. recovered must be re-run. 12. The temperatures are all recorded at first as uncorrected. The barometer Is read during the distillation procedure. The net correction Incorporating the barometric correction, thermometer correction ^nd stem correction (if required) Is calculated and applied fo the readings to obtain the corrected readings which are reported. HONS 046168 I ' IX. SPECIFICATIONS AMP 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 th following formula: y\Tp - (0.00012 T^) uy In which -<^T_ - Change In boiling point TB_ Normal bolting point In degrees absolute P - Change in pressure In ran. Hg (MacDougall "Thermodynbmlca and Chemistry", p.133.) 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 chart at the front entrance to th* Laboratory. NOTES: After the completion of a distillation test, the flask shall be disconnected from the condenser, and the oondenser 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 meroury has contracted Into the thermometer's expansion chamber. If there Is one. -Never cool a hot thermometer suddenly. The flasks and receivers ar* deemed with the proper reagents emd finally rinsed with distilled water and then alcohol. They are then plaoed In an Oven at 110-150*C. to dry. Before, using, the flasks and receivers are blown with filtered air for several minutes. See specific method for details. MONS 046169 I IX. SPECIFICATIONS AMD TEST MBTHpDS, contd. IX - 47 Test Methods 10,007-53 Date: 3/25-53 Material: Qefieral Method Method No. 10,007-53 By: 3MK,NPA:3MK Test: Color -APHA (Hawn) WOK O.M. No. 2* 1 Introduction: The oolour of WOK Plant products for which the tints (hues) are not very pronounced are estimated by comparison with standards in 50-ml. tall form Messier tubes. The standards are made up In accordance with the directions as given in the APHA Standard Methods of Water Analysis 7th Ed. 1933, pp. 9 as worked out by A. Hazen. Preparation of the APHA Stock Solution: 1, Weigh accurately on an analyltioal balanoe 1.245 gms. potassium ohloroplatlnate (KPtClg), Containing 0.5 gm. Platinum, and 1.000 g. oobaltous chloride (CoC1-.6H20) containing about 0.25 g. Cobalt.. 2. Add both components to one liter flask with 100 ml. C.P. HC1 and distilled water. 3. Make up to one liter with distilled water and mix well. This is the APHA stock solution. It haB a colour APHA - 500. 4, Keep the stook solution in a black painted bottle. NOTE: In the absenoe of a reliable supply of potassium chloroplatinate, chloroplatlnlc acid nuiy be substituted as follows: Dissolve 0.5 g. metallic platinum In aqua regia; remove nitric add by repeated evaporation to dryness after adding an excess of hydrochloric acid. Dissolve this produot together with 1 gram of cobalt/as above directed, chloride HONS 046110 IX. SPECIFICATIONS AND TEST METHODS, oontd. IX - 48 Teat Methods 10,007-53 general Method, Colour APHA (Hazcn), Method No, 10,007-53, oontd. Preparation of the APHA Standard^: 1. To prepare standards, add tt>e proper volume of the stock ~ . solution according to the fallowing chart, to a set of siatched tail-form, 50-ml, Nessler tubes. AFHA Std. ml- StwX Sol'n. APHA Std. ml. Stock Sol 3 0.3 5 0.5 8 0.8 10 1.0 15 1.5 20 2.0 25 ' 2.5 30 40 50 60 80 100 200 3.0 4.0 5.0 6.0 8.0 10.0 20.0 NOTSi For every unit of APHA, 0.1 ml. of the Btock solution Is used. 2. Dilute with distilled water contents of each Nessler tube to the mark. IMPORTANT i The prepared standards should be kept In the closed boxes provided fjor them to prevent excess evaporation and contamination. Procedure for Colour Determinations: 1. Pill a standard 50-ml. tail-form Nessler tube to tlje 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 sanqOe sh^ll be observed and oompared with that of the standard. MONS 046171 IX, SPECIFICATIONS AMD TE3T METHODS. OOntd. IX - 49 Test Methods 10,007-53 Qeneral Method, Colour APHA (Has<jn), Method Mo. 10,007-53, oontd. Procedure for Colour Determination, oontd. 5. Make the observation by looking vertically downward through the tubes upon a white eurfaoe plaoed In suoh a position that non-glaring daylight la reflected through the oolumn of liquid, the regular daylight lamps ban be used for night work. IMPORTANT: Since our products vary In hue, the property sought Is light intensity, rattier 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.P.H.A. 25", or In some oases as "Colour - Hasan 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) J.8 approximately 12" long with 3/4" O.D., graduated at" 50-ml. mirk. HONS 046172 IX. SPECIFICATIONS AMD TEST MBTyODS, oontd Date: 8-19-55 Material: Oenefal Method Byt DKLiSMK Test* 1 Melting Point IX - 50 Test Methods 10,052-51 Method No. 10,052-51 WOK G.M. No. 5 Apparatus: The melting point apparatus used Is the modified Thiel 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 crosBarm 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 Nlohrome ribbon heating elements i> The temperature is controlled with a variable transformer or other suitable voltage controlling device. A lighted magnifier is placed before the bath window to facilitate observation. The melting point tubes are unwaphed Pyrex glass capillary tubes, sealed at one end 1.20 + 0,15 mp O.D. and ,75 + 0-.15 mm . I.D. and oa. 125 mm long. These tubes are to be~stored In dean, and sorew capped bottles to protect them from dust. The thermometers, unless otherwise specified are standardized Instru ments of 35*0. range, graduated it 0.2*C. Increments and capable of being read to 0.05*C. and of the 3-lnch or 75 mm Immersion types. Manipulation t 1. Punch enough of the well minted powdered sample (ca. 200 mesh) Into the open end of the capillary tube so that when the tube Is righted and tapped and/of gently rubbed with a file, the sample falls to the sealed and to a depth of ca. 0.75 Inch. 2. Attach the capillary tube(a) (no more than four) to the proper range thermometer by means ft small rubber bands positioned above the liquid level so that the sample(s) lie adjaoent to the bulb (reservdl 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 MOWS 046173 ' ' IX. SPECIFICATIONS AND TK3T METHODS, eontd. IX - 51 Teat Methoda 10,052-51 general Method, Melting Point, Method Mo. 10,052-51. oontd. 3. oontd. that the thermometer will be properly lmmeraed at the teat temperature and the aample Is olearly visible when viewed through the window with the lighted imagnlfier. 4. Start the motor-driven stirrer. 5. Adjust the voltage control for the heating element so that the temperature rises rapidly urttll It Is within 10-20*C. below the anticipated melting point, and then adjust the rate of heating to 0.1*C. 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 whloh the material leema to pull away from the side of the tube and beoomes mushy. Melting Point; (First Meniscus); The jpolnt at *hleh there is first seen a portion of liquid that Is perfectly cleat extending from wall to wall in the oaplllary. Complete Melting Pointi The point at whloh the last trao*s of solid disappears Into the liquid melt. ' Report the points required to th* nearest 0.1*C, after applying t$e neoessary thermometer correction*. HONS 046174 T IX. SPECIFICATIONS AND TEST METHODS, oontd. IX - 52 Test Methods 10,056-54 Date : 8-12-54 By: SMK, DKL, NPA, OWMsVIJO Material: General Method Method No. 10,056-44 Test: Total Chlorine in WOK O.M. No. 4 Organios - Parr Sodium Peroxlde Bomb Method The ohlorlne 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. Sorub a Parr steel (30 HI) Na<0s Bomb thoroughly with a test tube brush in hot water. Dp not use acid. Rinse thoroughly with distilled water and drir on a hot plate or In an oven at 110*C. 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 ohlorlne equivalent to approximately 40 ml. of 0.1 N AgNOe (0.14 g. Cl) Is used. If the material being tested lp 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 gowdered sugar to give sufficient heat for a good fusion. CAPTIONt In no pass should more than 1.00 g. total organlos be fused In this manner, unless experience has shown It to be safe. PUT OH 8 A P B p Y BLASSES ! 3. Add one scoop (ca. 14 g.) N*0e to the bomb. 4. Stir the mixture In the bonjb with a clean dry stirring rod (1/8-ln x 6-ln.) until thoroughly mixed. Push any lumps of material below the surface of the materl#Q. CAUTION! doggies must be worn during this operation. Inas much as premature Ignition (Of the charge may take plaoe, especially when the humidity is high. It Is Imperative to MONS 0A6175 IX. SPECIFICATIONS AND THST 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 dlreatly above the cup In order to see into it. 5. Wipe the stirring rod thoroughly with a small pleoe (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 ion the bench top to oompaot the fusion mass. DO NOT MIX SHAKING. CAUTION 1 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 (oa. 5 min.). 11. Remove the Jacket and rinse the outside of 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 washlngB lr. the beaker. 14. Cover the beaker with a watch glass and add enough distilled water rapidly (between the Match glass and the beaker) to cover the bomb. 15. Heat slowly to boiling. MQNS 046176  IX. SPECIFICATIONS AMP TEST METHODS, contd. IX - 54 Test Methods 10,056-54 general Method, Total Chlorine in Organics, - Farr Sodium Peroxide Bomb MethodT Method wo. 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 undlssolved fusion mass. If any remains, boll further until dissolved con^letely. 17. Put a stirring rod with a rough end in the beaker to aid in boiling later. Cool to room temperature in rhe water bath. 18. Neutralize the solution with cone. HNOs to litmus paper (ca. 50 ml.). Add 5 ml. egeess. 19. Heat the solution to boiling. 20. Add 50.00 ml. standard 0.1 N AgNOs 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. 23. Add one ml. ferric alum indicator and back titrate with standard 0.1 N NH^CNS to fjlrst appearance of faint pink colouration. Whet, 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 so 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. MONS 046177 IX. SPECIFICATIONS AMD TEST METHODS, contd. IX - 55 Teat Methods 10,056-54 general Method, Total Chlorine lit Organics, - Parr Sodium Peroxide Bomb Method7 Method Mo, 10,056-54, contd. 24. contd. standard 0.1 N AgNOs (Step 20). If the duplicates do not cheok within 0.005 mllllequlvalents, re-run the blank determination. If the blank is greater than 0.025 mini equivalents, use fresh reagents. Calculations: (1) Blank Mllllequlvalents ml. 0.1 M AgNOs x N - ml. 0.1 N MHj, CNS x N (2) * Cl (ml.0.1 N AgNos x N;-(0.1 N NH4CNS x N) - Bik x 0.035457 x 100 Sample Weight The method is precise 6 + 0.05#. Report the results to the nearest O.ljf. HONS 046178 ' IX. SPECIFICATIONS AMD TEST METHODS, eontd. Date! 8-12-54 Material: Qenepal Method Byt LQ, WJOiSMK Test: Odour IX - 56 Test Methods 10,060-54 Method No. 10,060-54 WOK O.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 th analyst and a supervisor or shift leader. If necessary, the oplnloh 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 cabled 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. HONS 046179 XX. SPECIFICATIONS AND TEST METHODS, COntd. IX - 57 Test Methods 10,084-53 Date: 2-11-53 Bys HOH,NPA;SMK Material; Aroolors, Pyranols Method No.10,084-53 Inerteens, and Trl- WOK Dept. No. 246 TetrAchlorobenzane Blend Test: Appearance, Colour and Condition (Turbidity and Residue) I. APPEARANCE (Crude or distilled liquid or solid material); 1. Examine the material In the Cample bottle and describe Its appearance. Report as colourless, light yellow, yellow, tan, light crown, brown or black Mobile liquid, viscous liquid, sticky solid mass, brittle resinous mass, or otherwise If appropriate. II. COLOR (Distilled liquid material); a. If the colour of the sample Is APHA 250 or less proceed as follows 1. Pill a 50-ml. tail-form Nessler tube to the mark. NOTE; If the material 1* of high viscosity, warm up the material, carefully until It. flows readily. 2. Determine the colour of the sample In terms of APKA units by comparing with the APXA standards In similar tubes. Follow General Method No, 2 (Method No. 10,007). 3. Report the colour to the nearest 5 unltB. b If the oolour of the product Is APHA 200 tc 500, proceed as follows: 1. Pour a 50-ml sample Into a 250-ml. Erlonmeyer flask and compare with the APHA standards in similar flasks. o. If the colour of the material Is greater than APHA 500, use the following procedure; MONS 046180 * IX. SPECIFICATIONS AMD TBST METHODS, eonfcd. IX - 58 Tear- Methods 10,084-53 Teat on Appearance, Colour and Conditions of Aroclora, Pyranols, Inerteens, and Trl-Tetrachlorober|sne Blend, Method No, 10,084-54,oontd. e, contd. 1. Pill 1-7/16" x 5" NPA tube half full of sasiple. 2. Place the tube In the A3tyM Union Colorimeter and turn on the light at the back of the Instrument. 3. Determine colour of the sample according to Oeneral Method Mo. 11 (Method No. 11,733) by matching the sample and standard coloured glassed through the observation hole. 4. Match the sample to the dearest half Increment of oolour. The method Is preolse 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 sailple battle. Report the condition (beth 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, S.g., black specks, white lint, rust, etc. HONS 046181 IX. SPECIFICATIONS AMP TOST METHODS, contd. IX - 59 Test Methods 10,085-53 Date: 2-26-53 Material: Aroclors (Solid) and Mcjntars By: AKB,NPA:SMK Test: Softening Point* 1 Method No. 10,085-53 WOK Dept. No. 246 Introduction: The softening point of solid AroClors or Montars (Monsanto Pitch) Is determined according to the "ijlng-and Ball method (ASTM Desig nation: D36 - 26, reapproved in 1(949) for Softening Point of Bituminous Materials" as described m 1949 Book of ASTM Standard, Part 3, p. 10(1. The apparatus Is essentially the same as that illustrated in the ASTM procedure with the exception tr.st two rings end balls are in our assembly instead of one. Procedure: 1. To prepare the sample melt the material under test and stir It thoroughly. CAUTION: 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, out 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 Aroolor which has been provided for this purpose. NOTE: 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 fresnly boiled distilled water. MONS 04610^ f .` IX. SPECIFICATION AND TEST MZTHOpS, contd. IX - 60 Test Methods 10,085-?? Teat for Softening Point of Aroclprs (Solid) and Montars. Method Mo. 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 80*C. range, A6TM Softening Point thermometer Into a support and adjust It so 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 tne temperature of water at 5 (+ P.5)*P. for 15 minutes. 9. Plaoe the balls in the oenter of the upper surface c.f each ring, thus completing the assembly. WOTEs 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 0.5'C. 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. Reoord the temperature at this instant. 12. Correct the temperature reading (Step 11} by applying to it the difference between the observed softening point of the standard Aroclor and the known softening point which la or. the label, thus allowing for the variations in the technique. NOTEs No temperature corrections are made on Mortar "Softening Point" determinations. M0NS 046183 T -* . IX. 8PBCIPICATI0N8 AND TEST METHODS, contd. IX - 61 Teet Methods 10,085-53 Teat for Softening Point of Aroolors (8olld) and Montars. Method Mo. 10.085-53. oontd. 15. Report oorreoted temperature aa the "Softening Point" of the Aroclora. NOTH: Por Montar report the observed temperature. The method la precise to 4 0.5*C. Report the reaulta aa follows: Por Aroolors to the nearest 0.5*0. Por Montara to th nearest 1.0*C. HOTRi Por Aroolors (Montaps) with the Softening Point above 80*C. use a slighly modified technique. The modifications are aa follows: a. Use Dow Coming Pluld Instead of water In a bath.. b. Suspend the ring apparatus off the oenter of the con tainer and plaoe the burner midway between the oenter and the edge of the bleaker away from the rings. o. Use an ASTM High Softening Point Thermometer of a 0* - 360*C. range. MOMS 046184 -I ' IX. SPBCIFICATIONS AND TEST METHODS, contd. IX - 61 Test Methods 10,086-54 Date: 9-13-51* By: SB,DKL,NPA, WWK: WJd Material: Aroolpr, Pyranol, Method No. 10,086-54 Inertfcen, Tri-Tetra Chlorjobensene Test: Viscosity WOK Dept. 246 1. Determine the viscosity according to Oeneral Method No. 25 (Method No. 11,453) Part B - Kinematic Viscosity. 2. For the products listed below use the following temperatures and series number of Ostwald Viscosimeter tubes: Tube SeriesV Product Temperature Number 1242 Aroclor (Distilled) 100*F. (37.8*C.) 200 1248 Aroclor 130 P. (54.4'C.) 200 1254 Aroclor (Q.B. 1476)(Distilled) 210F. (98.9*0.) 100 1260 Aroclor (Q.E. 1482)(Distilled) 210*F. (98.9'C.) 200 1262 Aroclor (Distilled) 210*F. (98.9"c.) 200 1467 and 1488 Pyranol and Inerteen PPO 100'F. (37.8'C.) 100 1470 Pyranol 100F. (37.8'C.) 100 1478 Pyranol (TCB) 100F. (37.8*C.) 50 or 100 1481 Pyranol ~ 100K. (37.8'C.) 200 1 j Calculation: V - Ot Where V - Viscosity in cent!stokes at T*P. C - Tube constant (aocompary|img each tube) at TF., and t efflux time in seconds 4t TF. Determine V to the nearest 0.05 oentlstokes. Convert to Saybolt Universal Seconds using Chart No. B-7781 Report to the nearest C.l S.U.S. HONS 046185 n - 6i 1 r ' ' IX. SPECIFICATIONS AMD TEST METHODS, contd. IX - 62 Teat Methods 10,087-53 Dates 3-11-53 By s nn.f upA: SMK Material: Distilled Aroolors, Method No. 10,087-53 Pyranola, Inerteens and Trl -Tetrachlorobenzene Blend Test: Acid Number (O.B.Acidity) WOK Dept. No.233/246* 1 (For the products "as received" and after the "Corrosion Test"). Procedure: 1. Plaoe 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 300-ml. Erlenmeyer flacks. 2. Neutralize oarefully with the 0.01 N. KOH (to the first definite pink colour). 3. Pour the mixture back and forth between the two flasks several times. If the solution is *tlll neutral, divide It equally between the two flasks, not,repeat steps 2 and 3. 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). NOTE: For Aroolors 1270 and 1271, toluene Is used as the solvent and 300 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 0. E. Specifications) - mg. KOH/gram sample - ml, 0.01 N KOH x 0.56 Sample Weight HONS 046187 1 I ' IX. SPECIFICATIONS AND TEST METHODS, eontd. IX - 63 Test Methods 10,087-53 Test for Acid Number (O.K.Addltp) on Distilled Aroclora, Pyrenols, Inerteena, and Trl-Tetpaehlorobensene Blend,Method 10,067-53 eontd. Calculation, eontd.1 To convert mg. KOH/gram to mgj. NaOH/gram (on request only) mg. NaOIV'gram - (mg. KOfy/gram) x 0.7-15 The method is precise to + 0.002 for sold numbers below 0.01 end to 0.01 In the range of 0.1 to 0.01. Report the reeults 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 seoured from reserve samples of benzene whloh have been analyzed for Depts. 223 and 233. 2. Methanol - Anhydrous. 3. Phenol Red; A saturated solution of phenol sulfonphthaleln (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 Seotlon", Part 2, page 6). HONS 046188 1  IX. SPECIFICATIONS AMD TEST METHODS, oontd. IX - 64 Test Methods 10,088-53 Date: 3-11-53 By: AEB, DKL, NPA:SMK Material: Arocl<rs, Pyranols, Method No. 10,068-53 Inert*ens WOK Dept. No. 246 Test: Total Chlorine (Plxed Chlorine) 1. Determine the total chlorine cdhtent of Aroclors, Pyranols, and Inerteens by the Parr Sodium Peroxide Bomb fusion method according to deneral 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: Chlorine Content Expectancy In a Sample Sample Weight (Use analytical balance) Sugar Required ' (Use analytical balance) Required Ml.0.1 N AgNOs (By burette) 0-30$ 30 - 45$ 45 - 58$ 58 - 66$ 66 - 70$ . 0.5 (+0.0100 < 0.4 (+0.0100 0.3 (+0.0100 g. 0.25(+0.0100 g. 0.22(+0.0100 g. 0.3(+0.01)g. 0.4(+0.01)g. 0.5(40.01)g. 0.6(+0.0l)g. 0.6(+0.01)g. 50.00 ml. 50.00 ml. 50.00 ml. 50.00 ml. 50.00 ml. 3. If the sample Is liquid. In addition to the above reagents use 2 (+ 0.05) g. NatCOs (weigh accurately on a beam balance), to be placed In the bomb before weighing the sample. Calculation: $ Total (Plxed) Chlorine (as $ C|L) - [(ml. AgNOs x Normality - ml. NYLONS x Normality) - Blank*}x " ____________0.035457 x 100 Sample Weight * Blank mllllequlvalents - (ml.-AgNOs x Normality)-(ml.NH^CNS x N) The method Is precise to + 0.2$. Report the result to the nearest 0.1$. HONS 046189 r ' IX. 8FBCIFICATI0N3 AMD TEST METHODS, oontd. IX - 65 Test Methods 10,100-54 Date: 9-3-5^ Material: General Method Method No. 10,100-54 by:OKI>,NPA:WJQ Test: Water - Traoes WOK O.M. No. 7* 1 Introduction: Water may be determined In most opganlo and many inorganic compounds by means of a titration with Karl Fischer (K. F.) Reagent, using either the "Dead Stop" or visual hud point. A._ WD STOP^ Method^ 1. Place 100 to 300 ml. of dpy methanol In the tRation flask - (see note at the end of mjsthod). IMPORTANT: The stopper, trhlch 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 saddle. 2. Start the stirring motor and adjust Its speed so that effective agitation Is achieved without splashing. 3. Snap the toggle switch on the front of the electron-ray Indicator panel to the "Oh" position and allow the Instru ment to warm up-for 3 - 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 |nethanol-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 MONS 046190 IX. SPECIFICATIONS AND TEST ME|TH0DS, contd. IX - 66 Test Methods 10,100-54 Oeneral Method, Water - Traces, Method Mo. 10,100-54, contd. 5. contd K. P. reagent is added. The solvent Is "blanked" when the tube shadows remain fully open (ca. 100 each) for 30 seconds. Refill the burette with the K. P. reagent. 6. Weigh accurately (to three significant figures), by difference, a sample containing 0.03 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 BOlld. 7. Allow the material In the flask to be agitated until all the sample Is In solution. 8. Titrate the solution with K. P. reagent to the end point des cribed In Step 5. Record the volume of K. P. reagent used. Calculation: % H*0 - ml. K.P. it x HaO factor x 100 Sample Weight The method Is precise to + 536 of the water present. Report the result to ?he nearest 5 In the third significant figure. B._ VISUAL_METH0D 1. Place 100 - 300 ml. of dry methanol (see note) In a dry 500 ml. g.g.s. Erlenmeyer flask. 2. Titrate the solvent with K. P. reagent to the visual end point, 1. e. the first change from the yellow to reddish orange that persists for 30 seconds. Refill the burette. MONS 046191 IX. SPECIFICATIONS AMD TEST METHODS, oontd'. IX - 67 Test Methods 10,100-54 Qeneral Method, Water - Traces, Method Mo. 10,100-54. oontd. B. VISUAL METHOD, contd. 3. Weigh accurately (to thrfee significant figures), by differ ence, a sample containing 0.03 - 0.06 grams H*0 Into the flask. 4. Stopper and shake until the sample Is In solution, 5. Titrate the solution with K. F. reagent to the end point described In Step.2. Record the volume of K. F. reagent Used. CALCULATION: % HcO ml, K. F, Reagent x HtO 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. NOTH: Dry benzene or other suitable dry solvents may be used together with methanol In order to render1 some samples soluble. Dry glacial acetlo acid must be added In excess when amines are present in the sample to prevent Interference in the water determination. References: Mltohell, J. and Snlth, D. M. Chemical Analysis, Vol. 5, Aquametry, Interscience Publishers Inc., N. Y. (1948), Frederlokson's Report to Hehner, May 23, 1950. MONS 046192 T ' IX. SPECIFICATIONS AMD TEST METHODS, oontd. XX - 68 Test Methods 10,105-53 Date: 3-25-53 Material: Trlchlorobenzene Method No. 10,105-53 By: AEB,NPA:SMK Test: Appearance, Colour and WOK Dept. No. 233 Turbidity* 1 2 Trlchlorobenzene (TCB) Is usually a clear, colourless to light yellow liquid. Appearance: 1. Examine the sample and desoyibe Its appearance noting any unusual characteristics. Report as a dear, colourless liquid, or otherwise. If appropriate. 2. Observe the sample for residue (visible foreign bodies), such as rust, dark speoks, lint, etc. Report as none, very slight, slight, moderate, or considerable. Describe appearanoe 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 Oeneral Mefehod No. 2 (Method No. 10,007). Report the colour to the nearest 5 units. Turbidity: 1. For Information of the manufacturing supervision, determine the turbidity of TCB. Apply Oeneral Method No. 15, (Method No. 11,788). Report the result to the nearest Oeneral Turbidity Standard Number. MONS 046193 T ' IX. SPECIFICATIONS AMD TEST METHODS, contd. Date 1 3-26-53 Material;. Trlcfilorobenzene Byr CCS, NPA: Teat: Speolflo Oravity SMK 15.5/15.5*0. IX - 69 Teat Methods 10,106-53 Method No. 10,106-53 WOK Dept. No. 2331 1. Determine the speolflo gravity of Trlchlorobentene (TCB) by means of the hydrometer. Apply Oeneral Method No. 15 (Method No. 10,497), with the folioping Modifications: 2. Use a 1.400 - 1.600 range hydrometer. 3. Use a 0 - 110*C. 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 per*C. 6. Add this correction to any reading obtained above 15.5*C. and aubtraot it from readings obtained below 15.5C. 7. Then make the hydrometer correction, if one is necessary. The method is preolse bo + 0.001 unit. Report the Specific Oravity 15.5/15.5"C. to the nearest 0.001 unit. MONS 046194 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 2-13-52 By: DKL:SMK Material: Trlchlorobenzene (Pyhanol 1478) Test: Distillling Range IX - 70 Test Methods 10,108-52 Method No.10,108-52 WOK Dept. No.233-246 Determine the distilling range of the sample according to General Method No. 1 (Method No. 10,006-|50) using a 190 - 230*C. thermometer and a translte board with an opening 2" In diameter. Report the following for 1,2,4 TCB: First Drop 1-96 ml. (95# range) IOC# (First Drop to Dry Point) Dry Point The method Is precise to + 0.1'Ci., however. If appreciable quantities of low or high boiling material (ire present, the precision is of the order of + 0.3.oC. Report the results to the nearest 0.1C. Report the following for Technical TCB or Pyranol 1478: First Drop 5 OX 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 4 0.3C. Report the results to the nearest 0.1'C. HONS 046195 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 71 Teat Methods 10.114-53 Date: 2-11-53 By: BMS.RAC.SS NPAiSMK Material: Aroclors. Pyranols Method No. 10,114-53 Inerteen, and Trl-Tetra- ohlorobensmne Blends Test: Specific Gravity (by WKO Dept. No. 246 Hydrometer)1 1. Determine the specific gravity of Aroclors, Pyranols, Inerteen.;, and Trl-Tetraohlorobenzene Blend according to procedure des cribed In General Method Nq. 13 (Method No. 10,497) with the following modifications: NOTE: The temperaturesat yjhlch the specific gravities of the named products are taken vsjry 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 gilavlty Is to be taken for the par ticular product under test and heat the sample to 10*C. above that temperature. 3. 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 4 paper scale thermometer. 5. Adjust the temperature to the desired point by controlling the steam feed to the Jacket. iContinue stirring until the tempera ture remains constant for bjalf a minute. 6. Note the temperature, quickly withdraw the thermometer and allow the hydrometer to slrjk 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 ireadlng. Usually It Is one scale division below the highest visible part of the scale. HONS 046196 . . IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 72 Teat Methods 10,114-53 Specific Qravlty Teat (by Hydrometer) for Aroclora, Pyranols. Inerteen, and Trl-tetraohlorobenspne Blend, Method No. 10,114-53. 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. Or. Correction Temperature Range Aroolor 1142-1242 0,Q0090/*C. 50 - 105*C. Aroclor 1148-1248 0.Q0090/"C. 50 - 100*C. Aroclor 1154-1254 Aroolor 1160-1260 O.Q0095/*C. 0.Q0100/*C. 55 - 105*C. 75 - 130*C. Aroclor 1162-1262 Pyranol 1478-1470 0.00100/*C. O.QOllO/'C. 85 - 130*C. 11 - 30*C. Pyranol 1488-1467 0.0pll0/*c. 11 - 30*C. Pyranol 1481 O.ODllO/'C. 11 - 30*C. Pyranol 1495 Inerteen F.O.P.O. 0.0P100/lC. 0.00110/^c. -- 11 - 30*C. Trl-Tetraohlorobensene Blend 0.00110/*C. 11 - 30*C. Toluene Mixtures 0.0pl00/*c. Taken at 40*C. The determination is precise to 4, 0,001 unit (1/2 scale division). Reportthe Specific Gravity to the nearest 0.001 unit. HONS 046197 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 2-26-53 By: AEB,NPA:SMK Material: Arocldrs, Pyranols and Inerteens Teat: Loss on Heating at 100*0.* 1 IX - 75 Test Methods 10,116-53 Method No. 10,H$-53 WOK Dept. No. 246 Introduction: This test Is a modification of the test ASTM Designation D6-59T 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 balanoe) 3 ounce 0111 style, flat bottom, seamless ointment box (Jar). NOTE: If It Is necessary to sample the material hot, upon sampling, cool the box and l|e contents to room temperature In a desiccator before making the weight determination. 2. Place the box with the sample In an oven maintained at 100*c. 3. Keep the sample In the oven at the same temperature for 6 hours. 4. Then oool the sample In a deflccator and rewelgh on an analytical balance. Record weight. Calculation: % Loss on Heating (Loss due to volatilization) - /sample wt, (Step 1) - Sample wt. (Step 4)J x 100 Sample weight (Step 1) Report the loss on heating to the nearest O.Oljf. HONS 046198 T IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 2-4-54 By: AEB, LJW NPA,WK:SMK Material: Aroclors, Pyranols, and Inerteens Test: Distilling Range IX - 74 Test Methods 10,117-54 Method No. 10,117-54 WOK Dept. No. 246 Introduction: Distillation tests on Aroclors, Pyranols, and Inerteens are made essentially In accordance with the ASTM procedure D20-30 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, 3-lnch Immersion, Palmer 0-400*C. range thermometer. If a full Immersion thermometer Is used, correction must be made for emergent stem. Condenser: Electrically heated condenser controlled by a varlac to an Internal temperature of 125 1 10*C. The varlac settings, necessary for the desired temperature, for all available condensers are attached to the respective condensers. These settings were established using a varlac that delivered 100 volts at a setting of 100. When varlacs are ohanged, the voltage out-put at a setting of 100 must be checked with an A. C. voltmeter. If thU voltmeter reading Is not within 2 volts of 100, make the- necessary setting correction for the stated varlac settings. The voltage correction is assumed to be linear over the entire range of the varlac. Heat Souroe: Electrical-rheostat control. Material: Point at whlfh condenser heat should be applied: Aroclor 1254 Aroolor 1260 Pyranol 14671. Inerteen PPOJ Pyranol 1470 Pyranol 1481 At beginning At beginning When a pot tamperature of 250*C. Is reached When the distillate volume Is 40 ml. When a pot tamperature of 250*C. is reached. HONS 046199 ' ' IX. SPECIFICATIONS AMP TEST METHODS, contd. IX - 75 Test Methods 10,117-54 Distilling Range of Aroelors, Pyranols, and Inerteens. Method No~ 10,117-54, contd. Procedurei1 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 D20-30. NOTE; The eleotrloal condenser will be a permanent set-up so that no connection will be necessary. 2. Insert a 3-inch Immersion thermometer Into a cork bo 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. 3. 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 fl'ask, to ca. 120. Leave In this positlc|n until exposed meroury column Is within 20*C. of the approximate range of distillation. 5. When the distillation starts, reduoe the rheostat (on the still- pot) 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 peroent" instead of "Percent by weight". For this Pyranol, record the tempera tures as follows: -- MONO 046200 _ IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 76 Test Methods 10,117-54 Distilling Range of Aroclors, Prranols, and Inerteens, Method NoT 10,117-54, conCA. 8. contd. First Drop by volume 55* " " 65* " " 90* " " 9. Make the following thermometer corrections (to be added algebraically to observed temperatures): A. Barometric Pressure; C 0.00012 (760-P) (275 + T ) Where P observed pressure In mm. Tc 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. T temperature of emergent stem at mid-point in *C. MOTE: The use of a full-immersion thermometer Is not recommended because of the difficulties involved in obtaining an acourate measure ment of TD . Report the temperatures (corrected) to the nearest 1C. MOMS 046201 * IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 77 Test Methods 10,118-53 Date: 3-6-53 By: RAC, NPA:SMK Material: Arqclors, Pyranols, Method No. 10,118- Inerteens, and Trl-Tetrachloro- benzene Blend WOK Dept. No. 246 Test: Inorganlc(O.E.Free)Chlorides* 1 (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 3-5 drops of AgNOs and allowing 45 seoonds for full beam to evolve. Absolutely no dust or chloride beam should be present. Note: If beam is present rinse all equipment with dilute HNOs (1:1) and repeat Step 1. 2. When funnels 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 ae steam may cause stopper to fail. 3. Transfer 50-ml. of the sample from the sample bottle at a tempera ture of 95-100*C --into the separatory funnel containing the 50-ml. of boiling distilled water, NOTE: As a precautionary insure 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. CAUTION: Care must be exercised at all times to touoh neither the lower part of the funnel stem nor the ground part of the stopcock. HONS 046202 r * IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 78 Test Methods 10,118-53 Test for Inorganic (Q.B.Free)Chlprldes In Aroclors, Fyranola, Inerteens, and Trl-Tetrachlorobepzene Blend, contd. 5. Allow the layers to separate and drain off the sample Into the seeond 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 3, Note), drain off a few ml, of the sample Into a waste beajker before draining the sample Into the seoond 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 3/4" 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 equil (approx.) portion of chloride-free ether. CAUTION; Teat 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 Show no beam after adding 3-5 drops AgNOs. HONS 046203 * IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 79 Test Methods 10,118-53 Test for Inorganic (O.B.Free)Chlorldes In Aroclors, Pyranols. Inerteen. : and Trl-Tetraohlorob^nzene.Blend, Method No. 107118-53.oontd. 10. Shake the ether-water mixture until the emulsion In the sample disappears and the water lyer la completely beam free before adding AgNOs. If emulsion Is difficult to break, add Bample dropwlse through the ether and then shake. 11. Add 3-5 dropB of 10% AgNOs solution and test for chloride beam for 45 seoonds exactly. If no beam Is present at the end of 45 seconds, report a <0.1 ppm, The very faintest of beams la 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 3-5 drops of AgNOs and comparing at the end of 45 seconds. The method Is preolse 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.O.K. plant laboratory: Standard Chloride Solutionf (See "Procedure Manual for the Servioe Section Dated 2/27/52, Part 3, page 59). The following standards ar$ made up: A primary standard of 100.$ ppm by weighing 0.1648 g. C.P. NaCl Into a ohlorlde-free i-llter volumetric flask. Dilute to the mark with chloride-free distilled water and mix thoroughly. HONS 046204  XX. SPECIFICATIONS AND TEST METHODS, contd. XX - 80 Test Methods 10,118-53 Test for Inorganic (O.E.Free)Chlcjrldea In Aroclors, Pyranols, Inerteena, and Trl-Tetraohlorober|zene Blend, Method No,10,118-55,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, Standardsi For every 0.1 ppm of a standard, dilute 10 ml. of the 10.0 ppm Standard to one liter and mix well. MOTE; A 0.1 ppm beam Is considered the very faintest beam perceptible to tM 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 la easily visible (too strong) discard the solutions and make new standards. lOjt Silver nitrate Solution; Weigh on a beam balanoe 20 (+ 0.05) g. C. P. AgNOs Into a chloridefree darlt bottle. Add 20 ml. C. P. HNOa (chloride free). Dilute to 200 ml. with water. MOTE; All solutions should be freshly prepared every two weeks and stored In glass-stoppered Pyrex bottles. Source of light; Use the 2-battery Penllte flashlight, having a 3-4 mm light and aperture. New batteries (use "Eveready" No. 915, size AA; "Burgess" No. Z, chrome protected; or oompbrable batteries)must be used fre quently In order to perceive hearts properly. MONS 046205 I ' ' IX. SPECIFICATIONS AND TEST METHODS, oontd. Date: 7-23-54 By: AEB, NPA, QWM:VJQ Material: Aroclcfrs, Pyranols and Ityerteens Test: Electrical Stability (or Aging Test)* 1 IX - 81 Test Methods 10,121-54 Method No. 10,121-54 WOK Dept. No. 246 Introduction: Xleotrloal stability Is determined by measuring the resistivity of Aroolors, Pyranols, or Inerteens lat 100*0. before and after exposing the same sample to air at 100*0. for 96 hours. PROCEDURE: 1. Allow the Electrode assembly (Method No. 11,607) containing the produot under test, from the Initial resistivity determination to remain in the oven at 100*0. for 96 hours. NOTE: Por 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 regelated at 100*0. 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 lad to outer electrode) and measure the resistivity 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. MONS 046206 T IX. SPECIFICATIONS AND TEST METHODS, oontd. IX - 171 Test Methods 12,036-53 Test for Composition by D3.stlllttti.on of Trl-Tetraehlorobenzene Blend, Method Mo. 12,036-53, oontd. Calculation: 0 Trichlorobenzene - (wt. of Tracjt. 1 + 4 wt. Tract. 2) x 100 Sanyple Height (step 2) Total Tetrachlorobenzene (gins) - iiwt. of Tract. 3 + } wt. Tract. 2 (Tetra) + J Tract. 4) 0 1,2,3,4-Tetra Isomer - total wt. of Tetra x percent 1,2,3,4 isomer --------------,_________________ jgfeE-g) _ Sample Weight (Step 2) 0 1,2,4,5-Tetra Isomer - total wt. of Tetra x percent 1,2,4,5 isomer t (step 8) Sample Weight (Step 2) Example: A 700 g. sanqple of the (blend has been distilled. Total Tetra Traction weight Was 70 g. It was found from Dwg. A-5538 that Isomers were present In the following percentages: 1,2,3,4-lsomer 90.0ft and 1,2,4,5-isomer 10.00. Then the percent of each Isomer in the blend will be as follows: 0 1,2,3,4-Tetra Isomer 70 x 90 1- 9.00 by wt. of sanqple (Step 2) 700 0 1,2,4,5-Tetra Isomer 70 x 10 ' 1.00 by wt. of sample (Step 2) 700 0 High Boilers (as Fentaohlorobettzene) - fwt, of Tract. 5 + 4 wt. of Tractj 4+4 Residue (Step 9)J x 100 Sample Weight (Step 2) HONS 046305 [ ' IX. SPECIFICATIONS AMD TEST METHpDS, contd. IX - 172 Test Methods 12,036-53 Teat for Composition by Distillation of Trl-Tetrachlorobenzene Blend. Method Mo. 12,036-53, contd. ft loss on distillation - [wt. of Sample (Step 2) - (combined wt. of Fraots. + wt. Residue ____________________________________.___ ________ (Step 9)3 x 100 Sample Wei(pit (Step 2) Report all components, residue, and loss on distillation to the nearest 0.1J< Apparatusi 1 - A 2-liter, B 24/40 heck, round bottom distilling flask (pot). 1 - A four foot stainless .steel packed column. 1 - An Insulated and electrically heated distilling head with a thermometer (B 110/30 Joint). 1 - A 500-ml. "glass-col" heating mantle. 3 - Varlacs (to regulate Individual heating of the distilling head, the column, and !the pot). 1 - A 0* - 360*0. range, 9 10/30, thermometer (corrected)for the distilling head. 5 - Receivers! ' 2 x 500-ml. and 3 x 250-ml. Erlenmejyer flasks. MONS 046306 IX. SPECIFICATIONS AND TEST METHODS, oontd. IX -'174 Test Methods 12,169-54 Date: 9/23/54 By:VWK:WJO Material: Aroclors, Pyranols and Inerteens Test: Sulfates Method No. 12,169-54 WOK Dept. No. 246 -------------- ----------------------------------------------- 1------------------------------------------------------------------------ 3oope: This method of test Is intended for the qualitative determination ol Inorganic sulfates, by precipitation with BaCla, In chlorin ated biphenyl products. Apparatus;* 1 250-ml. separatory funnel, ). x 6 Inch test tube, and a burette or 5-ml. plpet. Reagents: 10J( (by wt.) aqueous Bade Solution and C.P. HC1 Procedure: 1. Place 75 ml. of distilled wpter In a clean 250-ml, separatory funnel. 2. Heat the water to boiling bp means of a Bunsen flame. 3. Add 100 ml. of sample to th> funnel. 4. Shake contents of the funnel thoroughly, venting occasionally through the stopcock, for c#. 1 minute. 5. Allow the layers to separatp. 6. Discard the lower or sample layer. 7. Drain 15 ml. of the water lpyer Into a clean 1x6 inch teat tube. 8. Heat to boiling over a Bunssn flame. 9. Add 5 drops of C.P. cone. HC1, then slowly add 5 ml. of Bade solution from a burette or pipette, and shake to mix. 10. A white precipitate reveals the presenoe of sulfates. Report as follows: If no precipitate Is noted immediately report as "None", if a precipitate f.s noted report as "present". Reference: ASTM-D117-53T and D0p8-49. MONS 046308 . ' IX. SPECIFICATIONS AMD TEST METHODS, oontd. - IX - 175 Test Methods 12,808-54 Dste: 8/20/54 Material: Aroclor-jButylacetate Mixtures By:OWM:WJQ Test: Composition Method No. 12,208-54 WOK Dept. No. 246 1. Ascertain that the lot number of the Aroolor 1254 (used In the mixture) Is recorded on the label of the sample bottle. 2. Determine the Specific Oravlty of the mixture at 29*C./15.5*0. using General Method No. 13 (Method No. 10,497) with the fSlowing modifications: a. DO NOT heat the material to greater than 35*C. b. Use a 1.400 to 1.600 range hydrometer. c. Use a 0* to 50*C. range paper scale thermometer. 3. Apply the hydrometer correction (if any). 4. Prom ohart A 7780 on the following page, IX - 176, determine If the oorrected 3p. Or. of the Mix at 29*/15.5*C. falls within the shaded portion of the ohart at a point corresponding to the Speolflc Oravlty* at 65*/15.5*C. of Aroclor 1254 used In the blend. Report only the Specific Oravltyiof the mixture at 29/15.5*0. and lndloate whether or not the material[passes the specification limits. (Whether it falls within the shaded area on the ohart or not.) Remarks: The diagonal lines on the cljiart Indicate the Butylacetate present In the mix at the corresponding coordinates of specific gravity of the mix at 29*/l3.5*C. and the specific gravity of the Aroclor 1254 at 65*/15.5*C. This Specific. Oravlty may be Obtained from the analytical ticket file. HONS 046309 l  IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 177 Test Methods 12,213-54 12,214-54 Date: 8/24/54 By: TT:WJO Material: 1254:Aroclor Butyl Acetate Mixture Test: Refraet^tieIndex Method No.12,213-54 WOK Dept. No. 246 -----------------------------------------------------------------------f------------------------------------------------------------------------------ 1. Determine the Refractive Inddx of the mixture at 25*C. using Oeneral Method No. 28 (Method No. 11,784). NOTEi Do net leave the sample bdttle unstoppered, slnoe possible volatilization of the butyl acetate would change the composition of the mixture. Date: 8/24/54 By: TT:WJ(J Material: 1251* Afoolor Butyl Acetat^ Mixtures Test: % Butyl Acetate Method No. 12,214-54 WQK Dept. No. 246 1. Tare on an analytical balano* a clean dry aluminum dish. Record the weight. 2. Weigh acourately on an analytical balance i 5 [+ 0.1000) g. of the mixture Into the dish an* record weight of dish and sample. 3. Subtraot weight of Step 1 fr{>m weight in Step 2. (This Is the weight of the sample). 4. Place the dish Into a 108 + t*C. oven for 3 hours. 5. Cool In a desiccator. 6. Reweigh and record weight ofi dish and contents. Caloulatlon: jf Butyl Acetate - Original samplb and dish (Step 2)-Final Wt.(Ste^)x 100 ^ Sample Weight (Step 3) Report to the nearest 0.l. HONS 046311 IX. SPECIFICATIONS AMP TEST [OPS, c-ontd IX - 178 Test Methods 12,215-54 12,220-54 Oates 8/24/54 Material: 1254|Aroclor Butyl Acetate Mixtures By:TTiWJO Test: 'Color ----------------------------- ------------- -- -- Method No.12,215-54 WOK Dept. No. 246 -- ------------ ------- -- 1. Determine the color of the mixture In terms of APHA units. Refer to Oeneral Method No. 2 (Method No. 10,007). Date: 9/29/54 By: WWKWJQ Material: Aroclors, PyranolB, Inerteens Test: Light transmission* 1 2 3 Method No. 12,220-54 WOK Dept. No. 246 Scope: The purpose of this method Is to measure the percent light trans mission through 246 product^ as compared to dlBtllled water which has a transmission of 1000. Equipment: 1. The Fisher Electrophotonjeter. 2. An empty plastic filter holder (no filter). 3. Round, 23-ml., matched absorption cells. Procedure: 1. Determine the Light Transmission according to General Method No. 18 (Method No. 10,723-51) 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 0 Light Transmission on the "B" scale. Report results to the nearest 0,10. MQNS 046312 Reference: National Cash Register Co.'s Method 2021.55 (9/24/52). I ' IX. SPECIFICATIONS AND TEST METHODS, eontd. ix - 179 Test Methods 12,306-55 Date: 3A/55 Material: Aro^lors and Pyranols Method No. 12,306-55 By: WWK:WJ0 Test: Parll^* # 10 Viscosity WOK Dept. No. 246 ------------------------------------------------------------- 1----------------------------------------------------- ----------------- IMPORTANT: Conduct this test in a room having a temperature of 23-27*0. 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-np.. graduate and your finger under the oup. 2. Center a clean, dry 50-ml. graduate under 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 th|e sample to 25 + 0.5*C. 5. Close the orifice by placing your finger under the cup. 6. Pour the sample Into the oupj, 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 por concave. 7. Remove your finger and measure the time, by stopwatch, it takes for exactly 50 ml. of Bample[ 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: Oelsman's memo to Schwartz, 8/5/54. This method is the same as that (ised by Du Pont at their plant In Pariin. New Jersey. HONS 046313 1 IX - 180 Test Methods IX. SPECIFICATIONS AND TEST METljODS, oontd. Mote on the Inorganic Chlorides jest. See also the comments on pages 13 - 17 in Section VII, above. It will be noted that the chlorides content Is expressed In parts ohlorlne ion per million. The specification limit of 0.1 parts ohloride per million calls for vary special control technique, especially in a plant area whereIthe 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 Krummrlch 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, Ootober 24, 1950,with drawings, and suggestions for improve ment arising out of Krummrlch plant experience. Mr. Harden reported on visit to the Krummrlch 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, 1953, Mr. Beauregard told us that 0. E. in America no longer had "wide open" liaison with B. T. K. in England, but that MCL would, nevertheless, be in order in giving details of the 0. 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 MCC 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 1953, deals with Bakelite Co.'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. BarLre suggested washing the condenser back into the sample,and using a Lumetron or similar MOMS 046314 IX - 182 Test Methods IX. SPECIFICATIONS AND TEST [OPS, contd. Mote on the Inorganic Chlorides Test, oontd. presumably because the tintetraphenyl, performing Its function of removing HC1 formed during the heating, has formed SnCl* or SnClj,. The 0. E. specification allows up to 5 ppm, but Mr. Kueter reports that MCC figures rarely exceed 2 ppm. While allowing the relaxation to 5 ppm, 0. E. still Insist thgt the separate main component Bhall show not more than 0.1 ppm. The same 5 ppm tolerance has be*n extended to "Inerteens" which contain glycidyl phenylether In place of tintetraphenyl, but experience Indi cates that this tolerance is urujwcesary. Presumably the glycidyl phenyl pther removes the HC1 by the opening of the alkene oxide ring: ------ d^-h -- + HC1 - / -- CC1-- C^--OH giving products which volatilise away, or at le^ st do not react with the silver nitrate. The very dilute sodium chloride standards required for the Inorganic chlorides test require very speoial care In handling, otherwise they Increase In strength by picking up HC1 etc. from the air. In practice they are not actually made up, (accept 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). 1 Occasionally a high "chlorides after heating" figure on Inerteen has been traced to contamination wil(h traces of tintetraphenyl picked up in the plant. MCL Research Progress report 1152 NR 52/103/3, September 195deals with a method of determining tin tetraphenyl In Pyranols. Report 1151 52/1/12, May 1955. phows that Aroclor 1262 is stable at 160*C. In air. Report 1151, NR 53/97/1, July 1^53, showed some darkening of 1262 in steel at 300C. In air. MQNS 046315 l IX - 185 Test Methods IX. SPECIFICATIONS AND TEST iOPS, contd. Note on Electrical Test Methodsj A great deal of work has been dcjne 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 assemblirjg data for various publications. See the list of reports-at the e|nd of Section VII, above. Finished Product Samples sent tcj MCL. A oomplete set of samples of Ardclors 1142 to 5460 was requested April 1, 1947, also of all Montajrs, and of Pyranols 1467, 1488, 1496, with analytical data on each sample. (Aroclors 1169, and 1269 had been abandoned In favour of 1170 and 1270). MCC report 171-1088, 2881, May 1953, oompares Anniston and Krummrlch plant 1260. Competitor's Products. Dr. Jenkins, February 20, 1952, Reported.a statement to the effect that Bayer's equivalent of Aroclpr 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 plasticlserp for PVC. Aroclors were better for this purpose. Certain MCL research reports undbr job 1151, discuss competitive products, for example, 1151 DF 5P/86/5, March 1954, on French ''Pyralene". MQNS 046310 X. PLANT OPERATING DATA X- 1 Operating Data Plant Capacity In 1946 the working rates of[the different units at the Krummrlch Aroclor plant were as set out) In the table below. MOWS 04631V l Operation TDK AROCLOR PBODOCTIOW liquid Aroelors 1242-1248-1254-1260-1262 Solid Aroelors 1268-1269-1270-1271 Time-hours ' Equivalent .Lbs .of fin. Aroclor Time-hours Equivalent Uts. of Pin. Aroclor Melting Charge CHB and DHB . Pumping Diphenyl 0.40* Charging Chlorlnator Chlorination 0.35 1242-13.00 1248-15.00 1254-19.00 1260-20.00 1262-21.00 Transfer to aerating tk Aerating 0.35 4.00 # DramUdg to drums Distillation - 12.W? -6100 5700 ** 7200 7800 8500 -- Drawing to drums Blending A treating Pilling containers Filtering Pilling containers Dropping to storage Cleaning press 4.00 e 5.00 e 2.00* 3.00* 0.40'* 0.35 1268-23.00' 1269-24.00 1270-26.00 1271-28.00 7000 7200 6800 - I268~ib oo 1269-24.00 1270-24.00 1271-24.00 1268- 3.00 8.00* 6.004 Resinous Aroelors __ 2565-4465-5460 Time-hours Equivalent Uts.of Pin. Aroclor .' 12.00* 0.40* 1.25 2565-24.00 4465-24.00 5460-28.00 6500 6900 6200 0.35 4.00 i fifi-1^65 i "................. 5460-16.00 it 4.00 e 5.00 e 4.004" 3.00* * These operations are performed at such tines during the operating cycle that no production tine - la lost. MQNS 046318 # . When the production rate is low, the aerating operation la perfomed similarly to (*) without any lost tine In production. However, during a high rate of production the chlorination and distil lation operations are frequently held up until tile aeration operation la completed, which results In a loss ofproduction. gjw* - v0 i 6 Approximately one and one-half chlorlnator batches make one still charge. J jj. > e Homallythese chargesare equivalent to approximately three chlorlnator batches. 4 ** The figures on page VI-5 would Indicate a figure of about 6300 lb. for finished 1248. . X. PLANT OPERATING DATA, coijltd. X-2 Operating Data Plant Capacity, contd. See also page 5 of Seotlon V|, above, for chlorination time cycles. With four main chlorlnators,I one air-blowing tank, and two vacuum stills, 9,624,188 lbs. of liquid Aroclors, and 121,812 lbs. of solids were made in 19^. The best month up to 19^7 had produced over 1 million pounds. The oapaclty In 1954 (five main fhlorlnators, two alr-blowlng vessels and two vacuum stills) was given1as l million pounds per month. In 1954 the capacity for Aroclors was given as li 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 19^7 as follows: Pump Aroolor to mlker Pump TCB to ml|cer Mix and sample Adjust composition and mix again Add tln-tetraphenyp., mix and sample Clean the press 8.0 hours 5.0 hours 2.5 hours 3.0 hours 2.0 hours 0.5 hours 21.0 hours * This period is required fojr each separate adjustment found necessary The elapsed time from startlhg a batch to finishing and loading was about 5 to 6 days. It tpok 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 chlorinators, and another looks aftjer 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, abcive, for the labour needed for the distillation of solid Aroclcjrs. One man, per shift, borrowed from the Aroclor department, does practically all the Pyranol jwork at the Krummrlch plant. HONS 046319 I X. PLANT OPERATING! DATA, oontd. X-3 Operating Data YleldB 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 way; the "consumption" of chlorine Is [reckoned baok from the "make" of Aroclors. ; other In the Krummrlch plant Arocljor 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 theoretloal yield flgurais 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 "Theoretloal" requirements of ohlorlne and Diphenyl are calculated from the month1s 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. Type Aroolor DKTRHMIUATItlN OF THKOBRTTnAI. YTRI.DS Pounds Aroclor Produced Diphenyl ReqSifed q.s Factor Faotor To Finish 1148 + 1248 32,685 1154 + 1254 187,407 1260 97,147 1262M U)l,800 1271 3,000 0.9$64 1.0*172 1.2(i 1.2:70 1.4)90 0.5304 0.4669 0.4038 0.3930 0.3200 31,587 205,623 116,576 2,209 4,257 TOTAL 322,039 (2000-1800)1 ~__|0O (1262 360,252 Diphenyl Required To Finish 17,336 87,500 39,228 707 960 145,731 (1) Use 9<# of total 1262 4ilx produced, or 1800#. * From page X-13. HONS 046320 . X. PLANT OPERATING DATA, oontfd. X-4 Operating Data Yields, contd. "Standard Conversion Factors"(also have been established as set out in the table on page X s 12b, in this case the crude and the distilled products being ijaken separately. Eaoh month the "Standard" requirements of chlorine and diphenyl are calculated back from the month's production figure for eaoh crude and distilled Aroolor separately (except that each crude Aroclor is bracketed with Its corresponding distilled Afoclor where one is made, and the factor used for each pair is a weighted average of the single factors) as set out in the example bel*w. DETERMINATION OF STANDARD YIELDS Type Aroclor 1148 + 1248 1154 + 1254 1260 1262M 1271 Produced 32,685 187,407 97,147 (1) 1,800 3,000 Clal Factor f 1.040: 1.181 1.295$ 1.3225 1.499^ Diphenyl Factor 0.5687 0.5011 0.4375 0.4210 0.3438 Cla Required 33,992 221,328 125,825 2,381 4,499 TOTAL 322,039 388,025 2000 - 1800 - 200 (12621mix) 322,239 gross ^otal production Diphenyl Required 18,588 93,910 42,502 758 1,931 156,789 1) Use 900 of total 1262 mi* produced or 1800 #. 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 compare* with half the chlorine received, (1. e. used). MQNS 046321 X. PLANT OPERATING DATA, oontd,. X-5 Operating Data yields, contd. Dept. 246 Monthly Ii^/entory 8 A.M. - June 1, 1946 CHLORINE: Theory 3IH52-- x 100 - 89,45' taken as 100# Standard Actual x 100 - 83.05 83.05 89.45 x 100 = 92.85# WM * ix 100 -85,26 83.26 8^45 x 100 - 93.08# DIPHENYL; Theory Standard Actual 322 239 145 731 x 100 - 221.12. taken as 100# 322 239 156 789 f x 100 - 205.42 205.42 221.12 92.95# 322 239 156 289 * x 100 - 206.18. 206.18 221.12 93.2^# 100# HCli Short tons 100# HC1 produced Short tons Cl* received \* 2 _ 88.34 . 00 " 9^.99 93.00 iofrsrx 100" 90,45 * Note 102,04 x 100 These figures are the totals jfrom page X-3. ft These figures are the totals from page X-4. * These figures are the totals from page X-7. HONS 046322 X. PLANT OPBRATINQ DATA, contd;. x-6 Operating Data The oomblned departmental monthly return covering all Aroclors on one statement Is then eet 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 Py|ranol department have no special features. HONS 046323 l X. PLANT OPERATINO DATA, contq. X -7 Operating Data MONTHLY [STOCK REPORT CRUDE MATERIALS USED May 11, 1946 1. No. of Material 2. Stook Plrst of Month 3. Reoelved 4. Total -------- cTT |C1 Oas Liauld Cl. Tolu Lime Att. Di ene Earth phenyl #231 4232 1 Total #529 6,400# ' 0# : 6,4oq# 400# m. mTwrr 4,000 (2) (3) 382,373 4,000 yf97WF 0 386,373 400 #565A #608 #611 (5) 1000# 225# 159,178# 2450 (**) 3450 200 (4) 425 100,000 (6) 259,178 5. Stock Last of Month 6. Difference _ 2,348 (1) 380,025 '0 4,000 2,348 384,025 200 200 1500 300 102,889' 1950 125 156,289 7. Required to 2,000 Pinlsh Previous Month - 8. Difference 378,025 \0 4,000 2,000 382,025 0 200 150 0 0 1800 125 156,289 9. Required to + 5,000 Pinlsh This Month 10. Total 383,025 :0 4,000 5,000 387,025 0 200 100 0 0 1900 125 156,289 11. Credit _ 12. Net Used 383,025 4#ooo 387,025 200 1900 125 156,289 13. Per 100 lbs. Finished Qoods 118,86 4.24 > 120.10 10.00 0.59 0.04 48.50 REMARKS: (1) In scrubber llqudr. (2) Prom Dept. 231(Cnlorlne) (3) Prom Dept. 232(Chlorine) (4) From Dept. 363(Warehouse) (5) 1178# In scrubber liquor. (6) Purchased. HONS 046324 X. PLANT OPERATING DATA, contd. MONTHLY jiTOCK REPORT X -8 Operating Data May 1946 High Boll >r Labor Crude Dlstl .led Operating Repair Packing Total 1. No. of Material 618 619 2. Stock First of Month 3. Received + 0# 0 0#: 0 0_ 0 1150 120 00 130 1400 4. Total 0 5. Stock Last Month 6. Difference _0 0 0 1 0 0 1150 120 130 1400 0000 1150 120 130 1400 7. Required to _ Finish Previous Month 8. Difference 0 0 9. Required to 0 finish this + month 10. Total 0 0 o! o' 6' 200 0 0 200 950 120 130 1200 150 0 0 150 noo 120 130 1350 11. Credit 12. Net Used 13. Per 100 Lbs. Finished Ooods 0 0' { 1i 1100 0.34 120 0.04 00 130 1350 0.04 0.42 MQNS 046325 X. PLANT OPERATING DATA, contjd. X*9 Operating Data MONTHLY STOCK REPORT PRODUCTION, Dept. 246 " ' 1 I. 1 " 1. Products or By-Products Aroclor Montar #4 2. Stock Last of Month , Delivered to Packing ,7' Room or shipped 4. Del'd to 363 Storage (1) 31,479# 560,385 250,131 0# 0 0 May 1946 By-Product 100* HC1 0 tons 0 0 5. Delivered to Departments 6. Total 2, 5, 4 and 5 7. Rec'd from Packing Room (2) 52,109 894,104 l f i0 0 0 0 (3) 93.00 93.00 0 8. Rec'd from 363 Storage 9. Rec'd from Departments 10* Stook first of Month 11. Total 7, 8, 9 and 10 12. Produced 15. Per Cwt. Main Product 540,000 10 (1) 31,865 ' 571,865 322,239 r 0 0 0 0 0 0 (4)4.66 0 4.66 88.34 (1) Process Goods stook (2) To Dept. A-246 (Pyranol Debt.) 48,509# To Dept. D-246 (Permasan Eppt.) 3,600 Total ............................................... 52,109# (3) To Dept.D-2l8 (Muriatic Acid Dept.)90.00 tons To Dept. 217 (Chlorsulphuric Acid Dfpt.) 3.00 tons 95.00 tons (4) Prom Dept. C-248, (Santolu|>e) HONS 046326 X. PLANT OPERATING DATA, contc|. MONTHLY STOCK REPORT YIELDS, DEPARTMENT 246 X - 10 Operating Data May 1946 Products or By-Products Yield on ohlorlne Yield last Month Standard Yield Theoretical Yield Yield on 611 Yield Last Month Standard Yield Theoretical Yield Yield on Yield Last Month Standard Yield Theoretical Yield Arocjors ' HC1 83.J26 81.93 1 83.05 \ 89.45 206 .|l8 208.^7 205.152 221.12 (93.086) (92.806) (92.856) (100.006) (93.2456) (92.986) (92.956) (100.006 93.00 92.79 92.56 102.84 (90.436) (90.226) (90.006) (100,006) Aroclors Produced 1148 200# 1248 32,485 1154 300 1254 187,107 1260 37,147 1262M 2,000 1271 3,000 Total.......... 322,239 MONS 046327 X. PLANT OPERATING DATA, contd, X - 10a Operating Data SUMMARY OF MONTHLY REPORTS Dept. 246 Production: Products Month) ------- March 1. Aroclors : -1 quid 2. Aroclor Si lid 3. Aroclor Tt tal 4. Muriatic .old 100* 400,000# 0 400,000 April 350,000# 0 350,000 May 319,239# 3,000 322,239 Yields: Raw Materials 1. Diphenyl 2. Chlorine 3. Chlorine (HC1) Inventory: Raw Materials 1. Diphenyl 2. Chlorine Process Ooods 1. Aroclor 12pn 2. Aroclor 12460 3. Aroclor 12V1 Finished Ooods 1. Aroolor 2. Muriatic Apld 94.20* 94.50 91.00 93.28* 93.43 90.75 93.24* 93.08 90.43 150,000# 5,000 3,000# 7,500 10,000 0 0 220,000# 2,000 25,500# 0 0 0 0 102,889# 2,348 0 31,479# 0 0 0 Liquidation Reserve: Raw Materials 1. Diphenyl 2. Chlorine 5.000# 2,000 1,000# 3,000 3,000# 1,000 Prooess Ooods 1. Aroclor 2. Murlatio Ajsid 0 0 2,631# 00 0 Goods of "No Value 1. 2. 3. -- ___ -- -- -- -- COMMENTS: (See attaohed report for detailed remarks.) Signed: Brief Comments Inserted. Operating Supt.________________ MQNS 046328 X. PLANT OPERATINO DATA, conttf. Rate of Operation OPERATION REPORT Dpt. 246 jtay 1946 X - 10b Operating Data Year Month Liquid Aroclors Solid Aroclor Total Aroolors 100j( by Produce HC1 1945 1 12 6 to date 5,400,000# 1,500,000# 300,000 50,000 5,700,000 t,550,000 2,200.0 tons I 500.0 tons 946 April May June Est. 300,000# 319,239# 500,000# 0 3,000 50,000 300,000 322,239 550,000 90.0 tons 88.34 t . 180.0 t. Brief Comments On: (1) Number of days operated. (2) Reason for rate of production. (3) Reason for estimated! rate of production. Crude Materials and Yields Crude Katerlals/cwt Aroolors Year Month #231 #232 Total Chlorine #611 #618 #6179 #565A #529/owt 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 0.03 0.03 0.34 0.02 0.42 1 5i to date- ' 117.0 3.5 120.5 47.0 0.2 0 0.6 11.0 0.03 0.02 0.32 0.02 0.39 9 April 117.5 4.2 121.7 46.9 0.2 0 0.4 11.5 0.03 0.02 0.38 0.02 0.45 4 May nos 1.24 120.10 48.50 0 0 0.59 10.00 0.04 0.04 0.34 0.04 0.42 MONS 046329 X, PLANT OPERATING DATA-, contf. OPERATION REPORT. Dept. 246, M^y 1946, contd. Peroent Yields (Theory 100)6) Year Month Aroclor on Chlorine on #611 100)6 by-prod.HCl on Chlorine 1945 12 93.24)6 92.17 94.38 1 5 bo date f 92174)6 94^46 951.51 9 April 92.80)6 92.98 97.61 4 May 93.08)6 93.24 90.43 X - 10c Operating Data Brief Comments on Yield. Servloe Charges/cwt. Aroclor Year 1945 Months 12 Steam M lbs. 0.22 KWH Power 2.14 KWH Lights 1.00 KWH Total 3.14 Comp.Air M Cu.Ft. 3.01 City Water Cu.Ft. 0.11 Well Water M dale. 26.00 Fuel Oas M Cu.Ft. 0.05 1 5 bo date 6.42 5.09 1.40 4.49 0.14 21.90 0.42 0.56 Stocks Stocks as of Warehouse Department H-46 532l000 571l000 1,103^000 9 April 0.33 2.40 1.27 3.67 0.10 24.50 0.44 0.03 4 ..way, 0.33 2.47 1.55 4.02 0.11 24.00 0.47 0.42 6-1 -46 100, 000 250,131 350,131 Brief comments on present stoc)c and amount shipped. HONS 046330 ! X. PUNT OPERATINO DATA, contp. OPERATION REPORT, Dept. 246, foy 1946, oontd. Operation* 1 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;. MOWS 046331 l ! X. PLANT OPERATINO DATA, cont<(. X - IX Operating Data The month's yield figure for th<e Aroclors, as explained above, is a composite one, depending to soi|ble extent on the ratios between the different Aroclors made. With this restriction, the following data give the results for 1946 at tl^i Krummrich plant. Raw Materials Consumption lbs, per 100 lbs, of Aroclor Chlorine Diphenyl Lime Attapulgus Earth 182.22 47.22 0.44 0.02 also Toluene 11.67 (lbs.per 100 lbs. 1262 M blend) Crude and distilled high boilers are not Included because the amounts used were small. Krummrlch plant standards, for 1954 were, per 100 lbs. Aroclor produced: -- 1248 : .254 1260 1262 mixture mixture 1260 1262 Diphenyl consumed 56.50 4$.75 59.54 58.02 41.78 45.45 Chlorine consumed 105.25 Ilf-56 117.21 119.47 151.29 Lime consumed Attapulgus Earth consumed Toluene consumed Muriatic Acid produced O.50 0150 0.46 0.46 0.50 0,04 $.04 0.04 0.04 0.04 46.55 5$. 75 1.40 US 1.40 US gallons gallons 52.02 55.60 58.94 ----- L ,, 128.80 0.50 0.04 - 57.82 MONS 046332 l  X. PLANT OPERATING DATA, oontja. X - 12 Operating Data Krummrlch plant standards, peri 100 lbs. Aroclor, for 1954, contd. 925,OOOlfcs./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 57,500 Compr.Air,ou.ft. 925>000 1,250,000 City water, U.S.gal. 278>000 576,000 Plant water,cu.ft. 46,500>000 62,500,000 The report "Process Description, for Aroclor, Dept. 246", Schwartlng and Schwartz, March 15, 1955, gives more recent figures. Yields of Aroclor (as $ of the ''theoretical figures on page x - 13). On chlorine consumed 95.(4$ (95.25) On diphenyl consumed 92.17$ (94.75) The figures In brackets'^ are for the first 9 months of 1955. / Yield of HC1 On chlorine consumed 94.(8$ (90.12) of the "theoretical" figure. MOWS 046333 * X. PLANT OPERATING DATA, contd. X - 12a Operating Data Services Consumed Per 100 lba. Aroclor (Production at the rate of 836,100 lbs, of solid Aroclor plus 6,753,775 lbs, of liquid Aroclor 7,p89,875 lbs. of Aroclor per year.) Steam 1000 lbs. ---------------------Power KWH-------------------------------- k Lighting KWH............................-->Comp. Air, 1000 cu.rt. -------City water, ou.ft. --------------Well water, 1000 U.S. galls Fuel gas, 1000 cu.ft. ---------- Labour, man hours-----------------i- See also the report "Process Description for Aroclor, Dept. 246" Sehwarting and Schwartz, March lj>, 1955, pagesl7- for more recent figures. MDNS 0A6334 X. PLANT OPERATINQ DATA, co^ltd. X - 12b Operating Data Department 246 Standard Conversion Factors (1946) AROCLOR 1142 1148 1154 1160 1162 1168 1169 1170 1171 1242 1248 1254 1260 1262 1262M 1268 1269 1270 1271 2565 4065 4465 5060 5460 CHLORINE 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 DIPHENYL [ 0.6074 0.547* 0.482} 0.4160 O.4O60 0.3625 0.3450 0.348J ' 0.638$ 0.5765 0.5089 0.4385 0.4267 0.3909 0.4060 0.4100 0.2866 0.2400 O.2667 -- -- DISTILLED CHUDE HIGH BOILER HIOH BOILER 100* HC1 0.3829 0.4J41 0.4945 0.5404 0.5485 0.5991 0.6271 0.6586 0.6880 0.4030 0.4568 0.5192 O.5689 0.5809 1.164 0.180 0.418 0.510 0.095 0.5827 0.7614 0.7999 0.8350 0.5886 0.5776 0.6415 0.5645 0.6883 A somewhat different set of! faotors, in use In 1953, Is given on the following pages X - 73 and 14. Molten diphenyl stocks (at |bout 90C.) taken at 8 lbs. per U.S. gallon. MONS 046335 X. PLANT OPBRATINO DATA, oontd. 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 5060-5^60 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 HIOH BOILER 0.437 These faotors were still In use In 1953. Aroclors are not pure compounds^ but are mixtures of two or more compounds, consequently, they d<* not have a definite composition, and for this reasoiy'cannot calculate the theoretical factors. See the Note by E. Mather marked * on the following page. HONS 046336 X. PLANT OPERATING DATA, contjd. DEPARTMENT 246 - CONVERSION fACTORS, oontd. X - ltt Operating Data * Note by B. Mather - May 1955j Theoretically 100 lbs. of; an Aroclor containing should give a chlorine conversion factor of of chlorine 00 and a diphenyl or high biller conversion factor of Thus % chlorine In Aroclor 42 48 54 60 62 65 68 69 70 71 Conversion factor chlorine diphenyl or high boiler 0.^4 0.9(6 0.591 533 l.C|B 475 1.2b 4l6 1.24 1.3b 397 368 l.3p 1.36 1.4)o 339 330 320 I.fc -------------- 1 310 By this test the Krummrich pla^it figures for chlorine for 4065 seems to be Impossibly low, and so <3p the "diphenyl" figures for 4065 and 2565 (taken as representing total hydrocarbon used). HONS 046337 X. PLANT OPBRATINO DATA, contd. X 15 Operating Data (on theorjf) at the Krummrlch plant In 1954 for Pyranola, etc, were:i 1467 Pyqanols 1470 1 1481 f 1488 Inerteens PPO PPO-TTCB mix TCB standard actual 195? 99.OX 99.85 -' 99.OX 98.51 99.OX 99.85 99.OX 99.85 TTCB standard _ 98.0; . ,, 98.0X actual 195? - 98.8} - - - 98.81 Aroolor 1254 std - 99.0: - - _ actual 195? 99.0 i - - .. Aroclor 1260 std, 99.0 aotual 195? 99.0 99.0; 99.01 99.0 99.0 " 99.0 99.0 99.0 99.0 ' 1' 1 1, l| The consumption figures were Aroclor 1254 Aroolor 1260 TCB TTCB Tip Attapulgus earth Olyeldyl ph. ether 60.60 45.4^ 75.75 - 40.40 - 0.126 -' 55.5$ 0.12$ 25.25 - 0.02 0.02| 0.02 - -1 " 1 ----------- 1-- 60.60 40.40 0.02 - 60.60 40.40 - 0.02 0.220 45.45 - 55.56 - 0.02 0.220 HONS 046338 T > X. PLANT OPERATING DATA, oontfd. X 16 Operating Data Labour, man hours Steam, lbs. Electricity, KWH Comp. air. cu.ft. City water Plant water PYRANOLS 936,000 lbs./month 1,250,000 lbs./month 813 278,000 813 374,000 3,700 5,000 Figures for earlier years are |glven by Lyles, Soffranko It Hiller, March 24, 1947. pages 51-58. Krummrlch Plant records fjor Aroclors up to 1946 are summarised on the following pages HONS 0<t6339 Dept 246 October 2, 1947 PRODCCTTOH REPORT SOJWART 7EAELT Tear 1936 1937 493^ 1939 1940 1941 1942 1943 1944 1945 1946 Gaseous chlorine #231 Lbs. #/c*t Liquid chlorine #232 Lbs. #/cwt Total Cl Lbs. #/cwt Initial production on September 4, 1937 18150 4002818 2881774 3526099 6447110 7387766 9415836 10665174 11338840 8264386 2.18 51.32 115.17 114.67 126.27 126.94 116.94 116,57 116,38 116.57 119.20 1067944 1386016 406623 191650 227748 1034700 693980 531680 338400 128,00 3.53 -0 13.22 3.556 3.913 12.86 7.585 5.457 4.773 4/05 1086094 . 130.18 5388834 54.85 3932722 6628760 7615514 ijy .CTO 127.99 161.83 166.07 10450536 11359154 11870520 8602786 129.84 124,16 121.84 122.82 123.25 Note; The cwts are 100 lb. Diphenyl #611 Lbs. #/cwt 361095 1735788 173472 1322914 2235099 2546476 3517935 4243212 4580000 3307987 43.28 44.21 42.90 43.02 43.78 43.75 43.71 46.37 47.01 47.22 Ct- |> p P rt r>e a r in g HONS 046340 O perating Data ITS 00 Dept . 246 Year 1936 1937 1938 1939 19*0 1941 19*2 1943 1944 19*5 1946 #11*8 Lbs. #/cwt 4550 0 0 0 0 0 0 0 0 0 0 .545 - - - CHCTDE MATERIALS October 7, 19*7 #1160 Lbs.#/cwt 10432 0 0 0 0 0 0 0 0 0 0 125.03 - - Hydrated Line #565A Lbs. #/cwt 7050 62445 45002 19700 57225 53780 30600 23650 38600 41850 - 1.591 1.799 .641 1.121 .924 .378 .258 .396 .445 - Crude High Boiler #618 Lbs. #/cwt 5400 26500 9000 17187 6000 0 0 0 1800 2000 - .647 .675 .360 -559 .118 - - .193 .180 - HONS 0^63<1 Dept, 246 Year 1936 1937 1938 1939 1940 1941 1942 1943 1944 1945 1946 Distilled High Boiler #619 Lbs. #/cwt CRUDE MATERIALS Toluene Lbs. #529 #/cwt 9609 19000 47890 54579 13200 0 0 0 1800 2000 1.152 .484 1.914 1.775 0.259 .193 .180 0 3427 1684 2554 4587 5176 475 2039 19446 7534 _ .087 .067 .083 .0898 .089 .006 .223 19.96 11.67 October 7, 1947 Attapulgus Earth #608 Lbs. #/cwt 0 1115 1050 1231 4952 6257 2725 3125 2285 1770 .0283 .042 .040 .097 .108 .034 .034 .024 .024 Vra>t i> e r a t n g HONS 046342 Dept, 2*6 Year 1936 1937 1938 1939 19*0^ 19*1 19*2 19*3 19** 19*5 19*6 On Diphenyl #511 #/cwt *Th 231.05 226.18 833.09 232.*5 228-.** 228.55 228.80 215.6* 212.73 98.19 97.97 98.13 9* .91 9* .08 93.06 96.16 9*. 12 92.17 95.60 YIELDS on Chlorine #232 #/cwt <Th 78.12 72.86 73.71 78.19 7TV02 76.*2 77.02 80.** 81.73 81.27 91.02 91.10 91.2* 91.28 91.90 92.83 92.08 93.2* 92.80 October 7, 19*7 HC1 - 100* #/cwt * Th 112.89 98.55 89.10 93.02 111.55 106.6* 10*.5* 102.20 10*.68 109.77 95.83 86.6* 90.*5 102.57 103.70 101.65 99.38 101.79 9*. 38 9*.*6 O p e ra tin g HONS 0*63*3 Dept. 246 October 7, 19*7 Year 1936 1937 1938 1939 19* 19*1 19*2 19*3 19** 19*5 19*6 Operating Hours Hrs./cwt 7016 25115 1*36* 12200 20206 17*** 18698 20660 22529 18077 .8*1 .6*0 .57* .397 39T .300 .232 .226 .231 .235 .31 Han Hours Repair Hours Hrs./cwt Packing Hours Hrs./cwt 937 1799 22*0 2778 21*0 .016 .022 .02* .029 .025 .0* Total Training Hours Hrs./cwt Hours 7016 25115 1*36* 12200 20206" 18381 20*97 22900 25307 18817 .8*1 .6*0 .57* .397 739T .327 .255 .250 .260 .260 .39 Added March 1*. 1951: See Dr. H. B. Dysons notes on his 1950 trip to St. Louis for some notes on the manning of the department. O perating Data HONS 046344 Dept, 2*6 Tear 1936 1937 1938 t95 19*0 19*1 19*2 19*3 19** 19*5 19*6 Total Llauld Aroclor 795*018 962*196 6753755 3*0*795 Prod. & Yields Total Solid Aroclor 9*97* 121812 336110 22962* Total Liquid and Solid 83*32* 3926076 2502161 3075121 5105790 581986* 80*8992 91*99*0 97*3008 7089875 363**15 October 7, 19*7 By Prod. HC1 Tons 209.60 1176.76 778.90 '9T*.5* 1501.90 1785.39 2*99.18 2778.63 2839.8* 2120.60 1092.81 eratin g MONS 0*6345 Dept 2*6 Year 1936 1937 1938 1939 19*5 19*1 19*2 19*3 19** 19*5 19*6 1119 0 20 0 0 0 0 0 0 0 0 0 11*2 8700 38975 13*36 11792 *885 1537 0 25 723 *67 0 11*8 1**00 1000 0 0 15*3 0 0 *85 0 0 0 October 7, 19*7 AHOCLOBS PRODUCED 115* 6000 0 5900 2360 8000 0 0 125 500 0 0 1160 0 0 0 0 72 627 0 0 0 0 0 1162 0 1*58 1**5 9065 19 1*65 0 0 500 0 0 1168 0 25* 100 500 8*96 2*089 0 0 0 0 0 1169 0 50 80 0 0 0 0 0 0 0 0 O perating Data HONS 046346 Dept, 246 Year 1936 1937 1938 1939 1940 1941 1942 1943 1944 1945 19*6 1170 0 15 55 0 0 0 0 0 0 0 1171 0 0 0 0 0 0 0 0 0 0 AROCLORS PRODUCED 1242 28593 43044 49735 22250 30431 0 12166 48875 74784 31556 1248 13000 53362 25363 59313 83013 79779 100242 95820 38784 100914 October 7, 1947 1254 231584 1299822 639878 801662 1329442 361063 0 4124646 6082785 3609168 1260 264400 1196468 842622 1542462 2910460 4202815 7727813 4333299 2776688 2858994 O perating D a ta HQNS 046347 Dept. 246 Year 1936 1937 1938 1939 1940 1941 1942 1943 1944 1945 1946 1262 39640 165223 122074 88216 140678 230056 121506 453236 464012 100444 October 7, 1947 ABOCLOBS PRODOCED 1262 Mix 0 10068 5000 0 41232 40594 4457 16524 182120 52222 1268 34514 51419 47375 50C 8490 24089 0 0 0 0 1262 78124 668517 179887 0 0 0 0 0 0 0 1270 0 0 240124 97990 179891 319959 94974 0 20657 330310 HONS 046348 1271 0 0 0 0 0 0 0 0 0 5800 1271 Is expected to reach 86.000 lb/yr, (textile use). O perating Data Dept. 246 Year 1936 1937 1938 1939 1940 1941 1942 1943 1944 1945 1946 2565 57429 240124 97990 179891 0 0 0 0 20657 0 AJtOCLORS PRODUCED 4065 0 0 40 200 0 0 0 0 0 0 4465 57710 115589 148919 193196 74451 0 0 0 0 0 5o6o 0 500 484 0 0 0 0 0 0 0 October 7, 1947 5460 0 14048 43460 38850 0 0 0 0 0 0 300 0 0 0 1 0 0 0 0 0 0 301 0 0 0 66 0 0 0 0 0 0 O p e ra tin g Data HONS 046349 X. PLANT OPERATING DATA, oontd. X - 27 Operating Data Cost sheets for the KrummrJjch plant Aroolors Dept, were sent to London, February 1946, and those for Anniston were sent February 24, 1947. Anniston cost sheets for crude Aroolors, distilled Aroclora, 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 totsj1 cost figures being arbitrarily split between the separate Aroolc:irs on the basis of previous experience. (Copies sent to London, see letter Mather to Durgln, May 24, 1945). Copies of the Anniston raon't}hly returns for August 1947, as given in the report of Havercroft arid Mather Just mentioned, come a little nearer to giving ooneumptioins of materials for eaoh Aroolor; the services oonsumed 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. HONS 046350 X - 28 Operating Data MONSANTO CMCMtCAt COMPANY [ COOT NCPONT Muer tlvMl 9r*r*4+" _ *** __ tMWIMMTM. . 0t T<p .... . . lua M un ------- 0 00marnWPW"- _ ............... * ""TT---------------------------------------- MMIN *T 1 1MM** VML* * . ---------------- --------- nwMM arf-- H -- |- ir- u_t. ,Z~tl . MM>fT *'*--*** Mfaaiai ss rss'Tzi" c^zr*" A n a.^- a t, hs+ r* 0**ra i*/ .j r* fa -* *j '-a. *> m "il *<* t**: ii. % * 1 ! %5 /T 1 1 *** IIWICIM toTTt --I*/ - c Y* '".f S.1 * 4-C '.-*4 I*.*--- Q 1 r*f I l'U4Ut VmaCi fruf Ml WM MTU wiaiiin aarrc kim 1 VMM miM WMMMMIIM ssr mSZSTU.. ' - o.ff If <1**t * t * , fa tr **7l; ia * --. __ j*t' t, - 5 in i iff a* M* - n r a la 0 174 v lit * 'f < #* W to** /" 9'fji ` - >* If j H f-JwT | wt ta f U | 1 V*M ** >.-* *H U **/ H IW i -1 or <? / <* ' 0/ <w * a k * f/l *r . *9 If* e-* ** M ' Of *-/ ** law './ .'w a / *04wf 1 0 1W # HW1 it* ?i a*V lM O' > -f fi Hu oof ki '*/ 'f -Of H 1a II it AT / " r t o M * to - lit f) >7 f1 -17" f> f> *7 ' - V ) w /** a** M 0*7 301 . O'J it A. 00* 0)7 XT </* '3* <0P P-/ 300 ' /* JoT 0`i O0 JOT '30f V?* f Iff <*T <t 34 0Wt ' aa ea* <** .Ml 00* -0>,* \1*p on* oak -- MW MIW MM MMMUWK M | MWaMMINM *a M* IMNMMM rm m r*~o c~ a Mm fc> [ 1*4wr -mi f of 1 Ml J* , a ->i k W * l** 10* if ** ) MV fcf mil *r 6Mo # -N IT/ 0O0 001 rtlf w.| 0^0 0if -0/7 . _u*fc----------1M. 0070 If 0M# `0)7 #/ Ml* I* ! ' * >- ____ tM_____ 0 0_________________________ -*!!_____ ' i v r fw MONS 046351 X - 29 Operating Data HONS 046352 noimrw ciuical company 4- wilirf ----------jssru. ------ "MM.M,________ Mm-* .jssns. -as- IWu*jOu *04 . 5 *4* YYi **Y It X - 30 Operating Data x~ -- *-- --- TllIMT --rrur1 -----------7C" ' * ISO ' '<* Unntn NMM *M -ssssra. ktVUiu U* 1 *ssr- [ ww mSSSSRSw -- !-*- *>*" t* wan * -aj til / MS ** at* wit mm fcwmiiw MNMM AM WM MM * - J > 9*4 0 * /* f -* i* 4* J* Jt> M 1 if * 9 9* *4 40 ? 04 T1 a Olf ' 90/ rXf Mt *3 ~"t 7 *1 Y7 *>* *5 XM m -1 - ' y 7J f* - t> - ) .t i t ib u X* - * *f He w 4 f T* 0>X MT . 33 *0 0t 3*1 <*>> J*J >b f H* HU 3fl 0>0 '35.4 J0 jot 'i r yit r yet yj * ur *'4 --? >40 e* yat 4**t MlIU MW . * Yf 4M H *J-i >n fcf TMioir i Ml I* * Ml IT 7* / tITrt 9'*) %f >3 ff f*M /f AI * -- - *f 4> - at/ - f6 > - %1 n /*. 14 ?X| 3*4 --u: /* <*M4 0* 4*0 0*/ -ML K xW vn *4#r * j*% y 0tf P)4 - 0*4 MONS 046353 Operating Data X. PLANT OPERATINQ DATA,Icontd. Month of ----} ------------- Aug.1947 i 0 0.98 65.12 33.90 Pounds 6,000 396,500 206,400 Production Aroclor 1142 1148 1154 1160 1162 1164 Pounds 6,000 4,935,373 1,178,200 1168 2565 4065 5042 5060 324,225 258,000 561,600 100.00 606,900 6,728 Per IF:--------- Pounds 0.600 0.472 0.419 3,600 187,200 86,400 Crude Aroclor Total It " lbs/Chlor- I. Day Raw Materials Used fi) Diphenyl 1142 1148 1154 1160 1162 7,263,396 6,719 Pounds 3,600 2,329,200 493,200 1164 1168 2565 4065 87,750 58,500 Year to Date1947 * .08 67.95 16.22 4.4n 3-55 | 1 7.7li 166.00 Per t,b. 0.600 0.472 0."19 0.271 0.227 1.000 1.110 1.226 6,000 440,000 253,000 (2) (3) It*) ! (5) J------- Santowax C 2565 29,250 Santowax R 4065 39,000 5042 5060 234,000 Santowax Isomers 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 CRUDE AROCLOR REPORT HONS 0.090 0.151 0.417 ; 000 1.119 1.242 l.3?9 1.326 1.272 046354 1 , X. PLANT OPERATINQ I&ATA, contd. X ?? Opera*, lag Dara Month of Auk.1947 Per Lb. Suantltv Services ouantlty 1.117 680,000 Steam - Lbs. 7,466,000 Water - City Cu.Pt. O.S46 150,000 1 Water-Reoovered,Cu.Ft. 1,512,000 0.064 59,000 Oas - Cu.Pt. 1,254,000 0.008 5,000 Electricity - KWH 100,500 Lbs.h.H. Cn Hours Labour Man Hours 825 2,859 758 Operating 215 i Maintenance 7,571 2,201 Packing 218 1 Shipping 4 Chlor.Hra, Operating Time 148 Chlor.Hrs. 100.00 48.95 51.05 4,464 Hour*-Calendar 2,185 1 Hours - Shut Down 2,279 i Hours-Oross Operated 107 ; Hour* - Delay 2,172 ! Hours - Net Operated 54,992 8,027 26,965 1,017 25,948 4.70 1 Delays of Gross Oper. Delays: Out of Chlorine 1 Waiting on Charge Clean Chlorine Lines 15 i Clean HC1 Line* 8 Clean Clro. Line* 15 Change Cooking Coll 169 Change Distributor 10 Chang* Chlorine Valve 15 19, Repair Ciro. Pump 14 | Repair Chlorine Lines 155 70 12 1 Repair Acid Towers 28 Waiting on Blowing Tank 1 Low Staam Pressure 51 27 : 52 Repair Water Line Miscellaneous Repair HC1 Line 95 152 166 Repair Charging Line 15 Change Water Line 58 Repair Cone Traps 48 Pound* Shipped and Packed 12 Shipped 12 Packed Repacked Container* Pound* Containers Used Pounds 40 Cal.Black Steel Used 545,95* 40 Oal.Blaok Destroyed 55 Oal. Fibre Dms-Used " Destroyed 100# Fibre Drums Used 650 " Destroyed Textile Cane - Used n " Destroyed 250 ______ L 50 Gal.Qalv.Drums 1000 Year -c Date 1947 Per Lb, 1.028 208 .170 .01" Lbs. 74.1?. 959 5,500 1,^91 2,102 * LOO.00 22.9* 77.06 74.15 5.77 * Pourd? 511,080 525.053 1,867 'Containers 661 1 7 2 . ..A. . of|udb aroclor report HONS 046355 . ' X. PLANT OPERATING DATA, contd,. Month of --------------------,------------------------ Aug.1947 Founds Production! Aroclor - 1242 founds T9.25 20.75 450,109 117,868 Aroclor - 1248 Aroclor - L254 Aroclor - 1260 Aroclor - 1262 Aroclor - 1264 4,882,430 1,066,967 100.00 567,977 17,476 Aroclor - 1268 Aroolor - 4465 Aroclor - 5442 Aroclor - 5460 Diet.Arocl or - Total Dlst.Aroclbr lbs/Stlll Day 240,581 11 488,608 6,678,597 19,948 i Reoovery Pounds 96.05 98.80 468,598 119,299 Raw Materi sis Used Aroclor 11 42 Aroclor 11 48 Aroclor 1154 Aroclor 1160 Aroclor 1162 Aroclor 11 64 Pounds 5,014,936 1,091,108 Per Found Quantity 1.160 659,000 - 1.144 650,000 0.751 0.026 427,000 15,000 Lbs/M.H. Man Hours 666 853 1.993 285 2,927 10,349 225 76 Aroclor 1168 Aroclor 4C65 Aroolor 5< 42 Aroclor 5< 60 Services Steam Lbs. Water-Cltj ,Cu.Ft. Water-Recc v 'du.ft. Oas - Cu. Ft. Electrlclt y KWH Labor Operating Malntenan4e Packing Shipping 259.998 559,601 Quantity 6,856,000 6,518,000 4,64l,OOC 82,000 Man Hours 8,103 1,206 1,520 1,074 x -35 Operating Data Year to Date 1947 73.10 15.98 3.60 7.32 100.00 i Recovery 97.36 97.78 92.53 87.31 Per Found 1.026 .976 t QC, .01? Xbs/M.H. 824 5.538 4,24! 5.58C DISTILLED ^ROCLOR REPORT MONS 046356 X. PLANT OPBRATIHO DAT*, oontd. X - 3** Operating Data Month of 100,00 44,76 55.2** 5.11 Istlll-Houra T755S-----666 822 42 780 founfla 567.619 106.599 2 5 27 1 4,999 2 .L9.jP Containers Pound! 215 106,000 101 59,725 970 19 1.125 Year to Date 1947 Operating Tina_________ (Still Hours Hours-Calendar 11,664 100.00 Hours-Shut Dom Oroaa Hre. Operated 2,989 8,675 25.65 74.37 Hours-Delay 658 Net Hours Operated Delaya % of Or|>ss Oper. 8,057 68.90 7.55 Delays: ; Out of Crude! Clean Cooaenpoks 17 Clean Still Change Coll 62 21 Change Pump 79 Change Cotto(i 15 Change Coke Drain Scrubber 15 Drain Trap 2 Repair RJeot) Halt on Bli 19 56 Low Steen Pi 266 Klso. Install New St Jets Shlppsd and ttjoksd -45 52 Pounds Shipped Arooldr 1242 1248 1254 1260 1.500 4,605.798 948,895 1262 1264 1268 4465 5442 5460 1,627 99,895 607 589,571 Toiar Paoked - Total Repaoked Containers pel Pounds ,445,89'ff 17.644 Container^ Drums i 55 Oal.Oalv.Lpoktop Used " Destroyed 1 40 Oal.Oalv.B^g Used '254,252 470 " Destroyed 50 Oal.Oalv.Bung Used ,1,555.950 " Deetroyed 5 2,288 50 Oal.Oalv.Used " E sstroyed 55 Oal.Fibre-Used " E sstroyed 467,115 150 959 55 1 100# Fibre-Used 5,960 58 " " Isstroyed Slaok Barrels-Used 7.268 50 ii ' Destroyed Textile cansjusad '< Destroyed >.* 490,520 106,000 Paper Liners-Used " " Destroyed! Tbnk Oars (1254) Tank Cars (1260) 5,564,8od 942,5151 HONS DISTILLHD AROCLOR 046357 X. PLANT OPERATING Dm. contd. X - 35 Operating Data Month of Aug.197 Pounds Production Muriatic Acid - Total ft Recovery Pounds Founds Day Raw Materials Used Anhydrous HC1 -Equlv.18"B4 Acid -Equiv.20 *b Acid 100.00 17,143 Muriatic Acid, 20"Be Per Pound Quantity Services Water City - Cu. Pt. Water Recovered-Cu.Ft. Electricity - KWH Lbs.M.H. Man Hours Labor : 1,207 16 Man Hours - Operating Man Hours - Maintenance 568 34 Man Hours - Packing 1,315 ft .12 Man Hours - Shipping Tovrer-Hrs Operating Tine Hours - Calendar Hours-Shut Down dross Hours Operated Hours - Delay Net Hours Operated Delays j< of dross 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 Chlorlnators 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 "A1' destroyed Carboys - Stranger Pounds Year to Date 19*7 Pounds 174,610 ft Recovery 155,009 100.00_ Quantity Per Pound Man Hours Lbs.M H. 75 27358 24 7,275 650 268 37 4,695 Tower Hrs, % Pounds Pounds 74,700 99,522 Pounds 173,698 17tt,0^0 Containers 1 875 rRIATIC ACID 18" Bi REPORT HONS 046358 X. PLANT OPERATIMQ PATAJ contd. Month of--i---------------- r~\----------- fives. 19*7 Founds Production 993.329 Muriatic Acid - Total 63,066 founds Day * Recovery Founds Haw Materials Used Pounds 349,000 Anhydrous HC1 4,226,850 |Equlv.l8*Be1 Acid 90.37 1,099,213 Uqulv. 20 "Be Acid 13,334,941 Muriatic Acid, 28* Be1 89,960 limestone 640,160 Per Pound Quantity Services Quantity water City - Cu.Ft. 292,000 0.580 576,000 water Recovered-Cu.ft. 6,572,000 Mlectrlolty - KWH LbsTH.H. Man Hours Labor Man Hours 4,415 41,389 223 24 Man Hours - Operating Man Hours-Maintenance 274 36,324 26 Man Hours-Packing 319 28,707 24 Man Hours-Shlpplng 180 i Tower-Hra. (Berating Time Tower Hrs. 100.00 "74? Hours - Calendar 5^32 47.85 52,15 356 388 10 Hours-Shut Down dross Hours Operated Hours - Delay 1,191 4,641 401 378 Net Hours Operated 4,240 0.026 Delays % of arose Oper Delays: Out of Chlorine Clean Acid Lines Clean HC1 Lines 4 Repair Acid Lines 4 Repair HC1 Lines 13 10 Founds 17,143 107,458 Founds 688,976 944,436 Containers 10 154 2 Rounds 671,420 17,556 Repair Vent Lines Repair Drowning Tower Repair Absorber Repair Coke Scrubber Work on Chlorlnatora Storage Full used and wasted Used In id* Be' Acid Used In A1C13 wasted Snipped and Packed Shipped Packed containers used Tpnk Cars - Monsanto Tank Cars - Foreign Carboys "A1' Used Carboys "A" destroyed 360 14 Founds 6,187,314 1,695.570 80,612 Carboys - Stranger X - ?6 Operating Data Year to Date 1947 Pounds 8,529,464 48,282 % Recovery 63.96 per Found 0.034 0.771 "TEsTHTfr 2,996 31.129 25,595 44,241 % 100.00 20.42 79.58 72.70 0.64 rounds 155,009 4,801,323 Pounde 7,963,458 8,164,674 containers 91 23 708 MURIATIC ACID 20* Be1 Report MOMS 046359 X - 37 Aroolor --< cm ^ 81ass*. Astail HmUmmi COT! fian Astasl ftlWlt Amb betas1 PUtlllo ^Aroclor Stilly Vo. of Sobs bsferw 4000 lbo. .59 ... 1148 4000 -- .534 -- U3* 3600 -- .466 .472 1160 3600 -- .417 .419 1162 1164 1X68 3600 3000 3000 -- .396 -- -- -30 ... .34 -- .84 .96 1.10 1.20 1.24 1.28 1-36 -- 1.122 1.7*6 -- -- -- -- 9T.57 97.W -- -- ... 1135 (Sis. 0 1047 5 ebafN 5 5 5 5 3 3 a*5 2290 **5 1950 9042 5060 -- -- 750 Iks. tat. C .276 1300 lbs. tat. X 282 4000 lbs. tat. 1 3000 lbs. tat. R .------ .282 .230 -- -- .098 .091 .147 .398 .417 .158 _ .417 1.30 1.320 1.30 1.3* .84 1.20 -- 1.251 1st distills -- 90.72 -- 85.0 1047 . - 3 3 3 Ik-- prsstle* flforu cr* for tbs psrltt Jsosary - Jims 19*7 la aost tastaaess. HONS 046360 X. PLANT OPERATING DATA, contej. X - 78 Operating Data. Nr. 0. K. Crouoh, in a letter dated May 16, 1955, shows that the theoretical figures for chlorine consumption at Anniston are on a different basis fron those given on page X-3 above for the Krummrlch plant. As an example of the Anniston methods; Aroolor 1268 should contain 6 theoretical yield 100 lb. of of chlorine, therefore at clor should be made from 2 x 68 - 136 lba. of jthlorlne. The theoretical yield on chlorine, therefore, should be 100 x 100 -135 73.5* The Krummrioh plant Theoretical Conversion Factors obtained from Experience are a little different in most oases. The Anniston Production Standage 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 J.27.8 133.50 165.8 Santowax C Santowax R 2565* 44655460 5442 1248 26.60 26.10 -- -- 55.0 |l32 1151.5 |l48.20 104.5 101.5 --------- 1 9.50 -- -- ' -- 17.40 50.2 69.2 ... the *Mr. J. X. Crouoh in his letter of May 18, 1955(aentloned at/top of this page) suggests that this figure is .'ather low. only small amounts of 2565 .ad been made at Anniston, so good data were not available. HONS 046361 X - 39 Operating Data X. PLANT OPERATINO DATA. oontd. Anniston The/standards for utilities, services, eto. are grouped for all the Aroolors, as follows: [ Crude Aroolors: Steam 106 lb./lOO lb. crule Aroclor Electricity 1.21 K.V.H. Plant Water 16.69 ou. ft. Puel 11.84 ou. ft. (naturtl gas) Laboratory 0.01 unit Labour 0.06 nan hour j Maintenance 12ft Supplies Iff Distilled Aroolore (from Crude 11 Steam 109.5 lb. per 100 Its. distilled Aroclor. Bleotriolty 0.69 K. W. H. Plant Water 76.95 ou. ft. Puel 67.09 cu. ft. (natural gas) Laboratory 0.1 unit (4ff) Labour 0.1 man hour Repairs 8^ Supplies 2i Mr. Bllenburg, January 20, 1948, gave 0.66 cu. ft. gaa/lb. Aroolors the gas being about 1060 B.t.ul/cu.ft. MONS 046362 XI - 1 Hazards XI. HAZARDS. Toxicity Thar* are many literature refeienees*to harmful effects of the type of "ehlor aone" resulting from exposure to chlorinated diphenyls, especially In cases where people working with small electrical com ponents have been exposed to tne fumes of hot, highly chlorinated, Aroclors. Chlor acne Is sometimes accompnled 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 A:roclors were being made from diphenyl which had oome from low grade fenzene. Since good benzene has been used, the same Aroclors have bfen made without trouble. In March 1955 It was reported that the Annls^on diphenyl and Aroclor plants had run 12 years without lost time accident. Prom the start of Aroclor manuf: eature at the Krummrlch plant the operators have been supplied a clean change of clothes every day, and time has been allowed at thie end of the shift for bathing, Operators are advised to wash {lands and face before eating. The Anniston operators do not have the same Issue of clean clothes. * Percy May, "Chemistry of Synthetlo Drugs" , 3rd edition, page 19, The "Chemist Analyst", September 19^7, Volume 36, Ho.2 page 33, and a report by Dr. M. C. Lpster, Anniston planE7 1937, give data on the toxicity of diphenyl. MCC Bulletin P-ll5/&en?lonst&?j>^to 1.0 mg. per cbm In air as the highest safe concentration cf higher Aroclors, and 10 ng. lor more highly chlorinated Arc dors, H. B. Bdklns "Chemistry of Industrial Toxicology", page 0.5 to 1.0 mg. as the allowable limit In working rooms. gives The MCC Bulletin "Physical Properties of Aroclors" mentions sye temlo effects arising from the oral Injection of Aroclors. See the letters, E. Mather to P.J.C.Haywood, December 17. 1953, and Mather to Newman, January (, 1952 reviewing the literature on the toxlolty of Aroclors. See also correspondence relating to the article In Chem. k Big. News -JMay 17. 195^. pages 2038 and the warning labels mentioned on page VI-3I< above. HONS 046363 XI. HAZARDS, oontd. XI - 2 Hazarda 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. 7. T. Marshall , St. Louis December II, 1951 AROCLORS::TOXICITY Since writing to you on December 3rd I have come across a letter of mine to Mr. W.j M. Cooper, London, June 24, 1948, (copies to W.D.S. W.H.O., and others), calling attention to an article in the J. T. Baker Company'8 "Chemist Analyst", Volume E6, 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 hot make any comments at the time, but the following extract from Mr. Barbre's letter is Inter esting: "During the 11 years of production here only one man evidenced derinatltls. He had also shown similar symptomb in several other departments. When making Aroclor #1270 which Is flaked, a noticeable amount of fine fume solidifies In the alrL 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". HONS 046364 E. Mather XI - HAZARDS, contd. XI - 3 Hazards The Chemist Analyst, Vol. 36, No. 2, page 33, J. T. Baker Chemical Co., Fhllllpsburg, N. J. September 1947 ON THE TOXICITy! OP THE "AROCHLORS" (slo) Robert M. Brown, Chief Industrial Hygiene Section, Division of Health Dept, of Public Weifare. City of St.Louis, Mo. <4A recently published artlole gllo, M. Martin, Chemist Analyst, 35 9.4 (1946) ), has recommended the substitution of one of the "Arochlors" as the melting-point bath liquid In preference to the oustomary sulphuric add. As s Hated in that artlole "Arochlors" are a group of ohlorlnated dlphpinyls produced by the Monsanto Chemical Company. There Is need therefore to give warning. For the toxicity of these compounds has been repeat idly demonstrated, both from the standpoints of their absorption from the Inspired air, as well as from their effects in produ .lng a serious and disfiguring dermatitis when allowed to rema| n In contact with the skin, Sinoe these effects have been ipeatedly observed, Industrial hygienists have taken care to s| e that the proper controls have been established wherever these| products are used. Por example. the maximum allowable conoentri Ion of ohlorlnated diphenyl for an 8-hour working day Is 1 milll gram per cubic meter of air. It Is probable that nothing llkp an uncontrolled Industrial expo sure will occur In the laboratory. However, whether an individual is subjected to a possible acutp exposure to chlorinated diphenyl, and Its serious consequences, wjlll 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 oareless handling of the material and th resulting contamination of the skin, olothlng, laboratory towe Ls, work table surfaces, etc. the way ls left open for the produc lng of dermatitis. Scrupulous cleanliness must be Insisted up bn wherever this material is handled. The foregoing remarks have beei prompted by the belief that in recommending the use of a materli with whloh is associated a potential hazard from the health standpol| it, it ls very Important that the possible oonsequenoes be presei led together with recommendations for correct handling. HONS 046365 XI. HAZARDS, oontd. | XI - 4 Hazards Mr. A. C. W. Pennington of Newport, reporting on his American tour, December 29, 1950, page p, writes: "HEALTH AND SAFETY": ; "At Anniston, no special! protective olothlng is provided for the Diphenyl and Aroclors operators. A dally change of olothlng was provided in the past but Uhls practice ceased before the war. Oauntlet leather gloves and face shields are, of course, available as required on the plant. i " Tins of cold oream olrjtment, theatrical quality, are to hand In the building, but the application of the cream is left to the operator's decision of the Job kn 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 reoord of tjath taking Is not warranted. "Emergency showers are provided on each floor of the Diphenyl building and safety notices aze widely used. "At St. Louis, Plant B, ;he Aroclors building Is rated a toxic department. Each operat >r Is provided with a complete set of olothlng comprising hat, co it, trousers, combination underclothes, Books and rubber shoe i. A clean change of olothlng, exoept shoes. Is plaoed In tip operator's locker in time for the following shift. Men working | ixtra shifts are given a clean set of olothlng. Canvas gloves I goggles are provided and 'Ply' hand barrier oream Is avallabl i 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 arc actually taken. Theoretically, food Is not allowed to be eaten within the Aroolors building, j Instructions are lasued that hands and face should be washed well before eating. "Employees In toxic depi 'tments are given an annual medical examination and a lung X-ray i ary three years." HONS 046366 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. P Rapps to E. Mather) the Admiralty expressed Interest in the dete ^mlnatlon of micro-quantities of Aroclors. MCC have a method f<kr the determination of traces in air by means of the "Halldometir". Mr. Ellenburg, March 15, 195 ^ mentions work done by H. B. Richards Jr., of MCC, June 17, 1953, on the determination of the concentration of Aroclors in air. Mr. Ellen!)urg 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 and will help us to know a little better Just what is the s|fe limit of Aroclor Vapours that one might work in." A question has been asked about the possible harm to plants if Aroclorcontainlng 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 havi 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 bf very positive ventilation. The vapours of hot Aroclors art 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 Krummrlch plant bear a label calling attention to possible toxic effects. MOMS 046367 XI - 6 Hazards XI. HAZARDS, contd. Plre Hazards Diphenyl, of course, will burn,land reasonable care Is needed In handling it. Precautions with toluene are mentioned also on pages VI-29, and under "Special Risksf, below. The Aroolors are handled as If i ion-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 dally inspection of safety showers, fire extinguishers and gas masks, a check list being provided. Planged 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 j Bach operator in the Krummrlch Aroclor plant Is supplied with goggles, rubber covered gloveB, 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 j The usual care Is necessary In 4eallng 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 chlorlnator were badly out of line. A Davis "Vapotester", model M-ll Type A, (Division of Davis Emergency Equipment Co., Inc., Newark, N..'.) 1b held In the department for use In testing the air of the working building after toluene has been used, and for testing vessels bnfore men are permitted to enter, and before "flame certificates" are given. The instrument contains a MONS 046368 XI - 7 ' Hazards XI. HAZARDS, contd Special Risks, contd. oatalytlo oell 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 kre present, the temperature of the oell 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, ajid In traolng spills of gasoline, etc., from a neighbouring oil refinery Into a public sewer which runs under Monsanto territory. Mr. Benignus, of St. Louis, September 1953, dlsoussed the dangers of using Aroclors In Indoor paints. He discounted the possible dangers from phosgene formed by flash dischargee In transformers charged with Aroclprs. See the references to safe handling of glycldyl phenyl ether on pages IX-161 etc. i MUMS 046369 XII. EQUIPMENT LIST XII - 1 Equipment List The following detallB are largely drawn from pages 18 - of the report by Lyles, Soffranko and Seeker, Hovember 1946, and they relate to the plant "B" (now Krummrloh Plant) equipment, unless otherwise stated. A list of Aijoclor equipment at the Anniston plant was sent to MCL June 7, }946. . Oeneral Mote Since diphenyl and some of the jAroclors become solid, or viscous, at ordinary temperature, atteniitjlon has to be paid to steam tracing or Jacketing of pipe lines, ancj to the provision of gas flames for looal heating where necessary With due care, because of the presenoe of diphenyl and in s<oite cases of toluene and butyl aoetate, naked flames are quite fii^eely used In the plant. (See operatlng Instructions, Section XV. below). Pipelines used for Aroclors ne ad heat Insulation, also proper allowance for expansion where nigh temperatures are involved. Flanged crosses are freely usee} to assist in locating and clearing blookaiges In the pipe lines, I^nes for diphenyl and heavy Aroclors should be blown clear after us4 This also refers to outdoor water and steam lines, for example ri'Ail tank oolls. In cold weather at the Krummrloh plant. Sohwartlng and others, "Process Description -- for Aroclors" November 12, 1953, page 3 stat^ "Since iron has a deleterious effeot on Aroolor electrical p:^parties, the distilled product Is handled In monel, monel-cla4 zinc or tin-sprayed, and 904 4stainless equipment. galvanic * Iron or stainless steel Is used for the process piping beyond the distillation stage ---------". l MQNS 046370 XII. EQUIPMENT LIST, contd. XII - 2 Equipment List Oaskets and Packings I The following gaskets have been found suitable for use In the Aroclor prooees(1948) s I #901 Oarlock - 1/16" 1" - 1$" - 2" - 3" and V. Used for all orude maturlal transfer lines. #900 - Yellow Oarlock l/8"and 1/161', sheet Gasket. Used for finished material transfer lines. Metallic ABbestos Ooetze gaskets 1" - 2" and 3". Used for solid Aroclor line flanges; will stand heat. Ooetze Aluminium Asbestos. 16" I.D. 21$" I.D. and 9" I.D. Used for Pyranol Car heads. Ooetze Metallic Asbestos 2" flange gaskets used Inside, top and bottom of 18" sparkler press. #262. 1/2 "x 3/8" square Oarlock gasket. Used In flange face of Sweetland presf. Qum rubber flange gaskets used in HC1 valves and lines. #900 Oarlock gaskets u fed on all Chlorine flanges, tank manhole covers. Inspection plates. Inspection plates, and between all pump and t,ink flange connections. Qum or Oarlock red rubber gasket material used on all HC1 tank flange oonneotlons. Samples of Ooetze corrugated fopper-asbestos gaskets were sent to MCL, April 9> 1947, and again iJune 24, 1948. The 2" I.D. x 4" gaskets at that time cost $0 189 each. MQNS 046371 XII. EQUIPMENT LIST, contd. | XII - 3 Equipment List Oaaketa and Packings, oontd. i See alao the London Engineering Dept. Final Report on the atart-up of the Newport plant, for a discussion of gland packings for uae against hot Aroclors. See alao MCL Research reporta bn packings and gaskets for hydraulic fluids, for example: -- 347 50/175/3 November 1950 355B 51/91/H 1151 DP 54/21/3- August 1951 June 1954 - DP 54/271/l1152 DP 54/1'V5 April 1954 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. Tpe 1" size cost $0,004 eaoh. MQNS 046372 .* XII. ' EQUIPMENT LIST, contd. XII - 4 Equipment List PUMP PACKING LIST SQUIF.NO. PUMPS P-0629 " 578 " 579 " 1056 " 731 " 575 " 604 " 573 " 574 " 580 " 1509 " 594 " 1277 " 565 " 1250 " 378 " 1054 " 1260 " 585 " 592 " 584 " 583 " 929 " 617 SBRVI 3E #1 Chlor Pump #2 " #3 " #4 " " " #1 Scrubber Pump #2 #3 " #4 " " " " #1A " " #1 Blow Tank Pump #2 l,i" - - " #lj.tllf' Pump- #2 #2 . - ti Re. Pum t> " City WaterPump t > Tourrill It It It II Tantalum 18" Sparkler Pres 1. Pun 18" " Head Oasket #1 Diphenyl Stg.T c. Pun #2 ,, ,,1 It #3 Aroclor Stg. T ink Pun #4 " " It #5 " " 1 II CT03*7 - Dlpheny. . Stg. Pun SIZE PACK. 5/16 inch II II II 3/8 It It " It 5/16 tl 1/2 II 3/8 1/8 It 3/16 1/2 x 3/8 1/2 It It II 3/8 type and no. op PACKING #234 Oarlock II tl It II M II M II II It II II It It tl II II It II II II It II tl Palmetto H #117 Oarlock II II It It #262 #234 V " ll tl It ll II II II Palmetto P-0595 P-0427 P-0943 P-01119 P-0725 P-0346 P-01111 Flaker Drum 1170 Stg. Pot Agl ;ator #1 Still Condense Pump D 218 Dept. Inhibitor Acid Pui Wllfley Pump at # , HCL Stg. " " " HC . Tr.Tk. Dept. A-246 #7 Sweetland & OS Press Pun #6 Stg. Tank Pump TCB Unloading Pum] 1 1/2 3/4 1/8 1/4 -- -- 3/8" -- 3/8" #234 Oarlock #234 Oarlock #117 Oarlock #234 Oarlock. Do not use ptkg. It II tl It Cutno or Palmettc No Pckg. req'd. -- Palmetto MONS 046373 I . XII. EQUIPMENT LIST, contd. j Coolcs and Valves XII . 5 Equipment List A 2" Crane all Iron Oats Valve #475$ Durlmet Stems. New Style I j 2" Meroo cook - Cast Iron) i 1 ii n ii ii n j Powell, Rising Stem flanged 1$" Stainless Steel Valves. Clip gate valves. Brass or all Iron. Barstook Needle Valves. j 3" Crane #475$ New Style with Durlmet stems. For all 2" Chlorine lines. For all prude Aroelor lines. Blow Tanks, chlorlnators, scrubbers. For all finished Aroelor lines, also for all Pyranol lines. For all Pity water lines. On all Manometers for ohlorlne and vacuum. On all HCl off gas lines between scrubbers and HCl absorbers. NOTBi Mr. D. 0. Furzey, December 5, 1951, reported that cast steel valves were used throughout fir the hot process liquors. Meroo lubrloated cooks with s;fecial high temperature grease are widely used. Monel or bronze valves, or cocks, are used wherever their use appears to be desirilible. See also the note on the use if Teflon lined cocks for chlorine at the Anniston plant, page 3i Section VI, above. HONS 046374 T .I ' XII. EQUIPMENT LIST, oontd. Blowra j | XII-6 Equipment List B-034-0148 B-034 Blower from American Blowier Company. Type 3V. Used to exhaust fumes from around the Pyranol filter press, P-0159. Oh roof of CR. Motor M-|I&1752. B-094 Blower from American B1 rer Corp. Serial #5364. Print 0-46215. #30-CCW-feHD-FH type E fan with LS wheel. Welded steel pedfestal for motor. Drive thru couplings. Clockwise rotation, hori)fcontal bottom discharge, Order B7377 on 4/14/36, peq. 69122 on 4/14/36. Price $104.21. Driven * M-0832-3HP-1220 RPM In lean-to on second leva1 platform. On flaker D-012. B-0105 Clarage Blower purchased from Anniston. Pan #47361, Type Cl #7 with outboard) sleeve bearing."V" belt drive to M-Q904,Ueed with eye,Ijpne CT-0852, On platform in lean-to. Driven by M-<09P'4. On flaker D-012. B-0148 Blower from American Bicker Co. Size #1-3/4 Slrocoo 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 1/29/40. At CT-0763, Bldg. CR. Direct connected to M-01I710. On melter and still tapping drums. All blowers are of ordlr ary steel construction (EM, March 10, 1947). Drawing D-6945 shows the fume exhaust system at plant "B". MONS 046375 [ XXI. EQUIPMENT LIST, eontd. XII - 7 Equipment List CT-0347 - 0744 Closed Tanks CT-0347 Tank 40' dla. x 16 3i" high, 1st course 1/2" metal, 2nd course 3/8" top! i" sheet - 2-6" Cl nozzles on bottom, 4-4" 01 noz| on top. 1-20" Cl manhole on side shell near bottom. |L-20" th. steel hatch on roof. Nay 1927 Drawgs. b-978 and C-1117 (tank and foundations) (diphenyl store}. CT-0743 Jacketed vaporizer, 2 parallel vertical 10" dla. x 4<4" tanks surrounded by 2'0" ID x 4'0" Jacket. Use XHy pipe - Jaoket of i"| plate, Drwg. C-818. Order B9038 on 5/6/36, Req. 696^'0. Price $180.00. 2nd floor 12' level south side BidIg. CR. CT-0744 Middle chlor. tank hade by Nooter. 3' ID x 16' lg. with fig. head, she^l 3/8" and head 7/16" thick, 3/16" Jaoket over lower half of tank. 3/16" Inner shell and 2 sets of 1" XKy pipe colls. Order B9037 on 5/6/36, Req. 69669. Price $716.00. Same as CT0745. In 1947 there were our chlorlnators In use, CT-0744, -0745. -0833 and -01283, al|1 essentially similar, and later CT-01432 was Instalk ed, only slightly different. Each chlorlnator Is a vertical steel vessel 3'0" ID, 16'0" high on the s freight side, with bulged bottom and flanged cover, Drawings E 880, E 6209. Relief connection drawing !-822. Chlorine Inlet, drawing B 659, The body of each chlorlnator has the following fittings; A Jaoket for waper and steam, starting about 18" up the straight slfile and ending below the level of the charge. This af:rangement leaves the bottom of the vessel available for flame heating, and It leaves room for a slmpfe manlld low down on the straight side, for the ofl lorins Inlet fitting described below. There Is a splr$:1 baffle In the Jaoket space, to Increase the coi$llng effect, but the baffles favoured the accumulation of mud In the Jackets, and at the MONS 046376 XII. EQUIPMENT LIST, contd. XII - 8 Equipment List CT-0744 Closed Tanks, eontd. CT-0744, oontd. 1. oontd. overhaul In No' 'ember 1948 most of the spiral was removed, leavl only enough to preserve the spacing between Jacket and liner. It was also planned to put two 4" nozzles low down on the Jaoket, to facilitate cleaning. Clt; water is used rather than well water, and the Jacket are cleaned occasionally by means of Inhibited acid The used cooling water goes to a collecting d CT-0752. There does not appear to be any trouble f: Hn flashing of water Into steam in the Jacket, In spl ;e of the high temperatures used. See? however, the n >te below on the bursting of a Jacket due to trapplni of water In It at high temperature. The walls of t] ie chlorlnators, above the Jackets, are thermally .nsulated, partly for safety and partly to keep down t! ie temperature of the building. .2 Formerly (but kow abandoned at the Krummrloh plant exoept In the new chlorlnator CT-01432) an Internal coll for steam and water. >. An Internal cy linder, about 24" ID, with perforated bottom, and a *etalnlng grid on the top, containing about 8' depth of Iron-turnings. See page 1, Section VII, above, fo:l> a description of the turnings. 4. A bottom outle with cock, to the circulating pump, P-0578 etc. A so formerly, from No. 1 chlorlnator, to the gas hea ed chlorlnator CT-0808, used for making the hlgl er Aroclors. A piece of heavy gauze Is placed over| the outlet to retain stray pieces of metal, and at he Anniston plant there Is a small catch pot In tl e line to the pump, for the same purpose. The lnea are arranged for easy clearing, and have steam! tracing. (Aroclor Jackets at Anniston). * See page XII|l0. MONS 046377 XII EQUIPMENT LIST, contd. Closed Tanka, contd. XII -9 Equipment List CT-0744 CT-0744, contd. A manlld very nearly at the bottom of the straight side, carrying the chlorine Inlet fitting, nils fitting consists of a shallow round box, set hori zontally below the Internal oylinder of Iron turnings, and having about 240 round holes 5/16" diameter on Its upper side and a 5/4" drain hole on the under side. The ohlorlne enters the box horizontally from the chlorine Inlet aontrol valve. It is advisable to have a spare Inlet box, because the holes Blowly 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 oast nickel. Cast monel has also been mentioned. Nickel oast 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 blockades 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 ea<jh chlorinator has the following fittings: .6 An Inlet, with l ight glass for diphenyl from the measuring tank CT-0767, aid formerly for high boilers from the melter CT-0765. 7. An Inspection cover, carrying the return inlet from the circulating pump. This Inlet Is carried through to the centre line]of the chlorinator, above the internal oylinder. .8 A vertical 10" Central pipe for the off gas,leading to the bottom of oie of the scrubbing columns CT-O759 etc-, and so to the HJ1 absorber. This exit pipe has a hand hole with cover! on the side, for cleaning, and has a MUMS 0463 78 XII. EQUIPMENT LIST, contd. XII - 10 Equipment List CT-0744 Closed Tanka, oontd, CT-0744, contd 8. contd. relief disc of 4 lb. lead at one oonneotlon. (See sketch on page 10a, Seq' tlon VI. ) ' If the relief dn: b;It bursts, the gaB will go directly to the HC1 absorbtlon unit. The disks rupturfe at about 25 pslg, but they usually last for at least several years. There if a mercury manometer on the 10" pipe to give warning bf blockage In the off-gas system. 9. A return line frtoim the scrubbers CT-0759 etc. goes into No. 1 ohlom;nator. 10. A vent valve, hspd controlled, to a drum outdoors. 11. A thermo well, ijeaching down Into the charge. The fifth chlorinati CT-01432, which has been Installed at the Krummrloh plabt, is of the-same type as the previous four, with Jacket anp internal coll, but the coll has been retained, whereas ttys oolls had been removed from the older chlorlnators. (At the Krummrlch plant, the Internal oolls had been abandjoined as being more liable to put water Into the batch, but |at Anniston it was the Jackets that were abandoned, beosbise on one occasion a Jacket had burst when water was[ trapped In It when the chlorlnato^ temperature reached |a high value). To give still more cooling capacity, thje stream of liquid circulated from and to the ohlorlnator, ^luring the chlorination, can now be passed through a honjpimade cooler consisting of two vertical lengths of Jacketed ^>lpe in parallel. (2" pipes in 3" shells). There is a| thermometer well (glass thermometer) In the top of each rngth of Jacketed pipe. The water goes up one Jacket thin down the other, and so out to waste, no special pipvision being made to keep the second Jacket flooded. HONS 046379 XII. EQUIPMENT LIST, contd. XII - II Equipment List CT-0744 Closed Tanks, contd. OT-0744, contd. The old uncooled 0: rculatlon line has been left In position, so that his external oooler can be byepassed. The circulation p\ therefore, delivers to a horlzon- tal header which hi a four outlet cooks facing upwards, plus a sample cock faolng downwards over a drip vessel (see sketoh),* One of the four cooks will direct the flow of liquid to he air blowing tanks, one will bye- pass It directly t< the top of the ohlorlnator, and the other two will dli ot half the stream through eaoh of the external eoolei and so Into the top of the ohlorln- ator. Thls same No. 5 ohlorlnator has been equipped with a flow reoorder-oontroller on the chlorine feed. An orifice plate with a sulpharlo add U tube Is used on the ohlorlne line, as with the older ohlorinators, and the gas feed to the ohlorlnator 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 whloh operates the flow reoorder-oontroller on the instrument panel. That lnstrument In turn actuates a 2" dlaphragm valve on thi ohlorlne 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 'or the other ohlorinators, except that the expense oannot be Justified at present on any saving of manpower, or on any neoessary increase in production. These two changes both make for shorter average time oyoles In the ohloliplnatlon. Research work indicates that faster ohlorlnatlop (at the same temperature) gives essentially the si product, though Infra-red analysis suggests a sllghtlb different Isomer ratio. This mainly concerns the higher Aroclors, and a suggestion has been made that more rapid chlorination might Increase *page 10a, Section hn. HONS 046380 XII. EQUIPMENT LIST, contd. XII - 12 Equipment List CT-0744 ClQBed Tanka, contd. CT-0744, contd. the proportion of (waste) hlghboillng material produced. Not much experience has yet been gathered on the chlorlnation speed which may be attained, but 800 to 900 lbe. chlorine have been fed per hour on occasion, and a batch of 1260 has been ruj> In 14 hours, and one of 1248 In 10 hours. The Krummrlch plant has not been pressed for output, and 'the present sohhune of working Is to run the chlorlnators at a moderate speed, using each In rotation, overlapping the oycles |bf the different units, so as to maintain a fairly fc'eady consumption of ohlorlne. This suits the ohlorlne epartment, whloh has no outlet for Dsnlft gas when the roolor department Is not talcing chlorine. The off-gas from eablh of the older chlorinators leaves by a 10" pipe runnl|fig about 12' up from the centre of the oover of the ohlorlmator, but the new chlorlnator has only a 4." exit pipe with a very small oyolone, draining back to the vessel. It has Its own Rasohig tower with Aroolor olroulatlon, then a cyclone, etc.. Just like the older units. Aroolors above 1262; are no longer made at the Krummrlch plant, so there Is |suoh less ohance of getting much chlorine In the off| gas, and the off-gas scrubbers, con- tsequently, are of ss Importance. They are still used, and they give a ol .er HC1 for the absorption unit, but If they should he out of action for a time, no partleular harm results The Aroolors lnvolvfl ng the use of diphenyl high boilers are no longer made |at the Kruamrlch plant, and the melterblow case, CT-0763,| for handling the hlghbollers, has been taken out. A seooriod alr-blowlng tank, CT-02086, like CT-0750, has been ihistalled for the ordinary Aroolors. HONS 046381 XII, EQUIPMENT LIST, contd. XII - 13 Equipment List CT-0744 Closed Tanka,contd. CT-0744, . contd. At the Anniaton plafit there are eight ohlorlnators, similar In shape to those a the Krummrlch plant. They have Internal colls for fteam and water, but the water Jackets have been put out of use. The ohlorinatore are located In an open-sided stf<el structure, outdoors, and hang from brackets about 30" bfclow their rims, so that they are free to expand gownwards as they become hot. This expansion distorted the connections to the pumps, which at first were rigid};,y mounted, so that pumps were given spring mountings on s}otted clips. More recently the pumps on two of the ohlorlnators have been mounted on rubber pads on stee} frames hung from the vessels themselves, so ellmlnat ng the distortion due to the expansion of the vessels. The new pumps are 1< rger ones, Taber horizontal Centrlfugal pumps, dlreot ooupled to 5 h.p. motors, 1730 RFM. All the^ohlorlnator pumps have Jackets for heating by Aroolor. The hot A:roolor comes from a standard gas-fired unit In a building near the ohlorlnators, passes through the pump Jackets, then through the Jackets of the pipes and of the cook on the bottom outlet of the chlorlnator, then through the heatlng[ "pad" on the bottom of the chlorlnator, and so baok to the heating unit. The other parts of the oiroulatlon system gn the ohlorlnators are steam Jacketed, and the pad was fo: rly used for steam. The return stream of process 1 terial from the circulating pump enters the chlorlnator by a pipe projecting a little way through the oov ii: r. This location of the return pipe perhaps favours entrLlnment of liquid In the off-gas, but If the pipe goes fufther down, It may dip In the charge, and permit siphoning at an inoonvenlent time. There Is a heavy steel gratl: over the bottom outlet of the chlorlnator, and thi:re is a heavy stool, of steel grating, with a perforated pgate on it, to support the oatalyst basket. The top of the basket has a screen welded over It to confine the 01gtalyst, an arrangement which prevents easy "topping up" o| the catalyst, but by the time that MONS 046382 , .' XII. EQUIPMENT LIST, contd. Closed Tanka, oontd. j ! : | 1 ; XII - 14 Equipment List CT-0744 CT-0744, contd. the topping up Is njseded, there.ls 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 colls In phe chlorlnators go In through the sides of the vessel^ The following notes' on an overhaul of the Krummrlch plant ohlorlnator. November 1948, are of Interest 1 - Chlorlnator covjs;r was taken off and all old oatalyst was removed and discarded. It was found that a solid mass of catalysjt mud, residue, etc. was In the full length of the ahroiular space between the Inner sleeve and chlorlnator) This solid mass was also present to some extent wl n the Inner sleeve. In addition, there was a ho! approximately 8" in diameter the entire length the catalyst bed. .2 The sleeve was premoved from the chlorlnator and the top half was riehiewed with 3/16" steel. Although the top half of the) sleeve did not have holes. It was considerably t nner than the lower half. 3. "Ears" were welded on the sleeve to make for easy removal next time. 4. Installed new reen 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 oast Iron chlorine distributor was Installed, The old dlstrll tor was discarded because many of the holes were enl;ak*ged and beyond repair. HONS 046383 XIX. EQUIPMENT LIST, contd. Closed Tanka, contd. XII -15 Equipment List CT-0744 CT-0744, contd. 6. A new grating, nbove the dlatrlbutor waa lnatalled to hold the catalyit In place. The grating made of x 1" atrips, was purchased as such. 7. A new monel scrsen plate was put over the bottom outlet of chlorLnator to keep catalyst from going Into pump. j 8. Welded corroded! portion on Inside, lower flange of 12" off-gas link. 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 la listed additional Information that may be of Interest and serve fs Information for future use. Chlorlnator Number 2 34 sleeve Biphenyl top of I 3600# 92" 92' 76" 68" 85' Outage of finished il6500 batch 18" 13" 371 All measurementa taken from top flange of shell and not the manhole. MOWS 046384 XII, EQUIPMENT LIST, contd XII - 16 EQUIPMENT LIST CT-074 Closed Tanka, oontd. CT-0744, oontd. ; The performance of the ehlorln&tor was Improved as evidenced by the following flgarea: Before Overhauling After Overhauling Chlorlnator Chlorlnator Time required to chlorinate batoh. 30 - 35 hours 20 - 24 hours Sp.Or. Increase per hour after reaching 1.450 at 90*C. 0.01a - 0.015 0.018 - 0.026 Chlorine pressure entering chlorlnator during last 6 hours of chlorination. 10-11 lbs.gauge 7-8 lbs.gauge Valve In cooling water line to Jacket wide open after 4 hours of chlorination i-2 turns open during entire chlorination Chlorlnator tempera ture toward the end of chlorination 150 - 165*C. 140 - 150*C. Scrubber liquor build up. Past Normal (Every 4-8 days) (15-25 days; Still bottoms pro duced, for all chlorlnators, after every 4 still batches 2500 - 3000# 1000 - 1500# The above data are only approximate but do show a very definite Improvement after overhauling the chlorlnator. HONS 046385 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 deflectcj>rs in that Jacket. The measurements dowr from the flange of the shell were: To top of sleeve To level of 3600# biphenyl charge Before overhauling After overhauling 92" 92" 68" 88" To level of finished 1160 batch 13" 31" To level of finished 1154 batoh 46" To level of finished 1148 batoh 56" MONS 046386 . ' ; < ! XII. EQUIPMENT LIST, oontd. j XII - 17 a Equipment Ust CT-07' 453 - 0750 Closed Tanka, oontd. CT-0745 West ohlor. tank sane as CT-0744. On Dept, struct, steel MCS-0650. #1 chlorlnator. CT-0748 Diphenyl storage tank made by Oraver Drwg. 0609, 10' dla. x 26' long straight side, dished heads 9/16", shell 1/2", welded lonst. 2" xHy pipe oolls, 1" risers, manhole oovers, outlets and sump. Pump P-0585. Order B7700 on 4/17/56, Rq. 69220. Price $1000.00. drwg. 609. Underground west of OR, 1st from south. Same as CT-O749. CT-0748 was originally Installed for general use, mainly on Aroclor brought from Anniston for use in the scrubbers CT-0759 etc., and CT-0749 was piped up to receive material, in emergency, from the vaouum 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 :n pits outside the shed. Submerged pumps actuated by remote control from near the scrubbers. Molten <iphenyl In from rail cars. Return overflow lines from the scrubbers, (disused^. Vent lines protected against weather and fire. Steam coll. One point of the thermo recorder Is In CT-0748. The submerged pumps arejcarried on the manlld covers. Return line from overflow connections of diphenyl head tank, CT-0767. CT-0750 Blow tank made by Oraver. Dwg. B-863. 7' dla. x 7' str. sides, dished heads ", shell 3/8". 5 turn coll of 2" xHy pipe supported on brackets welded. Order B7704 on 4/17/36, Req. 69224. Cost $325.00. On steel MSC-0650 dept, steel, 12' level, 2nd floor level Bldg. CR. 8/10/54sNetwork of pipe with 1/8" holes. Air Jet in sta^k. HONS 046387 XII. EQUIPMENT LIST, contd. XII - IS Equipment List CT-0750 - 0752 Closed Tanka, contd. CT-0750 The cover of Blow ta|hk CT-0750 carries the following connections: - Inlet from cluorlnator pumps, with sight glass, Float with linjdloator scale. Compressed a;' In, to a grid of perforated piping. Connections steam coll, Haveg vent octilumn through the roof. There Is an angle thermometer on the side. Bottom outlet to Punk) P-O58O for delivery to the stills S-043 and 8-062, or 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-OI292 replaced E-863. CT-0751 CT-0752 Cyclone collector pn' jrchased from Qraver. Dwg. B645, 48" dla. x 27" on stj;r. side. 3'6" long and tangei al Inlet near top of side. g3/16'' steel through' , of welded construction. Order B7712 on 4/17, On 2nd floor level, , Req. 69232. Price $84.00 lean-to of CR. Vertloal steel close'd tank made by Graver. Dwg. C -So4. 4' dla. x 5' high wl th flat bottom and dished flanged head, Sides, bottom and tip;ip of 5/16" flange i", welded cons*. 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 chlorlnatcrs. Formerly received the barometric legs of ejectors M3C-0760 etc.. HONS 046388 XII. EQUIPMENT LIST, oontd. XII - 19 Equipment List CT-0753 Closed Tanka, oontd. CT-0753 (also CT-01396) Coke scrubber on the v|acuum still system. Scrubber tank made by Braver. Dwg. C-807. Steel, closed tank, 3 dla. x 10' long with dished bottom and flgd. dlshel 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 oock, to fthe ejectors, MSC-0760, 01392, and 01686. The scrubbers are fll.lied with coke, which Is flushed with caustic soda solution p few times a year. There Is no history of serious co;itroslon trouble In the ejectors. Mr. D. 0. Furzey reported, December 5, 1951, that cotton wool In the scrubbers was renewed every few years. Wide hand hole at the top for oharglng 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 cut the need for an Inspection cover on the top of the scrubber. There la a layer of c< tton wool on top of the coke In the scrubbers. The scrubl ers are needed mainly for the distillatlon of high bollli Aroclors, because there Is a iit-le HC1 formed by deoompoi itlon, but they also trap water which might come back from he ejectors. Mr. Pemberton, December 1950, reported that inis ton gave up the use of caustic soda In the coke scrubbersj after the'Karbate ejectors were lnstalled. The cotton iool becomes glazed over with heavy Aroclors and the vacui lines may choke. See also the comments on pages VII - 4 and 5. MOWS 046389 XIX. 8QWIPM8WT LIST, contd XII - 20 Equipment List CT-0754 Cloasd Tanks, contd. CT-0754 Scrubber liquor pump tank made by 0raver. Dwg. C-800, 4'6" dla. x 5'6" onetr. side with dished heads, shell 3/8" thick. Heads 1/2" thick, welded seams, pads and nozzles. Coll 3 turns of li" xHy pipe. Order B7703 on 4/17/36, Req. 69223, mee 208.00. Tank mounted on stekl, east tank on 38' level. Same as CT-0755 and[ 0756. Of t,ne five scrubber liquor pump tanks, three are coll heated and the two newer ones are Jacket heated. Jaoket heating Is preferred as being less liable to put water Into the Aroolor circulation system. These tanks were formerly charged with Aroolor (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 ehlorlnator, pumped up by means of the ehlorlnator pump. With slew chlorination, especially In the efarly stages of chlorination, the scrubbers tend to pick up diphenyl, and the liquor becomes less dense. With faster chlorination, the circulation liquor tends to increase in density. When the liquor needs to be renewed It is dropped ta the smlter CT-0763 for return to one of tlie ehlorlnator*. The foreman calculates from the density w^at volume should be taken to give the equivalent of a fresh diphenyl charge to the ehlorlnator. See page 10 Section VI, for the method of calculating the equivalent. See letter E.M. to M. B., May 17, 19^8 on the handling of the scrubber charges. MOMS 046390 XII. EQUIPMENT LIST, oontd. XII - 21 Equipment List CT-0754 - 0756 Closed Tanks, oontd. CT-0754 oontd. Hie oover of the scrubber liquor pump tank oarrles the following connections Vent line with hand operated valve normally open to a drum outdoors. Steam coll. In and out unless a Jacket is used. Aroolor line ik from CT-0749. Aroolor line 11 from ohlorlnetor. Return line frpm tower and eyclone, 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 ils used. Exact temperature control Is not needed. Bottom outlets to chiorlnators and to melt tank CT-OTfiJ, and to a levelling 11 ne by whloh material may be passed from one scrubber taiik to another Overflow (disused) to CT-0748 and 0749. CT-0755 CT-0756 Scrubber liquor pump tank. Canter tank. Same as CT-0754 and 0756. #1 sorubber liquor pjnnp tank. West tank. Same as CT-0754 and 0755. HONS 046391 XII. EQPIPMBMT LIST, eontd XII - 22 Equipment List CT-0759 Closed Tanks, oontd. CT-0759 #4 East Aroclor scrubber,used on CT-0754. Made by Oraver. Steel tubular tank, 12" dla. x 8' high, reatovable head. Pkgd. with 6' of Rasbhlg rings. Chg. out $84.00. Drg. C-798 and B-660. 15r dla. cyclone. Oas In at bottom by ide descending pipe from the top of tthe ohlorlnator off as pipe (the HC1 manometer branch comes off the top ofl this line) and out at the top to the cyclone CT-01259( Oil279, 01280, 01281 and 01282.) Liquor In at the top from the submerged pump In the corresponding olroulptlon pump tank, and out.at the bottom by seal bend kith sight glass to the sasie tank. There are four water-cooled ohlorlnators and me gasfired one and for thuse there are five scrubber systems all alike except thap the one on the fired ohlorlnator can be gas heated phe off-gas from a water-oooled ehlorlnator ascends In a wl^e pipe to the bottom of a packed column with Aroclor blrculatlon. Prom the top of the column the gas goes via a cyclone to the header leading to the absorption sylItern of the Aroclor plant or to that of the ohlorbensol piant 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 topei r, plus any trapped in the cyclone, returns to the llquo: tank via a deep seal bend and a sight glass. There s a sampling cock at the bottom of the seal bend, and tfe<ere is a thermo-well near the 3. 0. The gas from the gas fired ohlorlnator goes to the monel gas ohamher CT-01258 where It deposits most of Its entrained solid Aroe. or, and thenoe by wide steel lines, with cleaning flangeu to a scrubber system whloh Is similar to the othern but whloh has arrangements for gas heating. (The gas-f:.red ohlorlnator went out of use in 1949). MOWS 046392 XII. EQUIPMENT LIST, eontd XII - 23 Equipment List CT-0759 Closed Tanka, eontd. 3T-0759 Only ohlorinator #1 .s normally used to feed the gas- fired ohlorinator #1 Is not recharged until the gas-fired ohlorlnato Is empty. Nevertheless, there Is a scrubber system fol #1 ohlorinator as well as for the gas-fired ohlorlnatoij The gas from #1 oan be put to either of these sor >bers. It oan In emergency be vented to atmosphere. Mr. 0. 0. Fursey repjo:rted, December 5, 1951, that the sorubbers and separab:ors sometimes block with solid which has to be melted out with blow torches. A scrubber was lnsti led at Newport, but after some ' experlenoe the Rasol g rings were taken out of It and tthe circulation was topped. It was found that tl off-gases from high boiler chlorin atlon batches deposlfated rather viscous material m the empty tower. This Halses the question of the contamination of diphenyl liquors an the scrubbers, with high boiler products, but the o<examination appears to be unimportant. The towers were flna:liy bye-passed, very little material was collected In the) cyclones which came next In line of flow, and there was X evidence of trouble due to organic matter In the HC1 a.losorptlon unit. At Krummrlch plant e increase in volume per scrubber 4came to about 10 rial gallons per week. The cyclone at Newpart corroded through. The seal bend was removed from Ita{ drain line as being unnecessary. MONS 046393 I XII. EQUIPMENT LIST, oontd. XII - 24 Equipment List CT-0760-0763 Closed Tanks, contd. CT-0760 #2 Center Aroclor scrubber. Same as CT-0759. CT-0761 #3 scrubber tank madq by Graver. Steel tubular tank 12" dla. x 8' high, immovable head. Packed with 6' of Raschlg rings. OrJ CT-0968. Chg. out $84.00. Drg. C-798. CT-0762 Vent line scrubber stj'ored In CR lean-to. Made by Graver. Steel tubular tank, *2 dla. x 8' high (50# std. pipe 3/8") removable head.' Dwg C-798. Packed with 6' of Raschlg rings. Drg. C-798. Supports B-663. CT-O763 Melt and feed tank madai by Graver. Dwg. C-810. Closed steel tank 4'6" dla. x 5'0" on str. side, shell 3/8", dished bottom and bo}ted dished head alii". 2" xHy pipe coll, 10 turn* with 3 supports welded to head. Tk. test 90# and ooll 300# Hyd:ro. Press. Order B7710 on 4/17/36, Req. 69230. Price $1jl6.00,4 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 hlghboller. Steam coll In and out. C. air connection and vent (Dry air from PC-046.) Inlet from all scrubbers CT-0759 etc. Outlet to drums and to header leading to chlorlnators. There Is a hand operated hoist with lifting hooks for drums over the manhole, ana a ventilation hood connected to blower B-0148. The melter Is set In the ground floor of the crude room. MONS 046394 I I XII. EQUIPMENT LIST, eontd. Closed Tanka, oontd. XII - 25 Equipment List CT-0764-0767 CT-0764 North Hopper Storage Bln made by Graver. Dwg. 0-512. Vertical, 6' x 6' x l'8i" high overall, with sloping bottom and bdlt 'angles. 3/16" 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 .001" zinc and then .003" tin. Order B7713 on 4/17/36, Req. 69233, Price $288.00 Southwest end of CR l$an-to. Same as CT-O765. CT-0765 CT-0766 South hopper storage bln. Same as CT-0764. Circulating cooling ti ink made by Graver.On No. 1 Still. Dwg. B644. Steel tanl 2'6" dia. x 3'0" str. side with dished head and weldei on pipe legs, shell i", heads 3/8". Coil of li" di xHy pipe, 4 turns on supports welded to inside of s: ill. Test tk. 225# and coil 300# Hydro press. Safety ralve. Gauge glasses. Order B7706 on 4/17/36. Req. 69226. Price $110.00. On 38' floor level, B$dg. CR. 1-0510 Taylor FUlscopb temperature indicating controller, 0-110*C., with steel diaphragm valve on the steam inlet to the coll in CT-076(5. Operated from the temperature in CT-0766. CT-0767 Diphenyl measuring ti Steel tank 4>6" ID x 3/8, top head 3/8 anc over it and extendi] out. Test tk. 60# line to store tank. made by Oraver. Dwg. C-799 '6" str. side, dished heads, shell bottom head 3/4" with i" Jacket 9" up on tank side. Welded throughjacket 105#.Hydro,press. Return Order B7701 on 4/17/ At 38' level. Bldg. Req. 69221, Price $329-00. Drg. C-799. MQNS 046395 XIX. EQUIPMENT LIST, oontd. XII - 26 Equipment List CT-0767-0770 Closed Tanks, contd. CT-0767 oontd. Steam traced vent to drum outdoors, Manlld. Dipping hol$ with cap. Plxed overflows at 4 levels back to diphenyl store tank CT-0748 by steam traiied line with sight glass and right angle cross pieces iq th blank flanges.- Lower part of vessel Jacketed for steam from the 70 lb. main. Angle thermom* ter 30" long through side of vessel, Bottom outlet to heaqlier leading to the 4 chlorinators. S. Q. at eaoh ohlorlihator. CT-0768 # 3 Aroclor 1260 fln^ shed product storage tank. Made by 0raver. Dwg. C-609 Horlz. steel 10' dla. x 26' long on straight side, diflhed heads, shell J", heads 9/16". Test tank 60# and 00:|1 300# Hydro. Press. Coll 2" xHy pipe with 1" xHy rls$re. Welded construction throughout. All inside and fig Surfaces, ooils, supports, etc., to be sprayed first .00$ zinc and then .003" tin. Same as CT-O769. Or$ier B77H on 4/17/36, Req. 69231. Chg. out $1385.00. $aCl vent trap. CT-0769 # 4 Aroclor 1254 Finished Product Storage Tank. Same as CT-0768. CT-0770 Tubular heat exohangfr made by Nooter. Dwg. B651, Plant A, Size 12" dla. x 5'0" lg. having 19 x 2" OD 11 ga. Monel Tubes, Monel tube shfiets. Monel reducer and carbon steel Jaoket and back-up ngs on flanges. Order B0848 on 5/1/36 Req. 69605. Price $660.00 Above No. 1 still SO*3, supported by 3rd floor steel. Plant "B" (Xrummrlch Plant) corUnue to reoomnend monel for the condensers on the vaouum stills. See also Item CT-01378. Only monel In contact with the goods on the "descending" side of the condenslnig system. MONS 046396 XII. EQUIPMENT LIST, eontd. XII - 27 Equipment List CT-0770 - 0771 Closed Tanka, eontd. CT-0770, eontd. Hr. Thrift, December 5, 1949, raised the question of the necessity of using monel for the vacuum still condensers and subsequent vessels. Mr. Bllenburg of Anniston replied, 15th December, 1949, stating that Iron contamination of the Aroclors would nave a bad effect on the resistivity and the power factor of the products. Steel also hastens the darkening of Aroolors at temperatures of SO*C. or higher. Messrs. Hodges and Barbre of the Krummrlch plant replied that monel was satisfactory for the oondensers 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, Krumnrloh plant do not oare to risk the use of steel because of the high standards required by 0. E. for Aroclors. CT-0771 Monel vacuum reoelvi made by Nooter. Dwg. C-795. (Plant A). Else 5*61 dla. x 5'6" str. side, 3/8" shell, i" bottom and removajllble head, 4 support brackets on outside of tank of steel, IP size xHy Monel coll with 2" inlet and 1" outlet with ijonel bars and U bolts. 3 turns 5' dla. along side and 3 tuifeis spiral on bottom. 60# Hyd. test on tank and 300# on cola. Order B7379 on 4/14/06 Req. 69118. Price $3240.00. On second floor levs!1, 12' level. Bldg. CR. No. 1 still. Return line, for spoilt material, to the stllL of the vanliuum still receivers The covert/ carry the following connections: Inlet from conqensers CT-0770, 01378 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 harid hole and dipping opening. MONS 046397 XII. KgPIPMBNT LIST, contd. Closed Tanka, contd. XII - 88 Equipment List CT-0771-0779 CT-0771 contd. Dial vacuum gauge and meroury U-gauge. Thermo recorded well. Vent cock. Steam coll In fnd out. This coll goes well down Into the bottom dlsfy 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-0565, -01037, for delivery td the blending tank, CT-0779. Electric strip heaters to drawing C-847, formerly used on these vessels have seen abandoned, so no copy of the drawing has been requested for MCL. Material 1268 requires H. P. steam In the coll to keep it molten.. There Is only one receiver for eaoh vacuum still In the crude room,no fractionation being attempted. There Is no gauge g}ass or level Indicator, only a gauging hole.* A receiver wl 11 hold a full batch from the still. CT-0779 #1 blending tank maqle by Oraver. Dwg. E-862. Welded steel tank 7 dla. x 7' high dished heads shell 3/8".> All im4lde surfaces and nozzles sprayed .005 zinc then .003 tin. 2" xHy pipe coll and supports, Yoke and drive suppiqrts. Cast bronze turbine stirrer and bronze shaft. Test tank 60# and coll 300#, hydrostatic Pressurd Order B777 on 4/177, 56 , Req. 69227, Chg. out 4599.00. On 2nd floor level. 12' level. Bldg. CR. Same as CT-0780 But see page 21, section VI. MONS 04639B XII. EgUIPMBNT LIST, oontd. XII - 29 Equipment Lift CT-O779-O78O Closed Tanka, oontd. CT-0779 oontd. See also CT-01399 4IS Blender and CT-O78O, Filtrate Reoelver. Drawings S-862 and [--6838 are essentially the same. Drawings A-459 and 8853 of the bearing have been requested. Drawings D-2076, 20f7, show the agitator rotor and stator. Anniston, Deoembsr 1949, state that their blenders are of steel, sprayed wa: th sine then with tin and that the agitator In one case is of Tobin bronse (stated to be 60* Cu. 39.25* Zn, 0.75 Sn), and In the other oase is of steel, sprayed with slno thtien with tin. The sprayed agitator Is said to be satlsfaotory. Plant "B", January 5, 1950, sta'te 0.005" Zn then 0.003" Sn for the tanks, and their agl tators are of bronze of unknown ooinposltion, probably "o:i^dlnary commercial bronse". Anniston and Plant "B" agree in distrusting plain steel for these vessels. Anniston Suggest Aluminium. OT-0780 #1 filtrate receive^ tank. Dwg. B-862, Made by Oraver. Welded steel tank 7 dla. x 7' high, dished heads J", shell 3/8". Same a^ 0T-0779. Materials 1260 and 4254 can be run from the reoelvers CT-0700 and 01400 td 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 needsiH.P. steam to keep It fluid. The filtrate receivers are like the blenders CT-0779 and 01399 exoept that the filtrate reoelvers have no agitators. HONS 046399 XII. BfflllPMBNT LIST, oontd. Closed Timka, oontd. XII - 30 Equipment List CT-0785 0808 CT-0785 Middle acid tank south of CR on foundation. Made by Ooodrlch. Dwg. C-82B. "Vuloalok" lines - ateel tk. 7'0" ID x 8'6", shell. 5/16", dished head 5/16", bottom 7/16", 4" outlet for safety plgg on bottom. 18" manhole and oover, 5 - 5" flgd. outlets In head, 3/16" Triflex lining, rubber covered float and card for measuring device. Head with 6 - 1$" couplings for railings. Order B9983 on 5/19/P6, Req. 69966. Chg. out 1945.65. South of CR on foundation. Same as 0784 and 0786. CT-O786 West acid tank, same as CT-0784 and 0785. CT-0808 Storage tank and ohlprlnator with stirrer and gas burner. (Qas fired ohlorinatpr). Made by Kilpatrick and Sons My. Co. Dwg.'sA?24, Cast; Iron, 61 ID x 4'11" 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 maohlne work $36.DO. Order B8162 on 4/24/36, Req. 69398, Cost $517.65. On 12r level SW comer Bldg. CR. Drawing C830 gas heater on exit-line. Subsidiary drawings: Pr. relief door on 6|' 0" Cl storetank Clamp for electric rip heater Vent for 01 tank Shear pin unit -- fo|t> drive on agitator Brick setting Drive for stirrer 8'3" x lO'll" steel phell for tank Vent stack for stlll{ heater Still heater B-613 B-684 B-686 C-665 F-867 E-888 E-88J B-689 E-886 This gas-heated ohl 1nator Is also called 3-0459. The 3chlorine enters the as-fired ohlorinator through a per- forated pipe ring. d there is a separate Inlet pipe1 HONS 046400 XIX. EQUIPMENT LIST, oontd. XII - 31 Equipment List CT-O808 Closed Tanks, oontd. CT-0808, oontd. with a simple open end for use when the perforated pipe becomes choked. The cover carries a wide neck through whioh material recovered from the 4onel catch vessel CT-01258 can be returned by means a wide steel runnel. There is another neck, wide ^nough to admit a sampling bottle - also used as a gaug: ng hole. Inlet from #1 chlorlnator CT-01283 by a gas h*iated gravity line or via pump P-0907 through lines with P. steam tracing. 9" monel duct, with cleaning flanges, rises at 45* from the chlorlnator cov< then descends at 45* to the monel gas chamber CT-0125$ From the monel chamber onwards the ducting to the Scrubber Is of steel with cleaning flanges. Compressed air oonnictlon 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-02$ and R-027 In an adjoining lean-to building. See Drawing E-867 for the furnace setting, E-881 for the steel casing of the setting B-888 for the drive C-605 for shear pin for drive B-613 for pressure relief door on furnace K-886 for vent stack, F-324 irhlch shows a shallower vessel; the ihlorlnator pot Is similar but Is 4'11" deep. The final chlorlnatl on to high chlorine content is more easily done In this separate chlorlnator because higher temperatures are neiSded to keep the charge molten. MONS 046401 t XII. EQUIPMENT LIST, contd Closed Tanka, oontd. XII- >8 Equipment List CT-0808 - 0858 CT-0808 oontd. Drawings B-684 strip heater B-686 clamp for strip heater B-689 vent stack for furnace have not been requestiied as they are not of interest, Strip heaters aw nolj now used. CT-0631 Mater condenser made by Heine Boiler Company. Dwg. B485 (Plant A), used as temperature control for Aroclor condenser CT-0770. *2 tubes, 1" OD - 10 QA seamless steel tubing 10'-Of long, lO'O" overall length of 6" std. pipe shell slngle pass. . .Req. 69576, Price $9^ 00 .Used on #1 vacuum sti;11 Order B8773 on 5/11/36, Safety valve on shell CT-0833 Chlorlnator puchased from Leader Iron Works. Size 3' dla. x 161 made up complexe including colls, inner shell, and grating. Dwg. B-880 and B-659. Order B-2813 on 2/5/37, Req. 76475 on 1/26/3? chg. out $790.00 on 3/31/37. Bast chlorlnator #3 chlorlnator. See CT-0744. CT-0848 CT-O852 TCB stg. Tank. Made1by Oraver. Tank dwg. B 4413 Coll C4412 for steam Oeneral B4366 Tank 8' ID x 25'6" lq:mg welded. 3/8" shell, 7/16" dished heads, 13-26" and 2-24" dla. manhole openings on top. 8-1" xHy. H. S. pip* coll, 71' approx. Order B3634 on 2/17/3'7, Req. 76931 on 2/12. Prloe $920,00 West of CR underground. Pyranol Plant. Raymond 2 stage oyoloime dust collector sent to B by Anniston Plant. Baolt cyelone approx. 20" dla. - 21" str. section 32" depth of oone, Bteel construction, used with B-0105. In lean-to building CR. No drawing. HONS 046402 - K-Mll MONS 046011 iylt Cyto**t CT-mTI fci-*Nr TlW "`ffl no loll CHIvvmIw *** . CIwmMt *211 Aahrft t-4%4 ,-? p.OY% :* (tltVIMT Ft** #> fir*t*r ** A* )*) T* CT-01*4 MONS 046012 mr*km Cf f n Jits!sr FLBW WIT OF FQUIPWIKjT. -rt 4 "n ** fMf.-wj < tv >u Uit 9hlt Cfet*M CT- crjfc* ** Coll* Wvbkin Arodor Str* T*% "~ um CT- eiM ' atMO QC C---r-v--*-- Ai irtonelarr St t-TU ffT.-OoT?,,*,q. MONS 046013 V. PLANT LAY-OUT V -1 Plan'. Lay-out The equipment at the Krummrlch 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 Aroelors, 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 370 P 373 P 374 p ?86 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 3teel work Is now very badly corroded, al30 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 11`tle corrosion of steel equipment and Internal platforms, out fh? 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 chlorlnator was Installed since those drawings were made, and more recently a fifth one has gone in. MQNS 046014 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 ohlorlnators and their pumps In an open (roofed) struoture nearby. Here again, most of the store tanks are outdoors. The HC1 absorber also Is outdoors, at some distance from the Aroclor building. There Is no equipment for making solid Aroclors at Anniston. Both plants have railway tracks alongside the main building. HONS 046015 VI. PROCESS IN DETAIL VI - 1 Process In Detail Handling of Diphenyl and High Bollprs Diphenyl and the Diphenyl High Boilers are made at Anniston and the Anniston Aroolor 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 colls, 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 coll to prevent develop ment of pressure from the main coll of the tank, (note the possibility of development of full mains pressure In the shell of the rail tank If the ooll 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 90*C., and their connecting pipes and vent fittings are steam traced. Their temperatures are automatically reoorded. The diphenyl Is pumped from them by submerged pumps P-0585, -0592, to the overhead feed and measuring tank 8T-O767. This tank Is steam Jacketed to keep the contentsat 85*C. 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 flow can be directed to whichever store tank is In use. Prom CT-O767 the diphenyl charges oari~go by gravity to any of the five chlorlnators CT-0744,-0745, -0833, -0183 or (No. 2, 1, 3 4 and 5 respectively), and -03 ' 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. HONS 046016 VI. PROCESS IN DETAIL, contd. vi - a Process In Detail Handling of Diphenyl and Hitch Boilers, contd. The crude and refined diphenyl high boilers.when formerly used at the Krummrloh plant,arrived there In lumps In 75 lb. paper bags, or as material which had been melted into 350 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-0763. The melted material was blown from there,by air pressure,to one of the chlorlnators. As far as possible, only the ohlorinator CT-0745 was used for the higher Aroolors, to prevent cross contamination of the different kinds of Aroolors. Before a ohlorinator 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 (N. Pt. 69*C.) 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 On the walls of the vessel, resulting in Incorrect charging of the ohlorinator. Handling of Chlorine At the Krummrloh plant, the Aroclor department Is supplied partly with revapourised liquid chlorine (the chlorine simply being allowed to evaporate Into the qgdorlne main, from the liquid chlorine store vessels which are sprayed with oold water; the vapourlzer CT-0743 Is no longer used), but the main supply Is direct cell gas, dried, and compressed to about 30 psig. Actually, the Aroclor plant is able to take all the "snift" gas, and low-grade chlorine generally, without 111 effect, though any considerable proportion of air In the chlorine may confuse the operator because the chlorlnators will not show a heat evolution corresponding to the flow of gas. Air dilution also Is detrimental In the HC1 absorbers. MONS 046017 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 vapourlzer, made from old gas cylinders set vertically In a water bath automatically controlled at about 95*0. The cell gas at Anniston Is compressed only to about 15 pslg, which Is Inconveniently near to the back pressure of a full chlorinator, so that the gradual Increase of head of material In the chlorinator a'S the volume and density of the charge Increase during the chlorination, necessitates clos* attention to the regulation of the flow of chlorine, and to the sharing of the chlorine between up to eight chlorlnators, some at different stages of chlorination. Ordinary ohlorine valves have been used for this regulation, but more recently, "Duroo" cocks, with Teflon lined bodies, and Durlmet plugs, have been found more convenient at Anniston. There are no flow meters on the chlorine feeds at Anniston, and the operator has. to be guided mdlnly by the temperature behaviour of each ohlorinatir. At the Krummrlch plant there is a branch from the ohlorine main for each of the five main chlorlnators (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 Ha30i| then there 1b 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 on the side of the chlorinator, where there Is another rising stem valve. The U tube ofthe H2SO4 manometer has a cross connection near the upper ends of the two legs, this oorineotlon being dosed by a stop cock (A) when the manometer Is In use. There are also two stop cooks (B is C)one at eaoh end of the U tube. When the flow of / MONS 046010 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 0 are opened, and A gradually closed. Between batohes, B and C are left closed, and A open. ,----------- ------ --------------------- 8c -* A See also the description of the flow controller to No. 5 chlorlnator on page XII-5 below. Chlorination The chlorination procedure is essentially the same for all Aroclors up to 68j< chlorine oontent, 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, beoause the lnorease in volume during chlorination is greater, also the time temperature schedule, and the end point of the ohlorination 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 100*C. gaining a little cooling effect, and so saving a little time. MONS 046019 i. wocna a amn. cent*, CBTfatTBATIOB BATC1 DATA lhtM flfBm rif to tbo itndii'd chlorlnetora 3*0" i.D. l6'0* 'deep. Taken nalnly fm Kyles, Soffreoko and Becker, Icfiatip 6, 19*6 and Tram Schwartlag and other*, 1953- Orhde of Aroclor 1221 Chars* Chlorination Diphenyl xie* Boiler cm* Distilled lb*. lbe. lb*. Bourn Chlorine ponemhitlon. lbe. T--pratar^ Final Sp. Sr. e. at *C. VelAt Produced Din tilled lbe. lbe. *000 MOO.^S- . 1 - 5 PInroDceesstail 1232 11*2, 12*2 1.118, 12*8 115*, 125* 1160, 1260 1162, 1262 1168, 1268 *000 *000 *000 3600 3600 3600 2800 1169, 1269 1170, 1270 1171, 1271 2565 *065, **65 5060,5*60 2800 2800 2800 1800 600 1800 1200 3600 *000 x ^0^ 12-1** 1 - 16^ 1 17 - SO* 18-22* 20-2* () 5735 6890 9550 10160 11089 10678 11*66 11950 88*9 10205 10062 120 to 135 120 to 135 120 to 150 120 to 150 120 to 150 or hleher 120 to 150 bat always 20-50* above the bold point ^ 1.3*2 to 1.3*6 65 l.*10 to l.*l* 65 1.502 to 1.506 65 1.558 to 1.562 90 1.566 to 1.572 100 1.570 then to hold point of 1*5 - 155*C. 100 , ae 1168 th<m finally to a bold fc - 195*C. - 120 to 175 i 1.500 &HJ than to softening point 68 - 70*C. 120 to 175 120 to 210 1.500 then to eoftenlng point 72 - 7**C. 1.500Al0*C. then to eoftening point 108 to 110*C. See page Tl - 26 for alight vari ation in cone of 8mh Unite. 6483 6600 7571 8227 8850 7800 8100 6100 "55RT 7725 7800 6165 6336 7200 78*5 8517 7000 *Ihe 195* operating instructions glee hboat 2 hoars lees ehlorlnetloe tine (external cooling of the circulation etreen). 7200 6800 Continue chlorinating in agitated chlor- Cootitme ehlorlnatlag in agitated chlor* etor to 290-295*C.. 2* bra. 220 - 32*C Continue chlorinating In agitated eh lor 6950 6200 * Calculated fraa Anniston Standards (a) The forenan, October 19*7, stated tl ehlorlaetion to reach a hold point ` 150* took 16 hrs. then a further chlorination In the agitated pot, t U71 end point, required 8 hr* .nor*. Overall tine cycles for the Arcelor: general ere given In the report of Kyles, Soffronko, Becker, iove*er page 16*. -- At the Kiumrleh plea the sparetore are given s table of dr. ranges a little nerroecr than t of the epecl fleettone (section iz b so as to leave a little argin for safety. HUNS O'*6020 vi - 6 Process In Detail VI. PROCESS IN DETAIL, contd. Chlorination, contd. Before a fresh charge Is put Into a chlorlnator, which has been emptied after a preceedlng batch, the chlorlnator Is allowed to cool to 150*C., 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 chlorlnator Is adjusted to 120"C. (Recent Instructions say 100C.) Circulation of Aroolor is started on whichever of the scrubbers CT-0759 etc. corresponds to the chlorlnator concerned, and the feed of water to the KC1 absorber Is adjusted to correspond to the expected flow of HC1, also cooling water as needed Is put on to the absorber, then chlorine Is admitted into the chlorlnator. 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 HC1 absorber Is kept closed until the diphenyl has been charged. Circulation of the charge In the chlorlnator 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 HC1 absorber, and the cooling capacity of the chlorlnator. 2" - 3" HgSO^ column^dlfferentlal on the 1.1" orifice Is a good starting rate, to be Increased as circumstances permit. See also the table on the next page mons 0460^1 VI. PROCESS IN DETAIL, contd. Chlorination, contd. VI - 6a Process In Detail lb.Cla /hr. Qauge 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 ll.l 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 9.4 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 H2S4 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, whloh appear In the column "Chlor. Back Press. PSIO" on the dally record sheets, refer to the off-gas pressure, sb discussed below, and, therefore,'refleot the working of the HCl absorbers, rather than that of the chlorlnators. Recent Kruimrlch 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 MONS 046022 VI. PROCESS IN DETAIL, cohtd. VI - 7 Process In Detail Chlorination, eontd. 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 speclflo 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 ohlorlnatlon to higher values, because the efficiency of absorption in the chlorlnator Is less,' and the ohlorlne passes through Into the scrubber, where It Is absorbed by the lighter Aroclor used for scrubbing. Ohlorlnatlon beyond 1162 was confined,as far as possible, to No. 1 chlorlnator to prevent eontiflllnation of liquid Aroclors with solid Aroolors. As the required test limit is approaohed, the oontrol tests are made at shorter Intervals,'and when the correct end-point Is reached, the ohlorlne feed Is stopped, the chlorlnator vent line is opened, the line to the HOI absorber closed, and the stream from the circulation pump diverted to the aeration vessel CT-0750 (for Aroclors up to and lnoludlng 1162). Aroclor 1168 went directly .to the vacuum still, the bottom outlet line from the chlorlnators being heated with gas flames, and formerly, when Aroclors containing more than 680 of ohlorlne were made, ohlorlnatlon would be carried to a hold point of 185 to 195*0. In the main chlorlnator, then the batch dropped to the "ohlorlnator pot" CT-0808, for further ohlorlnatlon, as indicated in the table on page VI-5, above. MQNS 046023 VI - 8 Process In Detail VI. PROCESS IN DETAIL, eontd. Chlorination, eontd. Eapeolal care is needed to prevent freezing during transfer of the higher Aroolora. Care muat be taken that the ohlorlnator vent is open and free when the ohlorlnator is being emptied, otherwise the batch may be con taminated with liquid sucked back from the'scrubbing system. The meroury manometer on the off-gas line will give an indication of any drop, in pressure in the ohlorlnator. Typleal record sheets are given at the end of this section. Chlorination beyond 6Qt, l.e. Ijor Aroclora 1169, 1170 and 1171 These products are no longer made, butt the following description of the former method of production may be of Interest. Chlorination was oarrled on in two stages, the first(in one of the ordinary chlorlnators as for Aroolor 1168, and the second stage in the gas heated, agitated ohlorlnator CT-0808. As the ohlorlnMlon in the main ohlorlnator passed beyond the 1168 stage, external gas flames on the ohlorlnator body fnd on the oirouletlng lines were needed to keep the charge always 25*C., or so, above the "hold" point, and the chlorination waa continued in the No. 1 ohlorlnator to a hold point of 185-195*. Towards the end of this stage, the gravity lines from No. 1 ohlorlnator to CT-0808 were checked to make sure they were dear, and -0808 cheeked to make sure there was room in it, then at the proper moaient' the charge was dropped to -0808, and the external flames kept on for about 5 minutes to drain the mainohlorlnator and the gravity lines. No. 1 ohlorlnator would not be recharged until it was oertaln that the gas heated ohlorlnator would be empty again in time to receive the next ohsrge, partly because the same scrubbing system served No. 1 ohlorlnator and the gas heated ohlorlnator. MONS 0460^4 VI. PROCESS IN DETAIL, contd VI - 9 Process In Detail Chlorination beyond 69jt, oontd. Chlorine was passed into CT-0B08,by way of a dip pipe,quickly enough to raise the hold point by about 15-20*C. per hour, the charge always being agitated and kept 25-50*C. above the hold point, until the final test was attained as set out on the table on page VI-5 for the different Aroolors. {The heat of reaction would usually main tain the temperature even with the furnaoe doors open, and the gas burners off. When the end point was reaohed, the burners would be put on to keep the charge molten, until It ftould be run off Into finished produot paokages, or Into the distillation pots of the solid Aroclor stills R-026 and 027, Ussarlteed' In Sectloj^xil, below. The off-gases from the gas fired ohlorlnator went through Inter ceptor CT-01258 to trap sublililng material, and then through the Aroolor sorubbera belonging to No. 1 ohlorlnator and so to the HC1 absorber. The Interceptor was oleaned after each second run, the oleanlngs being put Into CT-0808. ' Solid Aroolors . The gas fired ohlorlnator, CT-0808, and its ancillary1vessels, have been taken out, also the still R-026 eto., the flaker D-012, and the mill, MI,-045. The lean-to part of the building, whloh 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 Chlorlnatora In the early part of the chlorination, the off-gas,whloh leaves the ohlorlnator, carries the saturation amount of diphenyl, or light Aroolors, at about 150*$.i as the ohlorlnatlon prooeeds, there Is lesa of these materials In the vapour, but there will be heavier Aroolors, and as the ohlorlnatlon approaohes a high value, free ohlorlne will begin to come over. ' At the Anniston plant, the of?-gas handling Is simpler than at the Krummrloh plant, but It appears to be quite satisfactory. Usually there are two steel oyolones In series for eaoh ('air of chlorlnatora, (see sketch). The cyolones can be drained at Intervals Into opentopptd drums, and the material recycled. page VI-9a. MONS 046025 I CYCLONES or the CHLORINATOR VI - 9a Process In Detail OFF-GAS SYS TM ( Aroclors) An;;stci , March, 1955 i VI. PROCESS IN DETAIL, contd. VI - 10 Process In Detail Scrubbing of the Off-gas from tl^e Chlorlnatorg. eontd. At the Krummrloh 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 dona by passing the off-gas up one of the Raschlg columns CT-0759# -0760, -O76I, Q1014, or TW-0206, counter current to a 'Stream of light Aroclor circulated from one of the pump tanks CT-0754, -0755, -0756, 0968, -01013. See the sketch on page 10a Section VI. About a 3/4" 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 a|nd 1.400 at 63*0. (more recently the limits have been given as 1.325 - 1.450 at 65*0.), or if the volume increases too much,a note is made of the volume of liquid in the scrubber oiroulation tank, a sample is taken for specific gravity test, and the liquor Is dropped to chlorlnator No. 1, and the scrubbing system reoharged with fresh crude Aroclor of medium speol.flo- gravity. The weight of the discarded liquor Is calculated, and the % chlorine content read from the ourve of specific gravity vs. chlorine content on page III-15* see also pages VI-48 and 49. The equivalent amount of diphenyl ip oaloulated(assumlng theoretical chlorination), and the oharge matte up to the equivalent of a normal chlorination batch by the addltlpfl of fresh diphenyl. Pages VI-10b,c,d give" a ready reotoner'for the calculation of the gross weight and Ihe diphenyl equivalent of the liquor. In recjent years at the Krummrloh plant the heavier Aroclors have not been made, and the general tendency has been for the scrubber liquor to fall in density during use. The scrubbing liquor Is not heated while in use, unless It becomes too viscous. The gas leaving the scrubber passes through one of the oyolones CT-01279, -01280, -01281 etc. and so into a main leading to the HC1 absorbers,which are Just outside the south wall of the building. Any liquor collecting in the HC1 main drains to a drum outdoors. ' HONS 0C6027 8 ? 0 9 *0 SNOW VI. PROCESS IN DETAIL, contd. VI - 10b Process in Detail Dept. 246 Scrubber Liquor Diphenyl (8-15-46) The table below lists the approximate range of Sp. Or. of Aroclors that may be found In scrubber liquor. In addition to the Sp. Or. 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. Or. at 65*C. 1200 1225 1250 1275 1300 1.325 1.350 i;,375 1.400 Equivalent Aroclor 1126 1129 1132 1135 1138 1140 1142 1145 1147 Wt.Lb./U.S.Qal. 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 Oal. Heel 1" 2 3 4 5 0 7 8 9 10 11 12 730 745 760 776 791 806 822 837 852 73 540 529 5,17 504 490 484 *77 460 452 830 847 865 --552 900 917 935 951 969 83 6l4 601 5.88 573 558 550 542 523 513 930 9**9 970 ~935 1009 1028 1048 "IDES' 1086 93 688 ?P 65? 642 626 616 607 586 574 1030 1051 1075 109* 1118 1139 1161 "ITT? 1203 103 762 J*5 T3 711 694 682 672 649 635 113 1130 U?3 1180 1200 1227 125<5 1274 1293 1320 8J6 817 qoi 780 762 748 .737 712 696 125 1230 1255 1285 1306 1336 1361 1387 1407 1437 910 889 872 84? 830 814 802 775 757 133 1330 . 1357 1390 1412 1445 1472 1500 1521 1554 984 961 9*3- 918 896 880 867 838 818 143 1430 1459 1*95 1518 1554 T5S3 1613 T53J 1671 1058 10?? 1014 987 066 946 932 901 879 153 1530 1561 1800 1624 1663 1694 1726 * 1749 1788 1132 1105 1085. 1056 1034 1012 997 964 940 163 173 1630 1663 1206 1730 T1?15757 1280 1249 1705 1756 1810 1327 1730 1125 1836 1194 1772 1102 1881 1170 1805 1078 1916 1144 1839 ..1863 1062 1027 1952 ~I977 1127 1090 1905 1001 2022 1062 183 1830 1867 1915 19*2 1990 2027 2065 2091 2139 1354 1321 1298 1263 1238 1210 1192 1153 1123 193 1930 1969 2020 2048 2099 2138 2178 2205 2256 1428 1393 1369 1332 1306 1276 1257 1216 1184 * on each panel MQNS 046029 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 2173 2230 2260 2317 2360 2404 2433 2490 1576 1537 1511 1470 1442 6408 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 2446 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 i753 172^ 1677 1646 1606 1582 15?1 1489 18 253 2530 2581 2650 2684 2753 2804 2856 2889 2958 1872 igL 1795 1746 1714 1672 1647 1994 1550 19 263 2630 2683 2755 2790 2862 2915 2969 3003 3075 1946 1897 1866 1815 1782 1739 1712 1657 1611 20 273 2730 2785 2860 2896 2971 3026 3082 3117 3192 2020 1969 1937 1884 1850 1804 1777 1720 1672 21 283 2030 2887 ^905 3002 3080 3137 3195 3231 3309 2094 2041 2008 1953 1918 1870 1842 1783 1733 22 2930 2989" 3070 3108 3189 3248 3305" 3345 3426 293 2168 2113 2079 2022 i986 1936 1907 1846 1794 23 303 30?0 3091 317^ 321* 3298 3359 3421 w 3543 2242 2185 2150 2091 2054 2002 1972 1909 1855 24 313 3130 3193 3280 3320 3407 3470 3534 3573 3660 2316 2257 2221 2160 2122 2068 2037 1972 1916 25 323 3230 3295 3385 3426 3516 3581 3647 3687 3777 2390 2329 2292 2229 2190 2134 2102 2035 1977 26 3330 3397 3490 3532 3625 3692 "3700" 3801 3894 333 2464 2401 2363 2298 2258 2200 2167 2098 2038 27 343 3430 3499 3595 3638 3734 3803 3873 3915 4011 2538 247? 243^ 2367 2326 2266 2232 2161 2099 28 353 3530 3601 3700 3744 3843 3914 3986 4029 4128 2612 2525 255 2436 2394 2332 2297 2224 2160 29 363 3030 3703 3805 3850 3952 4025 4099 4143 4245 2666 2597 2576 2305 2462 2398 2362 2287 2221 30 373 3730 3805 3910 ^96 4061 4136 4212 *257 4362 2760 2669 2647 2574 2530 2464 2427 2350 2282 31 383 3830 3907 4015 4062 4170 4247 4325 *371 4479 2834 2741 2718 2643 2598 2530 2492 2413 2343 MONS 046030 T VI. PROCESS IN DETAIL, contd. VI - lOd Process in Dc t tJ X Dept.246 Scrubber Liquor Diphenyl (8-13-46). contd. 32 393 3930 4oog 4120 4168 4279 4358 4438 4485 4596 2908 2813 2789 2712 2666 2596 2?57 2476 2404 33 403 4030 4111 4225 4274 "4385" 4469 4551 4599 4713 2982 2885 2860 2781 2734 2662 2622 2539 2465 34 413 4130 4213 4330 4380 4497 4580 4864 **713 4830 3056 2957 2931 2850 2802 2728 2687 2602 2526 35 423 4230 4315 4435 "TO35 46o6 4691 wrr ' 4827 '4947 3130 3029 3002 2919 2870 2794 2752 2665 2587 36 "4330 4417 4540 4592 4715 4802 4890 4941 5064 433 3204 3101 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 "5530 33?2 4621 3245 4750 33i5 4804 3126 4933 "5024 3074 2992 5116 "5165" "5598 2947 2854 2770 39 463 4630 4723 1^5 4910 5042 5135 5229 "5283" 5*15 3426 ??17 32.86 319 3142 3058 3012 2917 2831 40 473 4730 4825 4960 5016 5151 5246 15W 5397 6532 3500 .3369 3357 3264 3210 3124 3077 2980 2892 41 483 4830 4927 5065 5122 5260 5357 . 5511 5649 3574 -3461 3428 3333 3278 .3190 3142 3043 2953 42 493 4930 5029 5170 5228 5369 5468 5568 155T 5766 3648 ..3533- 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 w 5690 5794" "5H5T 6000 3796 3677 3641 3540 3482 3388 3337 3232 3126 45 523 5230 5335 54&r 5546 5698 5801 5907 ~59&r 6ll7 3870- i3Iit9 37t12 3609 3550 3454 3402 3295 3187 46 5330 5437 5590 5652 5805 5912 6020 6081 "5234 533 3944 3821 3783 3678 3618 3520 3467 3358 3248 47 543 5430 5539 56195 5758 5914 6023 "5133" "3195" 6351 4018 3893 3^4 3747 3686 .3586 ???2 3421 3309 48 553 5530 5641 5800 5864 6023 6134 6246 6309 6"68 4092 3965 3925 3816 37?* 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 6O10 6076 6241 6356 6472 6537 6702 4240 4109 4q67 395* 3890 3784 3727 3610 3492 51 583 5830 5947 6115 6182 6350 6467 6585 6651 6819 4314 4l8l 4^38 4023 3??8 3850 3792 3673 3553 52 593 5930 6o49 6220 6288 6459 6578 6698 6765 6936 4388 4253 4209 4092 4026. 3916 3857 3736 3614 53 603 6030 6151 6325 6394 6568 6689 6811 "3579 7053 4462 Jt221 4280 4161 4094 3982 3922 3799 3675 MONS 046031 VI. PROCESS IN DETAIL, contd. VI - 11 Process in Detail HC1 absorption. The Aroclor department at the Krummrlch plant had a set of Silica tourllls and a Tantalum unit, used, more or less, in parallel. The feed of city water was hand controlled, through a Rotameter, to give 20.2'Bd acid measured at 65*C. The tourllls were cooled by being sprinkled externally with well water, and the Tantalum unit had well water through its Jacket. (las 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 chlorinators 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 tourllls on the HC1 off-gas line have been taken out, and a seoond 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 Cllffchar carbon are used for 3000 U. S. gallons of add, 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 acidsoaked Haveg could not be cemented. The various vessels have Pneumercator 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 chlorinator exits, combine into a header leading to a coke tower 4'0" diameter, 7'6" 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 whloh follows. In particular, a rubber-lined store tank for muriatic acid gave good service and was taken out for repairs only after IS 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 HONS 046032 VI. PROCESS IN DETAIL, contd. VI-12 Process In Detail 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 Rasohig 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 so to the aatch 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 20.8*Bd, 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. HCl 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" quality. Tor this treatment there is a rubber-lined pre-coat tank, a rubber lined treatment tank, an Adams filter with 18 tubes, a Karbate Wllfley pump, and various rubber-lined store tanks. Saran lining has not been so satisfactory. 10 to 15 pounds of Cellte are suspended in murlatlo add (or in water) in the pre-coat tank, pumped on to the tubes in the filter, then the oarbon-treated acid is pumped in without interrupting the flow, so that the cellte does not drop off the tubes. Any add produced in exoess of requirements is put, untreated, to the sewer, by way of a limestone pit, whloh also takes the spent carbon. , MONS 046033 VI. PROCESS IN DETAIL, contd. VI'-13 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) 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 highbollers, (2265 and 4065), and in addition the material from the scrubbers on the off-gas has to be worked up through the chlorlnators. it may contain some products derived from highbollers. In changing to 5060 from any of the other Aroclors, it is necessary to give the chlorlnator 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 0.3J< 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 Chlorlnator Charges, At the Krummrlch plant, the crude Aroclors are alr-blstss 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 of the building. At Anniston there are 3 air-blowing vessels, and the vent stacks are off-set frog the alr-blowlng vessels in two oases,so that nothing can drip back from them into the charges. The blowing vessel at the Krummrlch plant is large enough to contain 3 chlorlnator batches at one time, and it may be necessary to put MONS 046034 VI. PROCESS IN DETAIL, contd. VI - 14 Process in Detail Alr-blowlng of Chlorlnator charges, contd. unblown charges on top of blown material, In which case the air blowing must be repeated. The Steam oolls are not used during the alr-blowlng of Aroolors up to and Including 1148, but the higher Aroolors need temperatures of 140*C., or more, depending on their softening points. 80 pslg steam Is used In the coils for 2565 and 4065, but 200 pslg 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 needle of the pressure gauge on the alr-lnlet line will Indicate that air Is bubbling Into the veBBel. Aroolor 2565 Is not distilled, but is sampled In the alr-blowlng vessel, checked for add number and softening point, and if correct, is dropped directly into cans for sale. Distillation There are two vacuum stills for Aroclors at the Krummrlch plant, both being vertical steel cylinders 6'0" I.D., with bulged tops and bottoms, as detailed in section XII below. 3-043 is 5'6" deep on the straight side, and S-062 is 11'-10". Each still has the following fittingss -- 1. An external heating coll, set in a gas-fired furnace. 2. A submerged pump to circulate the charge through the coll and back to the still. The pump shaft has a water-cooled stuffing box, and there is an indicating ammeter on the driving motor. >. An Inlet with sight-feed coupling, for charges from the alrblowlng vessels CT-0750 and 0T-O2O86. 4. An Inlet from the chlorinators, normally blanked off. 5. A hand hole with a screw cap, for charging hydrated lime. MONS 046035 n. PROCESS IN DETAIL, oontd. VI- 15 Process In Detail Distillation, oontd. 6. {Formerly) Emergency lines to and from Aroclor store vessel CT-0749. 7. A Manlld 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. 11. A vapour outlet, to one of the condensers CT-0770 and 01378. 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 Krummrlch plant, the condsnser is cooled by distilled water, whloh is allowed to boil off into heat exohangers CT-O83 and 01491; the oondensate from the exchangers returning to the Aroclor condenaersby way of one of the buffer tanks CT-O766 and -01396. Wastage of the distilled water is made up by bleeding steam into the system at a convenient time. ' Formerly*!.for! the h&gher boiling Aroclors the distilled water was replaced by Aroclor 1242, circulated through the same system by pump P-OJ95. Each buffer tank has an internal coll 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 Aroolor circulation system was out of use in 1955, because higher Aroolors were no longer being made at the Krummrlch plant. The Aroclor oondensers lead to the vacuum receivers CT-0771, -01377, whloh have the usual fittings, including a connection to the 3-stage vacuum Jets MSC-O76O, -01392, -01685 by way of the coke scrubbers CT-0753 and -01396. HONS 046036 VI. PROCESS IN DETAIL, contd. VI - IS Process lr. Detal1 Distillation, contd. Although still S-062 at the Krummrlch plant Is about twice as deep as S-043, It Is given only the same charge (about 10,000 pounds) of crude Aroclor. The greater depth of S-062 was designed only to give more disengagement space for the vapour. See the comments on this feature under Item S-043 In Section XII below. The charge Is sucked to either still, or is pumped by P-0580 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 30 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 glv 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 musb also use Judgment in controlling the distillation. The higher Aroclors require considerably more gas. Cooling of the condenser Is not started until the distillation ha3 well commenced, because over-cooling of the first distillate might cause blockage with frozen, or very vlscou3, material. Judgmen*: 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. Typlcai record charts are given at the end of this section. M0NS 046037 T VI; PROCESS IN DETAIL, contd. VI 17 Process In Detail 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 coll Inlet and outlet, or between the coll Inlet and the vapour outlet from the still; about a 40*C. spread through the coll 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 *t 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, ork least blocked with coke. If the ammeter Indicates overloading. Borne 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 k#ep the "heel" of residue hot enough to circulate freely without coking in the coll; 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 gas 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 pesldue 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. gallonsJn the still. To stop the distillation, a little air Is admitted to the still. MGNS 046038 T VI. PROCESS IN DETAIL, contd. VI - 18 Process in Detail Distillation, contd. The outlet cook Is heated. In good time, with a gas flame, a little air sucked m 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 glvesoff 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 Bale 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 freezo. 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 batoh has been well worked down In the still (temperature spread in the ooll at least 35C.). 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 oouplee at the Inlet and outlet of the coll should show the same temperature -- this checks t.hem 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, bo that the pump circulation must stop, the heating coll must be sucked empty. "Sb 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 arrsmgement, air can be pulled into the still In either direction along the pump circuit. MGNS 046039 VI. PROCESS IN DETAIL, oontd. vi - ig Process lr. Detail Distillation, oontd. The shallower still, S-043, Is being worked semi-continuously at the Kruimnrioh plant, but there is very little to add to the des cription of continuous working, as given In my report of March 29, 19557 on the Anniston visit. The material Is continuously moved from the alr-blowlng vessel to the still by the vaouum 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, 2i" deep., of steel plate, with i" 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 oolls are of 2" pipe. It Is doubted if the Anniston 3" colls offer more surface, because, of course, the turns of the 2" oolls oan be at closer pitoh. 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 Krummrlch plant are worked at the highest available vacuum. 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 coll, 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. HONS 046040 VI. PROCESS IN DETAIL, contd. VI - 20 Process in Detail Distillation, contd. At Anniston there are two vacuum stills, each of the shallower type, 6'0" In diameter, 5'-6" deep on the straight side, like S-043 at the Krummrlch plant, and the heating and condensing arrangements are generally similar to those at the Krunmrich plant (vertical monel condensers, cooled only by recycled distilled water). The submerged pumps now used In the stills are Taber pumps with 3" outlets, and the furnace colls are of 3" piping, nine turns at 5" pitch, 24" diameter, to centres. Each coll stands on four short legs on the bottom of the furnace, and there are short steel distance pieces welded between the turns of coll 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 coll, 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 coll, upwards through the coil, then back to the still, by a pipe projecting Just through the cover. The lowest turn of the coll Is the only part which bums 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 (lj"), 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, 7'0" 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 sketoh).* ' * page VI - 20a. MONS 046041 u. MONS 046042 I VI. PROCESS IN DETAIL, contd. VI 31 Process in 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 oondenser shell by a lj" valve bye-passed by a i" line having a fc" 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 exohanger 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 atmospheric pressure. Even so, some skill it required to get proper condensation of the Aroclor without ooollng bo far as to freeze the heavier Aro- clors In the condensers. Each of the two vacuum still receivers at the Anniston plant has a sight glass In the oover, 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 11'O'1 below the bottom of the receiver. This 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 eame pump serves the receivers of both etllls. By using this pump without stopping the still, it is possible to work the still In a semi-continuous manner. Instead of purely batchwise, so a level controller has been fitted through the cover of each still,, and the crude Aroclor la 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 MQNS 046043 VI Pro; e De t a l VI. PROCESS IN DETAIL, contd. Distillation, oontd. 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 whioh the still bottoms are tapped, are placed on the ground floor, under a steel canopy, about 8'0" diameter, coming down to about 3'0" from the ground, and connected to a powerful exhaust fan. There is a canopy under eaoh 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 batohes, 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 3ame 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 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 gcod a vacuum as could be obtained with the four-stage Jet, but at MONS 0^60*^ VI - 23 Process In Detail VI. PROCESS IN DETAIL, eontd. Distillation, eontd. Anniston It has been found better, and more economical In steam, to use only a two-stage Jet for some of the Aroclors, for example: ~ Aroclor 1260 1250 1242 1248 (probably) 1268 4465 5442 5460 m.m. Hg In the receivers recommended 30 30 30 30 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. <n. for 5460. The temperature "spread" between the Inlet and outlet of the heating coll, of course, determines the heat Input to the still, for any given rate of pumping. Uhder the present conditions at Anniston,the spread Is about 8 to 12*C., widening towards the end of a run. For the continuous working,the spread usually runs between 8 and 10*C. HONS 0A6Q45 yj. PROCESS IN DETAIL, contd. VI 24 Process lr. Detsl1 Distillation of Solid AroclorB. Sea also I<yles, Soffranko and Becker, November 1947, pages 6l-and 97-, In spite of Its high melting point, when Arodor 1268 was made, the distillation was done In the ordinary vacuum stills, as with tne lower Aroclors, but with greater precautions against freezing in the pipe lines etc. 1169, 1170 and 1171, as formerly made, were kept hot in the gas fired chlorlnator CT-0808, and drawn off In portions Into retort pots R-026. and 027. The pots were placed in turn, on a rail cart, on a weighing scale, under the bottom outlet of the chlorlnator, the outlet llr.e heated with a gas flame, 30 lbs, of lime put in the pot, and about500 lbs. (600 lbs. In 19^7) of the hot Aroolor added, a (vented) ltd 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 Aroolor, which distilled up on to the upper part of the wall. A pipe connection from this channel. Into the pan of the flaker 0-012, was made after the pot was In position. The pots were gas heatsd, a pre-run cut being diverted to a drum, then the sain out 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 chlorlnator, and the main out was flaked, t'he 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 dlstlllatioryindicated 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 VI-24a. MONS 046046 VI - 24a Process Seotlon A-A HONS 046047 VI. PROCESS IN DETAIL, contd. Distillation of Solid Aroclors, contd. VI - 25 Process in Detali 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 Lt round the elevator, then sampled for the control lab. When approved, lt 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, lt 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 lt through to clear the system. The distillate 1b 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 Krummrlch plant, the heel now Is usually left In the still, .gven If a different Aroclor Is to be distilled, the first two chlorinatlons being carried Just a little further, If a heavy Aroclor Is to be charged on the bottoms from a light Arocicr, 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 la 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 coll 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. MONS 046048 VI. PROCESS IN DETAIL, contd Changing from One Aroclor to Another, contd. VI - 26 Process In Detail AROCLOR TO BE MADE: 1142 Heel remaining from 1142 usual 1148 usual 1154 usual 1160 -0.001 1162 -0.003 Temperature at which Sp. Or. Is measured j V I 65 *C. 1148 1154 1160 1162 Specific Gravity to be attained + 0.003 usual - 0.001 '- 0.003 -0.005 + 0.002 + 0.003 + 0.001 + 0.001 usual - 0.001 usual usual -0.003 - 0.003 +0.005 +0.003 +0.001 usual usual 65 *C. 65 *C. 90 *C. 100*C. A + sign means that the chlorination should be carried a little further than usual, and - a - sign means tha* the' chlorination should be stopped a little short, for example + 0.005 above means that the 1163 should be finished at 1.574 to 1.576 instead of at 1.570 as given on page VI-5, below, and - 0.005 moans that the 1148 should be finished at 1.406 to 1.408, Instead of at 1,410 to 1.414. HONS 006049 VI. PROCESS IN DETAIL, oontd. VI - 2/ Process In Detail Treatment of the Distilled Aroplora. Prom the still receivers at the Krummrlch plant,the Aroclors up to and including 1262 are moyefl by pumps P-0565 and-01037, to the blending tanks CT-0779 and 01399 for treatment with Attapulgus earth, mainly to remove traoes of HC1. If the distillate contains moisture. It Is warmed and alr-blowr to remove the moisture, before the earth Is added. ThO 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 lev*l, and supplies of dried earth are sometimes drawn from Anniston, where the drying Is done In an eleotrioally heated tray dryer. The normal dosage of earth is 10 pounds for the distillate from 2 distillation batches, eaoh 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 Aroalor. The earth is added, by hand, from a bucket or sooop. The Aroclor and the earth are agitated together for. 4 hours, the temperature being raised to 150*C. 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 aotlon, and the batch Is recycled through filter P-0238 (formerly the smaller filter P-0172) until clear, (about hour), then the stream of the filtrate Is tumad to one of the filtrate receivers CT-0780 and-0l400, a half gallon sample of filtrate being taken In a hot dry sample Jar for the control laboratory. Plltration 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, P-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-Aroolor blends. These blends are made up In the Aroclor finished product vessels CT-0780 or CT-01400, rather than In the Pyranol mixers, see page VI-29. The Krummrloh plant were depending on supplies of thoroughly dried Attapulgus Barth from the Anniston electrically heated oven. MONS 046050 VI. PROCESS IN DETAIL, contd. VT 2H frc ' In Detail Treatment of the Dlatllled Aroclora, 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 0. E. apprdval, the filtered Aroclor may be moved to finished product containers, or to store tanks CT-0768, 0769, 01310. If 0. E. approval is required, a fresh sample is taken from the bulked material in the store tank. At Anniston a Sparkler filter 30* 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 baok 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 85*C.), before use, In an oven, and there Is one compartment In the oven for storing the dipper and funnel used for sampling Aroolors, also the sankple 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. HONS 046051 T VI - -J -j Process in Detail VI. PROCESS IN DETAIL, oontd. Treatment of the Distilled Arqclors, oontd. Aroolors 4465 and 5465 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". Thw 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-0780 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 detarmination of specific gravity, and the com position adjusted. If neoessarjr, as indicated by the following charts, pages VI-30 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 Aroolors. See also MCC report 171-4013, "Aroclor 5460 - Toluene mixture MONS 046052 Process In  mm co. k-6567 Process In VI. PROCESS IN DETAIL, contd. VI .... P w::s5: ir Detr..U Blending for Pyrancls. The compositions of the different Pyranols (Pyroclors, Inerteens, Askareis) are given on page 4, section I, above. Pyranol 1467 Is the main product, 1481 Is blended only In relatively small batches (2100 0. 3. gallons). The main components are Aroclor 1254 or 1260, and trichloro benzene, or a trl-tetra chlorobenzene mixture. The Aroclors used are made by MCC, and so Is most of the trichlorobenzene, but the trl-tetra mixture Is bought from the Hooker Chemical Company. The "chloride scavengers", tln-tetraphenyl and glycidyl phenyl either, are purchased, but the tln-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 corrcslon tests discussed In Sections. VII and IX, below. Bulk quantities of the Aroolor 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 80*C. (or even through the materials after blending). The Aroolor may be treated agqln with Attapulgus Earth to lower the chloride test figure. Alr-blowlng 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 la 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 MQNS 046055 T VI. PROCESS IN DETAIL, conrd. VI r ro' "3 1 Detail Blending for Pycanolaj oontd. proportion of Aroclor to trl- or tri-telra-c.hlorbenzene. 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 baton, 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 everthlng 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 neceasary, for submission to the customers. For blending with tlntetraphenyl, it is usual to agitate the batch at about 50"0. to make sure the TTP goes into solution. When the bulk Is known to be satis factory, it is filtered into 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 73 and 852, size 12, for the General Electric press type FP-30. It is said to remove traces of moisture and inorganic chlorides, even without the help of Attapuigu? Earth. All possible care should be taken to have the batch correct before ar.y 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 pre3enoe of scavenger also complicates the"corrosion" test as discussed in Section VII, pages 12--, and Section IX, page l3l Traces of Attapulgus earth which have carried through to the finished product amy interfere with the test for inorganic chlorides, ee page IX-lSi. M0NS 046056 VI - 34 Process in Detail VI. PROCESS IN DETAIL, contd. Packing The finished Aroclcrs are nyi 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 Aroolors, 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 Krummrlch 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 1951, page 108 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 Aroelor 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 any 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 & Casket Co. to the Krummrlch 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 Krummrlch plant; one a patent list label, and the other a warning label on toxicity. The effeot of exposure of Aroolors to metal contact is discussed in Section VII, comments, page 17 below. Generally speaking, the distilled Aroclors are packed in galvanized drums, the undlstllled 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. MONS 046057 VI. PROCESS IN DETAIL, contd. VI - >5 Process In Detail Packing, contd. Since the Aroclors 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, DP 5V26/7 and DP 5V277/6 and 1152 DP 4/16/7 and 8 July 1954, etc., also the Section III, Physical Sc Chemical data, above. Drums for electrical grades of Aroolors are not painted. Newport Plant Technical Committee meeting, April 14, 1953, page 2, reported some promising teste 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 Krummrlch plant the manhole of the oar Is protected by a tarpaulin tent during filling. Newport plant report for July 1954 mentions the Installation of tank-filling facilities. The Krummrlch plant operating Instructions, August 10, 1954 mention that rail oars for Pyranols and Aroclors are Insulated and have either a steam coll 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 pleoe fitting carrying air valve, dip pipe, release valve and pressure gauge, for use on rail tanks. It Is Important to drain the coll or Jacket of the rail tank In cold weather. Qalvanlzed or lacquered drums are used for Pyranols. MONS 046058 T VI. PROCESS IN DETAIL, c-ontd. VI 36 Process In Detail Operating Records. The following pages, VI-37 to VI-46, show typical Kruminrlch 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-4o to VI-44. Also shown m this section Is a sheet giving Dept. D-2l8 Muriatic Acid, Acid Receiving, Treatment and Piltratlon Batch Data, on page VI-45, and page VI-46 Is an example of a Pyranol Batch Record Sheet. See alBO Operating Records, pages25b-, of the "Notes on the Plant 'B1 Process", Mather, April 1947. A list of transferB(ihlorlnatcrs to air-blowing etc. etc.) also Is made eaoh day. HONS 046059 CHLORINATION RECORD - D.pt 246 Air Inr No. Chloimoioi N#, 1154 223 3 Cl..rq B,r*"|.l._J6DO// . . ...... dm.a. Oparolot Slotted Boland Fm.shed Tennyson e>2 Total Hrt 2^*30 |n5. t0 Gos Hf$ Ins. in Scrubber r- U 8:301 / 7:00] vi - a Process in Detail Batch Mo. Co** 3-31-38 4-1-33 Tank Iff C o/- 1.01* GPPUSrAIGO* ol,i 10:00 26 TC 120 u? FRooot*d "MU CPUho,*lco,k,r.* PSIG CMor Fd Roto H I l|f. 36 350 SpH, Oolrd. P*, c Soft Pi. -- lltOO 27 12:00 27 112 112 36 36 350 oOt O -- __ 1:00 27 115 3 6 300 -- 2:00 27 115 3 6 300 10.76 - 65 3:00 27 114 3 6 300 4:00 24 114 3 9 300 L210-- 63 5:00 27 114 3 9 350 0:00 7:00 8:00 27 23 23 114 116 116 39 38 36 290______ 1256 - 65 400 400 1295 - 65 9:00 Busy sc rul bers 10:00 24 120 3 8 400 1338 - 65 11:00 12:00 27 121 123 3 fl, 3* 8 400______ 450 1374 - 65 1:00 25 134 9 475 2:00 2? 136 3* 9 475 1410 - 65 3:00 Pfi 133 H 9 4:00 Bus y 5:00 27 144 3i 10 6:00 26 150 3i 11 _ 475 500 500 1485 - 65 And !'* - 60 r r Unit HA6B70coUi*dFnit I- m * ."e pat u VI- 6a. HONS 04 ______ 1______ |,, ...... 6'clor No, 111*8 Ripli*nyl L'M.",. . CHLORINATION RECORD Dtp* lit CMotmotor No, Op.,otf 165 CHoig* 3 Started Robinson Finished Edmonds - Wyatt Cl2 '* .. Total Hr* 12.2S In*. to Gat Hr* Ins. in Scrubber VI - 5b Process in Detail 9:15' / 10:3 / 0,1. 5-10-55 5-11-55 Tonk ti tt r Qr. CPPUSroIGGo.t 11:00 30 13:00 16 T*C 135 130 FPC#elet!ed `Ho Ch lor PPBSarIocGhti. Chlor Pood Roto 0 1 Hr. 3i 9 3i 8 450 450 1:00 Bus V 2:00 16 126 4 8 475 3:00 30 130 4 8 475 4:00 20 5:00 33 138 4 135 4 8 8 475 475 6:00 22 135. 4 7:00 B u E ,Y 8:00 30 134 4 9:00 34 140 4 10:00 34 139 4 10:30 F1n1 aht 8 8 8 8 d a' 475 475 475 475 10:30 . SoHS. oG*fltdr. PPt.t. C Ac.d n6(30t,UP*n.t ASc* id* 60 * F If7 Unit 1.176 - 90 1*240-90 1.288 - 90 1.333 - 90 1.380 - 90 1.416 - 65 Swltc tied * o 11 6. Finished at 10:30. Holt inn : or room. tONS 0460 41 T ... 1 CHLORINATION RECORD 0 41 CMafinotof N#, 1160 414 Started 5: ' Finished Charf* Cl2 fitphenyl 3600 i.in.n, lotot H* Go Hm 246 Operator Robinson Boland In*. to ln. in Scrubber T<* a* pm 4 00 / 11:0C / VI - < Proces j Deta.t 1 OolcH No. l'*<. 4-26-55 4-27-53 ^onfc sr........- i,.,,* CIl'S.IA~ICG*a.i T<*C 6:00 26 124 7:00 26 125 8:00 27 126 y:00 27 120 10:00 27 127 11:00 2'j 137 12:00 1:00 2:00 3:00 23 22 22 19 136 138 145 140 4:00 B u s y !>:00 21 141 6:00 7:00 8:00 9:00 10:00 11:00 16 18 22 22 22 21 135 135 133 137 140 150 Fc'#8 PotO "<1 CPPDhifol*GiceMkf . Chlof Rofe f \ M. 4 4 4 4 4 1.246 - 90 4 4 1.309 - 90 4 4 1.367 - 90 4 4 4 4 4 1.505 - 90 4 4 1.538 - 90 4 Finished %pHJ. c0hM,.RPt.t. ftc AcM T*f0lvUrl Ac itf Sj/, L--------------------| .... 1 1 1 1! t MGNS 046062 KRUWIRICH PLANT BATCH DISTILLATION VI - 40 Process In Detail 16I.'. kmi- DEPT 246 STILL RECORD Ar.lm. lg4g Botch M..___ __ still No. StoMtd By Finlthyd By Robinson C&rnl&l (NS FROM BLOW TK STILL OUTAGE IN . TIME 1:00904rk 4:00 DATE 4-17 - 55 4-17 - 55 CHARGE TOTAL HRS STILL BOTTOMS LBS NO BTCHS (* ORG RES LIME LBS 46" e c @ C 15.00 psig nm t Bwm> T*my#ftur* 0 C Con4. T*m R*e Still Ejaciar Flow 1 7 3 4 Rtt . Vayot Inlat Owtlat Wata REMARKS 88 4:00 6 5:00 / 6:00 / 7:00 'v 8:00 V9:00 10:00 / 11:00 y 12:00 / 1:00 / 2:00 / / F 8 // // / l/ // // // y/ / V / / 'i 1n 2? ,/ / </ / / / / ./ h ?5 / / / / / L. / / / 1/ // / yL. vi_ yL. ' / ed 5 50 / 68 / 58 / 58 / 58 / 58 *L- 58 V 56 / 55 / 53 / 53 52 51 160 163 165 166 168 169 171 170 170 175 ML 180 184 h-> W CO VjJ 166 172 175 178 180 182 183 186 187 192 201 04 r0 171 on 177 / 180 / 183 185 / 187 / 188 / 188 / 189 jL____ 194 / 197 207 / 257 off MONS 046063 T KRUMMR2CH PLANT -- Semi-continuous Distillation VI - 41 Process In Detail I- DEPT 244 STILL RECORD At.Ut H.. *242 B.,c|, M>, 18 TIMf DATE x Starts ty Edmonds - Wyatt 3 too ..jk 4-20-55 Fli>Uh*d By INS PROM BLOW TK t50" 1 .c limHapVMVWM Tli** Rh Still 3:00 6 8 STILL OUTAGE IN. 8:35 Charge 4-24-55 TOTAL HRS STILL BOTTOM* LBS NO BTCHS *ftr DBG RES LIME LBS a c 89.50 200 Sheet No. I (of 4 sheets) E|ctor Fl*w 1 2 3 4 Rm 175 30 10 6 6 5 ^2 TmftMlvrn * C V9r Iftlof OwtUt 167 180 187 WC**tn*r4. on REMARKS 6iOO / / 7 tOO 8 tOO / // 9tOO 10(00 / // 11 too / 12100 / // // 1:00 / 2lOO / // // 5 tOO / 4 tOO / // // 5:00 / 6t00 / // // 7 tOO / 8:00 / y // 9:00 / lOiOO / // // 11:00 / 12:00 / / // 1:00 / 2:00 / // // 9:00 / 4:00 / // // 5:00 / 6:00 / // // 7 i9 _*L_ JL-- / / / / / 61 165 178 185 / 38 165 178 185 / / r' / / / 54 165 178 185 y S3 165 178 185 / E' / / / V 165 178 185 / y V 50 167 180 186 / y/ / / / 50 167 180 186 / y / / / 50 167 180 186 / / / / / / 5P 168 181 187 y y/ / / / 50 168 l8l 187 / y/ ' / / 50 168 181 187 / 1 1242 Pumped ree.Away / ' / / / 49 169 182 188 / / / / / / 4 i 170 183 189 / / ' / / 4$ / : 7 / / "P 170 183 I89 170 182 189 / / / ' / / / 4|t 171 183 189 / / / / 171 184 190 / / 1 / / / 4? / 1 / / / *P y/ / / / 49 / / / / / 5P 170 184 189 170 184 189 170 184 189 171 184 I89 / / / / / / / / 50 171 184 189 / / / / / 5f> 171 183 191 / y/ / / / / 50 171 185 191 / / /// 5 171 185 191 / / J- uL y- 5C-- ILL- 183- 131 j.-- HONS 046064 vi - 4a Process In Detail I.. muiiM DEPT 246 Storf4 By STILL RECORD Ard.r N.Botch No.Still No. ---------TIK|-------------- CATE 4m pm Finished By m pm INI FROM BLOW TK 0 *c ------- 7 Tim* R* Still 8i00 9:00 IOiOO lliOO 12:00 1:00 2:00 6 / // / / 8 J / / / / / 5:00 4:00 5:00 6:00 / / / / / / / / 7:00 8:00 9:00 10:00 / / / / / / / / 11:00 12:00 1:00 2:00 5:00 4:00 5:00 6:00 7:00 8:00 9:00 10:00 11:00 / / / / // / / / / / / // / / // // // / / J STILL OUTAGE IN. TOTAL HRS STILL BOTTOMS LBS MO BTCHS *fl* ORG RES LIME LBS a c SHEET NO. II (of 4 sheets) E|*ct* Flew i BvmmMl------------1 2 3 4 R*c 4--~7T-7TV--------------1- V*pe |nl*t OvM* WC*tnMr . REMARKS 175 50 10 6 6 5 p 171 185 190 on y / / y y y 49 170 184 189 / y/ / y y / 49 170 184 189 / / y/ y y y y / y y y ^9 170 184 189 / 48 170 184 189 y y y y y/ / y y y/ / y k>7 170 185 190 / *7 170 184 190 / 1 1242 // / y yy y *7 170 184 190 / y / y y /47 170 184 190 / / // yy y y yy y y 47 47 /170 184 190 / 170 184 189 ,/ / y y y / 47 170 184 190 / / z_ y / z y 48 170 184 190 / / / / y y y y 48 / y y y 48 171 185 191 171 185 191 / / y y y y 48 171 185 190 / / / / y y y 45 171 185 191 / // y y y y 45 Z y y y 46 171 187 192 171 186 191 / / / // y y y y 45 172 187 192 / y / y y 48 172 187 195 / / y y y y 49 172 187 195 / y y / y y ? /172 187 195 y y / y y yy y y 49 4? 172 187 195 172 187 195 y / /y y/ y/ yy yy y y 49 49 172 189 195 172 189 195 / / / y y Zy y /172 189 195 Pumped rec.Away MONS 046065 T VI - 43 Process In Detail Storied By DEPT 246 STILL RECORD 18rclW.. lg4g Batch N. Still M.. 1 -------------------------------5Tfl----------------------------------- n pm Finished By *ih i M8ii sra* tk STILL OUTAGE IN. 4R pi CHAIlfri TOTAL HRS jVlU. BOTTOMS LOS HO 8TCH4 ofter DRO RES LIME LM < *c *c SHEET NO. Ill (of 4 aht) ------- 7KINK SlMRttl T W4flWM * C Time Roe Still E|eeter Flow 1 2 3 4 "t Veper Inlet Outlet Veter 12 >00 liOO 2:00 6 / / 8 175 25 5 5 5 5 / yy y y y y / y 49 y y y y *9 172 189 173 189 189 189 195 195 195 on y y 3:00 / 4:00 / /y /y y/ yy yy yy y / 49 50 172 189 195 172 189 195 y y 5:00 / 6:00 / /y /y yy y y yy yy yy 50 51 172 189 195 172 189 195 y y 7:00 / 6:00 / 1/ y /y yy y y y y 51 172 190 196 y y y y 51 172 190 196 y y 9:00 / 10:00 / /y /y yy y y y y yy yy 50 49 172 190 .96 172 190 196 y y 11:00 / 12:00 / / y y n/ y y y 49 172 190 196 y y y y/ / / *9 172 190 196 y y 1:00 / 2:00 / y y y y y y y 49 172 190 196 / y / y y y y 49 172 190 196 y y 3:00 / 4:00 / / / yy y y y y y y 48 172 191 197 y 7 / y 50 172 191 197 yy 5:00 / 6:00 / y y y y y/ y y y/ / / / 50 172 192 195 / 5 172 190 195 y y 7:00 / 8:00 / y y y y y y y 48 170 190 195 y y y y y y/ 48 170 190 195 y y 9:00 / 10:00 / yy yy yy y y y y 48 169 189 195 y y y/ 48 169 190 196 yy 11:00 / 12:00 yy yy yy yy yy yy yy 48 48 169 190 196 170 190 196 yy 1:00 J 2:00 / yy y y y y y y y y 48 171 196 196 y y y/ 48 171 191 196 yy REMARKS Puapad no.Away 1242 3:00 J-- _y_ ^L_ j-- y 48 171 12L_ 196-- _y_ HONS 046066 f VI - *4 Process In Oetsll L miain. DEPT 246 Started By STILL RECORD Attl N. Tit am *m 1242 Botch H. 18______Still H*.__ ^ BTfl Flnl*h*4By Boland (NS FROM BLOW TK STILL OUTAGE IN. 8:35 " f* ____________ 4-24-55_____________________________________________ 6i|roi TOTAL HRS ' STILL BOTTOMS LBS NO BTCHS *ft*r ORC RES LIME LBS 9 "C e c SHEET WO. IV (of 4 sheets) Tin* Vacuum Burners R* Still E|ct*r Flaw 1 2 i 4 R*c Tm*M*lwss 0 C V*p*r Mat Outlet WCa*tne4r REMARKS 4|00 7 too 8t00 8i35 6 8 1Z_ A. A A. 5 J!Z_ 172 192 197 on Plumed a*ay / i/ // / / / / 47 172 192 198 / y / / / / 58 175 200 308 / at 4:}o a.n. / auto, off //// /// / / h 52 177 306 212 / 49 186 230 240 / / r 1 n 1 s h 1 49 190 246 255 off 1 Osu i 88 HONS 046067 DEPT. D-218, MURIATIC ACTD ACID RECHIVINO. TREATMENT AND FILTRATION BATCH DATA CARBON BATCH NO--2----------ACID BATCH NO. 318 Date: VI - 45 Process In Detail 1955 Time flow started to _2_ Receiver 8:10 pm. Operator! Maclln A. Hourly Readings TTMR INCHES OPERATOR TANKS WASHED BY OPER. TIME 10100 Dm 26" Macip.n_____ 12:00 mn 35" Moespr 2:00 am 4:00 am 45" 55" Moessr MoesSr 6:00 am 69" Moessr carbon added 8:00 am 69" '>? Hall 10:00 am 79" Hall 12:00 pm Hall 2:00 pm 89" by stick Hall 4:00 pm 89" by stlok Hall 6:00 Pm 90" Hall 8:00 pm 93"gage Hall 9:00 pm 96"gage Haip. xx xx Time Start Stirring 9i00 PM Peer. Hall Bid 9;30 PM Peer. Hall Sattllng Time XX XX- Time Finished 9:50(5-12-55)PM AM Time Start Filtering 9i30PM (5-12-55) Oper Fin.PM Oper. ACID ANALYSIS AND ADJUSTMENT Be at 60*F. i/ After J Pals. Water added. Be t/ Color____ Lab. Report St Final analysis - Color J AM Be J_______ Color / Time pumping to # / Stg. ___ _________ PM Oper. i/ Oper.\_ AM Time finished J PM Oper. ______ ________________ (SONS 046068 VI - 46 Process In Detail PYRANOL pATCH RECORD SHEET Batch No. 27 Iner PPO Lot No. i^-1813 Pumped TcB to Mix Tk.#l To 1070ut Prom Car No. _________ Prom #6 Stg. B.P._2fi, A.P.14" Pumped Aroclor 1260 to Mix Tk.#l ' to fin "out No. 5 Stg. B.P. 72" A.P. 36$ 1st. Sample to Lab at ______ __ TIMEDATEOPERATOR 7:45 pm May 10/55 "Mac" 11<30 Dm May 10/55 "Mac" 1:45_.-Bm_____May 10/55_____Moeser So. Or. Ref.2nd HaO Sh--------- 1-567 Added 1.6160 "1260 at .0010 L| - 10 No. 6 Stg.. B.P. A. P. , Added 2 "TcB at 4:45 am #6 Stg. B.P. 14"A P. jLO" MIX Tk . B.P. A .P. Sample to Lab at 7:00 am So. Or. Ref. 2nd NaO CL No. StK. B.P.~ A.P. Mix Tk B.P. A.P. . Added "ToB at #6 Stg. B.P. Mix Tk. B.P. Sample to Lab at Sp. Or. 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.Y.F.D. Mix Tk. Sampled by Lab. at 11>3^ am PPO Is OX Moeser Moeser Moeser Added 1 bucket of Att earth 10# |;|6ama%-?f-55 Hall 11:30 am 5-11-55 Hall HONS 046069 r VI. PROCESS IN DETAIL, contd. VI - 46a Process in Detail Process Records, Krummrlch Plapt Daily Inventory At 7:00 a.m. each working day a "Dally 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 ohlorlnators alrblowlng 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 reoeipts 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. HONS 046070 VI. PROCESS IN DETAIL, contd. vi - 47 Process in Detail Monthly Inventory The usual measurements of tank contents, temperatures, densities eto. are made. Prom the densities of the chlorlnfttor batches at the time the Inventory is taken, it is possible to calculate from the curves on pages III-15 and VI-48 and VI - 4p, how much chlorine is still required to finish the batches, and the batches are then evaluated as if their oontents of diphenyl had been carried through to crude Aroolor, with a deduction for the chlorine still needed. Other materials in prooess 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. MONS 046071 VI. PROCESS IN DETAIL, contd Dept, 246 Monthly Inventory Pooda In Process - Aroclor (| A.M. vi - 50 Process In Detail 3hlor. Batch Diphenyl Sp. No. No. pounds Or. Charged Temp. Equlv. *C. Arcelor 1 BSnpty 2 641 3600 3 Empty 4 Empty 1.366 90 1145 (45.6 $ci) Finished Lbs .Cls Aroclor required to be Finish Equlv.Lbs. of Finished Aroclor 1260 . (i) 5000 (2) 7800 .__3600 0.4385"9^ recovery (1) Prom curves attached, pages IJI-15, and VI-49. (a) From table attached, page X-lSb. * Notes Mr. Purzey reported Dec.11/51 that the distillation yield was 'about 95$ at the Krummrlch plant and a little higher at Anniston. Tank No. Batch No. Type Aroclor Ins. Out age u.s. Pals. Sp. Or. Temp. *C. Lbs. H-- Per US Recov lalion ery Total Lbs. Recovered Blew Tank 640 1160 Old Still Empty 2?n, 651 1.525 at 120 12.7 95 7854 New Still 894 1160 114 784 1.535 at 110 12.8 95 . 9533 Old Blend Tank Bnpty New Blend Tank 893 1160 73 706 1.545 at 100 12.9 98 8923 Less 10$ contingency Difference In Chlorlnator Total goods In prooess 2,651 23,679 7.800 31,479 MONS 046074 VI. PROCESS IN DETAIL, contd Dept, 246 Monthly Inventory 8 A.M. PlnlBhed Poods - 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.Or. 1.555 1.555 1.495 Temp, Lbs, Per. c. dal. 90 12.96 90 12.96 70 12.46 Inches in Tank 30" outage 53 52 U.S. Lbs.Finished Oallons Aroclor 1725 6492 6587 22,356 84,136 82,073 #5 Stg. Empty Care MONX 809 Empty (Solid Aroclors) Tank Batch Lba. Fin. Lbs.Cla No. Diphenyl Hold Equlv. Aroclor Req'd.To charged Pt. Aroclor To Be Finish Lbs. Lbs. * Fin. Crude Rais'd. Aroolor #1 Chior. Stg.Pot Empty Empty 1 Still Pot - Bnpty Pre Runs - None Finished Poods - Aroclor North Hopper Snpty Inohes out - South Hopper Empty Inches out - Lots 0 No.Baas 50 Cu.Pt. x #1 Cu.Pt. Cu.Pt. X #1 Cu.Pt.5 No.Lbs. Lbs. In container HONS 046075 # # VI. PROCESS IN DETAIL, contd. Dept. 246 Monthly Inventory 8 A.M. Raw [Materials Diphenyl In Scrubber Liquor {See page VI-53). In Measuring Tank In #1 Storage Tank . 82 Inches In. - 11736 U.S.Oals. x 8#/U.S.0al. In #1 Storage Tank 0 Inches In - U.S.Oals.x#/Oal. In Cars - None Less Reserve Reported Total VI -52 Process in Detail 8401 3600 93888 105889 3000 102889 Chlorine Liquid In cylinders - o Oas In 3crutber liquor (See Sheet following this page Pounds Crude High Boilers 0 Distilled High Boilers 0 Aroolor Trappings Lime 30 bags at 50# each - 1500# Attapulgua Earth 6 bags at 50# each = 300 # Toluol 1 drum 200# MQNS 0460 76 VI. PROCESS IN DETAIL, contd. Dept. 246 Monthly Inventory 6 A.M. Scrubber Liquor VI - 53 Process In Detail Scrub- Inches U.S. Per Innage Oals. Sp.Or. Temp. Equiv.* No. c. Aroclor 1 10 172 1.200 65 1126 0.3. #/3al 10.00 Lbs. Lbs. Lbs. Ci, Diphenyl Total (1) U) 447 1273 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 1.230 65 1130 10.25 833 1945 2778 1A 20 271 1.230 65 1130 10.25 833 1945 2778 3348 Less Reserve 1000 Total Reported 2348 8401 0 8401 11749 Note: (1} Lbs. total x % Cl* - lbs. Cl,' (2) Lbs. total - lbs. Cl, - lbs. diphenyl * corresponding to the % chlorine from the curve on page III-15. See also the ready reclcner oh pages 10b, c and d. Section VI. MOWS 046077 VI. PROCESS IN DETAIL, contd. Dept. 246 Monthly Inventory 8 A.M. 1142 1148 1154 1160 1162 CRUDE AROCLOR Lot R-2 = 1 part drum 258# T-2 = 1 II ft 485 It T-l = 1 (1 't 492 II T-l = 1 II II 530 II T-l = 1 II <1 597 1168 0 1169 0 1170 1171 Lot R-l = 1 part drum 170# II T-l 1 II II 220 4065 0 5060 0 2565 0 300 ~ 0 301 0 VI - 54 Process Detal1 MOMS 04607a VI. PROCESS IN DETAIL, contd. Dept. 246 Monthly Inventory 8 A.M, 6-1-46 .1 VI - 3'. Process ir, Detail Aroclor On Total'- Hand Produced Net To 5-1-46 Reed. Account For 1119 1132 1142 1148 1154 1160 1162 1168 1169 1170 1171 4065 5060 2565 , 0 0 260 285 194 530 596 0 0 170 220 0 0 0 00 00 00 200 0 300 0 00 00 00 00 00 00 00 00 00 0 0 260 485 494 530 598 0 0 170 220 0 0 0 To On rfand On Hand 363 To Total 6-1-46 6-1-46 Net ft-246 Transfer by Diff by Inventor 00 000 0 0. 0 0 0 20 2 258 i-.p 00 0 485 485 20 2 492 422 00 0 530 510 10 1 597 507 00 00 00 00 00 00 00 00 00 0 170 :?o 0 220 2*0 00c 000 000 275T 1242 400 1248 415 1254 230,818 1260 307,296 1262 440 1262M 205 1268 0 1269 0 1270 116 12703 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 0 0 0 400 iOO 32,900 11,800 0 11,800 21,100 21.100 1*17,926 325,352 0 404,443 217,963 48,509 325,352 92,573 92,573 266,472 137,971 137,971 440 148 0 148 292 pop 2,209 2,000 00 0 . 2,000 205 205 0 000 0 0 0. 0 0 0 116 116 0 116 0 0 00 00r 3,143 3,001 0 3,001 142 0 0 (1) 0 00 29,775 0 3,600 3,600 26,175 26, IV'". 0 00 00 0 00 00 TOTAL 571,865 322,239 0 (1) To Dept. D-246 894,104 560,385 52,109 612,494 In process Finished MQNS 046079 281,6:0 31,470 T^rnt VI. PROCESS IN DETAIL, contd. 57 Process in Detail Bnergency Measures Power Failure Chlorlnators 1. Shut off the chlorine feed. 2. Shut off the cooling water. 3. Shut off the feed w$ter and cooling water on HC1 aosorbers. Stills 4. Shut of still furnaces. 5> Suck out'still coll*. - 6. For a long stoppage close off, or vent, the still, St:p the steam on the ejectors, then the water. 7. Drain the still If only a heel 13 left In it. Aroclor Filter 8. Blow the press contents to the blending tank. HC1 Handling 9. Close valves below all acid tanks. 10. Replace all plugs and manllds. Oeneral 11. Throw all motor switches to the "off" position. 12. Turn off allgas burners. ' 13. Leave rail care In safe condition. Air Failure 1. Affect tank unloading, air-blowing of 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. HONS 046080 VI. PROCESS IN DETAIL, contd. Emergency Measures,, contd. VT - 58 Process In Detail Plant Water Failure 1. Chlorination would have to stop because of lack of cooling for the HC1 absorber. 2. Ejector Interstage cooling ecuid fail. 3. Water supply to the heat exchangers on the stills aould fall. 4. Chlorlnator pot gland, water cooling would fall, also the cooling of the flaker (solid Aroclor plant no longer In use). 3. Water supply to various pump glands would fall. City Water Failure The following units depend on city water: -- 1. Chlorlnator Jackets. 2. HC1 absorbers (feed water). 3. Safety showers, toilets, drinking fountains, wash bowls. natural Qaa Failure Natural gas serves: -- 1. Chlorlnator circulation line etc. 2. Chlorlnator pot. 3. Still furnaces. 4. aeneral local heating. HONS 046081 VI. PROCESS IN DHTML, oontd Bnergency Measures VI - 59 Process In Detail Low Pressure Steam Failure Low Pressure Steam serves: 1. Steam tracing 2. Alr-blowlng tank colls 3. Chlorlnator Jackets 4. Scrubber liquor tank colls and jackets 5. Under-ground store tanks 6. Blending tank colls 7. Plaker drain 8. Condenser make-up water 9. Rail-car heating. High Pressure Steam Failure High Pressure Steam serves: 1. Tracing from No. 1 chlorlnator to the still. 2. Tracing from high boiler melt-tank to the cfilorinatirs 3. High boiler melt tank coll 4. Still receiver colls 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 colls with a minimum of furnace heat. HONS 046082 VII. COMMENTS ON THE PROCE3S VII - 1 Comments See also Section II, "CHEMI3TIW OB' THE PROCESS". See alBO 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 plaoed in a heap on tne 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 Hr. Harden, In August 1950. See Section VII, page 10, for 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 oontent 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 coil or Jacket, naturally Increases the rate of consumption of the Iron. Normally the wastage Is about 200 - 300 pounds In 3 to 4 months for eaph chlorinator. Chart A 8393, page VI-48, showing the relation between density, chlo rine oontent, and ohlorlne usage In the ohlorlnatlon 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 chlorinatlona. Chart A 8394 Is used also in cal culating the Inventory values of unfinished chlorination batches. Chart A 8395, page Vll-lb, Is a calibration curve for the flow of chlo rine through the 1.1" orifice as used on the lines to the Krumnrlch Pit HONS OA6083 HONS 046084 VII. COMMENTS ON THE PROCESS, contd. VII - 2 Cqmments Chlorination Stage, contd. chlorlnators. Note that the curve refers to gas at 8 pslg, but the actual pressure at the orifice varies with the rate of flow of the gas, and with the depth and density of the charge in the cnlorlnator. The use of low grade chlorine appears to be harmless, as mentioned on page 2, Section VI. MCC Short form report 267?, 171-790, December 10, 1951, deals with the use of 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 clearing,with 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 pslg were used on the chlorlnators, but failed by plnholing. Later, similar discc falled under pressure when the gas outlet 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 ehlorinator Inlet fitting of nickel cast Iron was installed -- said to be the same as used at Anniston. The cooling colls were lengthened In 1953, giving a 33j< lnorease In chlorination rate. Crystallization trouble was encountered with 5^60 batches, but washing of the ehlorinator with Santowax, before use, gave improve ment . A suggestion has been made at Anniston to work two chlorlnators 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 givn to setting up continuous working through a cascade of chlorlnators, drawing off the different grades at different points. The production rate is net yet thought to Justify this. MOWS 046086 VII - 3 Comments VII. COMMENTS ON THE PROCESS contd. Chlorination Stage, eontd. In a report on a Visit to Anniston, March 31, 1952, Mr. Ealton mentions dlsousslon 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 polychloro 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 120*C. 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 135*C. would have about the same vapour pressure, so that about l/60th of a mole more would be carried away during chlori nation to dlchlor, and similarly with chlorination at 150* to trl-chlor. After that, the vapour pressures drop more quickly than corresponds to the batch temperature increases,so that vapourization losses beoome almost negligible In the later stages, and the total vapourisation Iosb cannot exceed about 5 of the batch. Cooling the off-gas to something below 100*C. would condense almost all of this vapour, so the Anniston cyclones, with the long outdoor gas main, and the qoke towers, are probably as efficient in this respect as are the scrubbers etc. at the Krummrlch plant. Reaction with unused chlorine la another matter, and the Anniston arrange ment does not Include any provision for this. Havereroft and Mather. 19t7 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 chlorlnators were running rather aold.' When the higher Aroclors are being made, there Is a less depth of diphenyl etc. in th chlorlnator 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 HONS 046087 T VII - A Comment 3 VII. COHKENTS OK THE PROCESS, contd. Scrubbing of the'Chlorination Off-gases. contd. report fairly good chlorine efficiencies, (see Section X below). With the Anniston off-gas arran|ements, any material volatilising from higher Aroclora can fairly easily be kept apart from any coming from lower Aroclors. Alr-blowing of Crude Aroclora. It Is desirable to use thoroughly dried air because It helps to remove moisture from the product, and probably this makes the HC1 easier to remove! London Engineering Dept, report,September JJ51, (page 107) ,on the start-up of the Newport plant, reported that a dense cloud of JIC1 was fcnned when alr-blowlng started, and a simple lime scrubber was Installed to prevent trouble with the Alkali Acta. The amount of HC1 was about 2 lbs./batch. Resinous Aroclor required longer aeration -- up to 6 hours. Page 1P3 - 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 oarrled above the roof level. A letter, Mather to Thrift, Kay 2, 1949, mentions a Haveg stack at the Krummrlch plant, and states that there was no ft*ne nuisance there. The molster ,ir at Newport could cause the HOI to be more noticeable. The crude, before alr-blowlng,on occasional tests, showed 0.5 to 1.0 mg KOH, equivalent per gram of sample, corresponding to about 2j to 5 lbs. HC1 per chlorination batch. Anniston In 1947 were-uslng 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 cpver of the scrubber Is removed, the soreen taken out, and the upper layers of coke removed. The coke In MOMS 046088 vz: - Cora,err VII. COMMENTS ON THE PROCESS, contd. Plat Illation, oontd. the tower Is Impregnated with 5058 caustic soda solution once or twice a year. The scrubber IS filled with the solution, left 24 hours, then drained through the bottom outlet. Later reports state that the caustic soda has been given up at Anniston and at the Ki'ummrich plant. At the Kruitimrlch plant the scrubbers are heated externally by gas flames about each 10 day;, 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 remain will be taken up by the AttapUlgus earth in the subsequent trea'r. 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 below the main still. See also page 79, Section XII. The tube plate the condenser leaked at high temperature. steam leaked Into Jacketed lines, and gave colour trouble. It appeared advantage to direct the return stream from the heating coll tangentially lr. the still. It was easier to keep a steady vacuum at 12 mm than when working at 5 - 4 mm was attempted. There was discussion of the relative advantages of a Hagen sepa:, inside the still, and a cyclohe separator outside It on the vap: .1 stream. Mr. Furzey reported, December 5, 1951. that the return lines the colls at Newport had been carried down below the level of \ncharges In the still. This arrangement, however, did not give ai better coloured distillate, so It was abandoned. The return section. In particular, should be arranged for easy rodding, to clear It. At the Krummrlch plant, Merco cocks are .* on the circulating line. MONS 046089 VII. COMMENTS OK THE PROCESS, contd. VII - 6 Comments Distillation, oontd. 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 coll to become choked with coke etc. The Anniston stills have a cyclone on the vacuum line from the receivers. Early experience at Newport broqghtout 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 Bpread 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 punjp falls as the charge In the still diminishes. Directing the returln stream of liquor up through the bottom of the still appears to be bad practice, also the sucking out of the coll at the end of a run Is more difficult. Aroolor 5460 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 Aroolors 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 Aroolor. Schwartlng 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 Pyrjanol, will reduce the chloride figure from 0.3 ppm to 0.1 ppm. A larger amount of earth may be useful In some cases, but a badly contamln|ated batch would be returned to the alr-blowlng stage and then redistilled. MONS 046090 v:i 7 Comments VII. COMMENTS ON THE PROCESS, oontd. Treatment of Distilled Aroclors, contd. Mr. Ellenburg, December 1949, eald that finished Aroclors should not be maintained above 80*C., 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 Fuller's earth, and KN4 grade of Fuller's earth, but have not found anything to equal the Attapulgus earth either m respect of re moval of chlorides (and moisture}, or in respect of speed of filtration. MCL Research Progress Reports 1151 DP 53/86/4 February 1954 DF 53/97/6 March 1954 1152 DF 53/85/7 December 1953 NR 53/103/12 July 1954 etc. deal with this question. The removal of tin-tetraphenyl 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%, ao electrical heating was installed to give a drying temperature of 250*C. The drier earth bo obtained gave shorter working cycles in the treatment of the Aroclors. Aroolor - Toluene blend's. The curves on pages VI-30 & EC-89ehow the change in density to be expeoted 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 quality have been set out on pages VI-32 and VI-33 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. MONS 046091 VII 6 Comment 3 VII. COMMENTS ON THE PROCESS, cbntd. Note on "Chloride Scavengers" Hr. Stlckley, September 1, 1953. quoting Dr. Jenkins, wrote: -- "The use of glycldyl 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 tln-tetra phenyl. I understand that 0. E. has either abolished royalty payments, or so lowered them, that Westinghouse Is now going back to tln-tetraphenyl The only reason for using giycldyl phenyl ether, Is that It Is more soluble In the Askarel. It 13 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 tln-tetra phenyl lp the customer's plant during cold weather, and deposits of tln-tetra phenyl have several times been seen in rail tanks returned to the Krummrlch plant for refilling). Mr. Stlckley adds that the glycldyl 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 chlorhydrln. A possible alternative discussed at MCL R & D meeting, October 1949, was dlbutyl 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 trl-tetra chlprobenzene. Mr. Stlckley, February 28, 1953, quoting Dr. Jenkins, wrote: -- "---- the use of trl-tetra chlorobenzene was a G. E. develop ment. MCC make the blend, for G. E. licencees and use a Mltetra blend supplied by Hooker. Most of a. E.'s licensees are expected to go over to the new formulation containing 45j< Aroclor 1260 and 555< trl-tetra chlorobenzene mixture." HONS 046092 x vi: - 9 Comments VII. COMMENTS ON THE PROCESS, contd. Stabilizers MCC Central Research report 543."Studies on Light Stability of the Kleotrloal Resistivity of Aroolor 1254" White and Ruehrweln, deals with this question. Incidentally discussing the solubility of oxygen In Aroclors. MCL Research Progress report llgl.DP 53/86/1, September 1953. deals with the solubility. In Aroclor, of certain, anthraqulnone derivatives whloh had been proposed for use as stabilizers. About the end of 1951 MCL were asked If they had a method of estimating beta-chlor anthraqulnone In Pyranols, and enquiry revealed that stabilizers are sometimes {added by the users, to Aroolcr 1252 used In capacitors (see letters Ellenburg to Mather, December 28, 1951, and Mather to Quartly, January 8, 1952). Rosalia J. Ulm,of Dayton,In a letter tc R. J. Good, March 12, 1951, discussed the isolation of substituted ar.thraqulnones 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 Product*. The finished products have at times been unsatisfactory for different reasons, as set out below: -- 1. Excbbs Moisture air Possible oauses are (a) lmpeyfect drying of the blew!''V(activated alumina not oorreotly regenerated); (b) imperfect drying of the Atfcapulgus earth; (c) entry of moisture from rain, or moist- air, especially during sampling. Batches may be blown with dry air (not. above 80`C. for the lower Aroolors) to remove excess moisture. HONS 046093 T VII - 10 Comments VII. COMMENTS ON THE PROCESS, pontd. Quality of the Finished Produett, contd. 2. Excises Colour. Around 1950-51 the distilled Aroclors at the Krummrich plant sometimes showed yellow to gfeen colours. In the running-ln 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-dietillation, even In glass. The origin Of the oolour was never ascertained, though at Newport the occurenoe of oolour 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 coll -- use of Hagen separator or cyclone on the vapour exit, also may play a part -- also the frequency of tapping the still bottoms. Air leak tnrough the bottom cock on the still may be haimful. Very high vaouum may actually be disadvantageous because of the very high linear velocity of the vapours which results. Note also that a tubular condenser, once fouled, may not quickly dear Itself In use. Re-startlng after a long shut-down may give oolour trouble for a time. Mr. Bllenberg, 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 not be effiolent 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 chlorinators might cause oolour. MCL Research Report 4l6A, 52/1/1, January 17.. 1952 Indicated that lime treatment would remove the green odour. Dr. Jenkins, January 8, 1952 mentioned that Arcclors sometimes contained traces of chloroph<|nols. Possibly air in the chlorine may favour the formation of phenols. Mr. Ellenberg, December 21, 1951, suggested that the chlorine gas may carry other Impurities. See Anniston report 2673 In the list, at the end of this section,. Diphenyl sometimes shows a yellow or plnklBh colour, but ooldurless Aroclor has been made fr6m such Diphenyl, and It is not tjhought that the colour of the Aroclors is m any way related to that of the Dlphepyl. MONS 040094 VII - II Comment, s VII. COMMENTS ON THE PROCESS, contd. Quality of the Finished Produces, oontd. 3. Partial Crystallization, (possibly after admixture with solvents). At Anniston, the trouble with crystallization in Aroclor 5460 Is attributed to the presence of diphenyl In the Santowax used. This may come about by crqBS-contamlnation in the Aroclor plant, as well as by Incomplete fractionation In the diphenyl still. Attention to this point hes been more effective than dropping the setting point of the Aroclor. The setting points are now In the range 98.5 to 105^`C., Instead of 100 to 105^"C. as formerly. There are some Indi cations that Santowax from "low-conversion" runs of the dlpher.yl 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 tc give material which would match 1232, 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 differer:*- in other respects, aB discussed in Section II above. Complaints of deposition of solid in solutions of Anniston Aroclor 5460 in -white spirit were ascribed to the presence -,f hexachloro 1,4 -diphenyl benzene. See also MCC neper's "Formation of precipitate in organic solutions of Aroclors". May 1950, and 2272 "Solubility of Aroclors 5460 in verlois solvents", Wade, December 1948, (detailed in the list at -. end of this section). 1248 has also shown incipient cry?ta. llzatlon. An acetone solubility test was developed, to detect the t<=m,-, y to crystallize, but it was not completely satisfactory, the, was improved by the UBe of the technique of seeding the te*` solution with a little of the insoluble product. See MCI, Res<-ai Report 4l6 A, 52/1/4, April 11, 1952 etc. HONS 046095 VII - 12 Comments VII. COMMENTS ON THE PROCESS, oontd. Quality of the Finished Products, oontd. 3. Partial Crystallization, oontd. Refrigeration to remove the crystallizable materials has been proposed, but not put Into effect. A suggestion was made that the Insoluble matter might be tln-tetra phenyl, but though this might occur In some cases, the usual cause Is the presence of sparingly soluble chlor-dlphenyls 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 dlsoussed In (K)L research reports under Job 4l6 A. High diphenyl content of the diphenyl hlghbollers 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 1232 appeared to be 4-4' dichlorodlphenyl. 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 u*e of standard NaCl dilutions, and ex pressed as parts chloride per million on the original sample. Another portion of the Arcelor Is heated with a strip of alumi num foil for 6 hours at about 210*C. under a condenser, cooled, HONS 04609b VII. COMMENTS ON THE PROCESS, contd. VII - ]J Comments Quality of the Finished Produces, contd. 4, Excess Inorganic Chlorides, contd. 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 method* are given In Section IX, below. These tests arise from the use of the Aroclors in electrical equipment. The first chlofide test covers possible corrosive effectB of the Impurities In the Aroclor as received, and the second one Is Intended to never stability of ihe Arcelor, and the development of corrosive materials when the Aroclor 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"non+volatlle" chlorides. The volatile chlorides are supposed to 50 off frot. the transformers, etc. In whloh Pyranol is used, without corroding 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 te#c flask, confusing them wltr the 'hon-volatile". See also the notes or. the test method itself. Section ix, pages 77 abd 181-. Dr. Munch and Mr. Ashworth at St. Louis nave developed a test In which the "HOI" liberated during the heating is continuously aspirated over into sllver-r.ltrate solution, a method which would appear to give a better measure/the stability of the material. There is a long history of trouble with the venv stringent speolfloatior. laid down by users In respects of tne chlorides tests on Aroclors for the electrical Industry. MONS 046097 VII. COMMENTS ON THE PROCESS, contd. VII - I4 Comments Quality of the Finished Products, contd. 4. Excess Inorganic Chlprldes, contd. In the first place, quit* special precautions have to be observed In taking Bampl*s and In making the tests, especially In factory conditions wh*re 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 AnnlBton has developed a satisfactory method of taking samples fromrall cars and factory tanks. New, dry, sample bottles, not oleaqed or washed In any way, are used, and plunged well below the surface of the liquid to be sampled, and washed out at least thre* times with the material, blown out with dean dry air or nltfrogen, then filled and closed. This procedure oan 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. Amber coloured glass bottles are better. Laboratory arrangements necessary for the chloride test are described In 3ectlon IX, below. The direct test, for chlorides In the sample before heating, will estimate fcee HC1 and metallic chlorides such as might result from oorroslon, sa|y of the still condensers. If chlo rides get through to the "clean" side of the filter, they may be very troublesome. Alr-blowlng of the warm material under warm conditions, will bring the HC1 down to a low limit, and reaction with tln-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 slnoe the tetraphenyl Is used In excess, there would appear to be a chance of the formation of materials such as SnCiphj which would carry through Into the finished produot, and so spoil the chloride teat. Gradual MONS 046096 T s VII. COMMENTS ON THE PROCESS. contd. Vll - 15 Comment a Quality of the Finished Produces, contd. 4, Excess Inorganic Chlorides-, contd. addition of the tln-tetra phenyl might precipitate ail the reactive chlorine as smCl^, so preventing the formation of the hypothetical SnClFhs etc. In practice, the tetra phenyl Is the last Ingredient to go Into the blender, eo 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 fall to pass the inorganic colonies test, but sometimes quite heavy treatment Is nee led. If blends such as Pyrattols 1467 and i470, which are required to contain Tln-tetraphenyl, are heavily treated with ear*h, a good deal of the T.T.P. will be removed by the earui, and the amount bo lost will have to be made up again. Possible causes of high "direct" chloride test sre: 1. Contamination of the system with metal..lo chlorides already mentioned. 2. Insufficient removal of HCi by air -blowing. 5. Insufficient amount of lime used lr. the dl*tl-iatlon. 4. Entrance of HC1 from the factory atmosphere. 5. Entrance of CaCI* from the air breather cr, the tank vent. 6. MolBture (in the Arcelor cr Pyranol or In the At'apulgus Earth) will delay the removal of .411 by air blowing, and will, promote the formation, of chlorides which will remain in the batch. 7. High chloride content of the chloride "scavenger" used. MQNS 046099 T VII - 16 Comments VII. COMMENTS ON THE PROCESS, contd. Quality of the Finished Products, contd. 4, Excess Inorganic Chlorides, oontd. Oeneral Klaetrlo (1950) reported that tnoy eould Improve the electric properties of Pyrfcnol 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 Krummrlch 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 Krumrorlcn plant early in 1951 was found to test 0.15jpm chlorides, and was, therefore, returned from the rail oar to the plant for re-treatment. By this time it showed 0.8 ppm. It was 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 diminished 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 Aroclors, as indicated by the Inorganic chlorides test after the sample has beer, heated m the corrosion test, presumably .arises from the presence of traces tf moderately Stable organic chlorine compounds, rather th?.r. Iren a_-.y instabillty of the chlcrodlphenyls themselves, since good batches show really high stability. Ring substitution of chlorine for hydrogen In the diphenyl nucleus should yield stable compounds; the unstable impurities may be ring adi.iM.tr 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 chicnne derivatives, Little exact information on tfrese points appears to be available, and It might be thought that the unstable materials wculd be destroyed during the prolonged heating cf the charges In the vacuum stills, except for ary which might distill over In the early part of the batch. RONS 046100 VII - 17 Comments VII. COMMENTS ON THE PROCESS, contd. Quality of the Plnlshed Products. oontd. 4, Exoess Inorganic Chlorides, eor.td. Similar considerations apply tc trl- and tetra- chlorobenzenes. Trouble with Pyrancls In 1947 was traced to the Instability of trlchlorbenzene due to the use cf too little catalyst In the manufacture cf the TCB, resulting presumably in the formation of small amounts of ring addition products. Trouble also arose from th* presence of "chlorides" in the purchased tln-tetra phenyl, Some deliveries contained as much as 500 ppm, and MCC found it expedient to purify the T.T.P. as dlsoussed In Section IX, pages 4-. Trouble with Inerteen In 1953 was ascribed to Instability of the glycidyl phenyl ether used. 5. Unsatisfactory Electrical Properties. Moisture and Inorganic chlorides naturally axe '.01601.1008016, 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 V1I-25 }. The choice of containers is discussed ir. Annlstc.n report 277?. See also MCL research progress reports 1151 51/141/ 24 etc. 1$5? and 416A 52/1/8,-October 1952 (Arcelor 1254 net discoloured In plain steel, 1 week at 60cC.). Packages are air cussed on pages 34 and 35 of Section VI. above. Report 1151 RR 53/57/2, May 1953, shows very little deterioration In electrical properties under severe conditions cf exposure to steel, and even less with aluminium. Mixtures containing TCB or TTCB have a more powerful solvent effect than straight Aroclors, and this has caused trouble, for Instance, In cases where Jblntlng materials, dlyptal "dopes" on pipe Joints, etc. have been attacked lr: the customer's plant, with detriment to the electrical properties of the Pyra-xl. MONS 046101 VII - 18 Comments VII. COMMENTS ON THE PROCESS., oontd. Uses for the Products; Appllpatlon Work. The MCC Bulletins "Physical Properties of Aroclors" and P-115, "The Aroolors, Physical Properties and Suggested Applications", mention the following possible uses: -- Adhesives (adhere to metals) -- low vapour pressures advantageous. Eleotrlcal 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 outtlng oils. Heat transfer media (See also the speolal bulletin P-130). Plastlolsers in PVC, nitrocellulose, chlorinated rubber eto. -- 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. k Chem. Data, Section III, above, for references to lists of compatibilities of materials with Aroclors.) MONS 046102 VII - 19 Comments VII. COMMENTS ON THE PROCESS, oontd. Csss for the Products ; Application Work, eontd. Extender for the costly Camauba wax In polishes. Prevent sticking of dr&werB in furniture. Wood treatment (along With pentaohlorophenol). Por many of these uses, gaskets and packing materials, which are resistant to Aroclors are needed. On this question see Section XII, page 8, below. See also MCL research reports, 1152 DP 54/16/7 and 8,July and August 1954. 1 Aroclor 2565 has been used to make non-flame roof sheeting, (Anniston visit report 1947, page 3). Propertles_favourlng_the_use_of Aroclors_are^ 1. The wide range of properties available. 2. Low vapour pressure. 3. Very low corrosive effect. 4. Compatibility with numerous materials. 5. Chemloal Inertness and thermal stability, 6. Waterproof. 7. Non-Inflammable. 8. The solid Aroclors are odourless and tasteless. 9. Good eleotrloal properties. On the other hand, the Aroclors are not quite above question on toxicity, and they have a very high viscosity Index, 1. e. a large drop In viscosity with a small rise In temperature. Viscosity MONS 046103 VII. COMMENTS ON THE PROCESS, contd. VII - 20 Comment s Uses for the Products; Application Work, oontd. 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 54/26/5, July 1954, 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 54/26/13, Feb.1955 Material for publications on application in capacitors etc. 347 52/47/1, Sept. 1952, and the corresponding Final Report, Mar.3/53 Literature survey on electrical uses Final report 347D, June 1953, Methods of testing dielectrical properties. Research Progress report 347 51/141/17, November 1952, "Electrical properties of Montars," and U51 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 poln+s Autogenous ignition V. I. improvers See also reports under Job 454 E in 1952. HONS 0A61Q'* T VII - 21 CommentB VII. COMMENTS OK THE PROCESS, contd. Uses for the Products; Application Work, contd. Work on uses aa plasticizers lp described In: - MCL Research Progress Report 347 51/59/1 etc. "Aroolors In PVC". Work on uses In paints, and polishes etc. Is described In: -- 1152 DF 53/89/5 May 1954, 1242 improves solvent polishes FR 52/9Q/6 Jan.1953, No gloss imparted to sllloate paints DF 54/27/1 eto. 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 eto. was discussed In correspondence, January 26, 1955. Miscellaneous Uses: Use as rust Inhibitor Is described In DF 54/26/11, January 1955. Use In lithographic Inks has been suggested In correspondence, (May 3, 1954). Aroolors also have possibilities as chemical Intermediates. See MCL Res. Prog. Rpt. 347D - 51/14l/ June 1952 etc. for nitrated Aroolors. The MCL Progress Research Department report for November 1952, page 4, mentions the preparation of Aroclor derivatives for trial aa lnsectloldes. Report ll6l RR 54/17/1, November 1954, discusses the hydrolysis of Aroolors to hydroxydlphenyl. Mr. Stark of the Krummrlch plant, September 24, 1954, suggested that Montars would make a good sealing compound to cover the oast lead whloh holds the carbon anodes In Hooker chlorine cells. MONS 046105 I VII. COMMENTS ON THE PROCESS, contd. VII - 22 Comments Patent Position. lories, Soffranko and Becker, November 6, 1946, page 167, state: - "In 1935 the Swann Chemical Company was acquired by Monsanto, which gave the latter access to the patent rights for the production of Aroclers". MCL Research and Development pept. report for August 1949, page 26, states that the market fop Aroclors in the electrical industry was largely dominated (in Britain) by B.T.H. patents up to about 1946. These patents had run but, 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 1949 report, pajjp 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 30, Indicated that discussions were still In progress with B.T.H. Meanwhile the Anniston alternative material, dlbutyl 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. MONS 046106 VII - 23 Comments VII. COMMENTS ON THE PROCESS, ontd. Lls^of^egorts>irela|jjln^^oi^roclor6^nd>iP2rwiol^ PROCESS REPORTS 1. Dept. 246; Aroclor Process Lyles Soffranko and Becker November 1946 2. Notes on No. 1 above. E. Mather April 1947 3. Notes on AnnlBton Aroclor plant Havercroft and Mather September 1947. 4. Dept. A-?46; Pyranol Process Lyles Soffranko and Miller March 24, 1947 5. Process Description for Aroclors, Dept. 246 Sohwartlng, Neff and Craves November 1953 6. Revised version of No. 5 above Schwartlng and Schwartz March 15. 1955 7. Process Description for Pyranols and Inerteens Schwartlng, Neff 4 Craves October 1953 8. Aroclors Operating instructions Dept. 246 Alnsley and Schwartz August 10, 1954 Date CopleB sent to MCL April 26, 1947 and October 24, 1950 April 25, 1947 October 7, 1947 October 15, 1947 March 26, 1954 May 17, 1955 May 83, 1955 MQNS 046107 VII. COMMENTS ON THE PROCESS, eontd. List of Reports, eontd. 9. Anniston Equipment list for AroclorB, Ellenburg 10. Notes on a Visit to the Anniston Plant, Harden August 5> 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. Krummrlch plant Monthly Operation Reports 17. Krummrlch Plant Investigation Reports VII - 24 Comments Date Copies sent to MCL June 7, 1946 March 29, 1955 routine routine routine routine routine HONS 046108  ' IX. SPECIFICATIONS AMD TEST METHODS, contd. IX - 82 Teat Methods 10,123-53 Date: 3-10-53 By:AKB,NPA:SMK Material:Aroolofs.Pyranola, Iner- Method No.10,123-53 teens, and Tri-Tetrachloro- benzen Blends WOK Dept. No.246/233 Test: Plash and Fire (Burn)Polnt* 1 Introduction: The flash and fire (burn) point 4>f Aroclors, Pyranols, Inerteene, and Tri-Tetraohlorobenzene 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, For 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 Plre (Bum) Point described under (B) at the end of the method. A Complete Procedure: 1. Fill the cup to about 3/8"from the top with the sample. 2. Insert a 20-760*F. range ASTM Open Flash (1 Inch ImmerBion) thermometer so that the bulb is 1/4" off the bottom and midway between the center^and the bck edge. 3. Adjust the flame so that the rise of the sample's temperature will be at the rate of 9 - ll'F. per minute. 4. Adjust the testing flame so that It will he produced through a blow-pipe with an opening 1/32". This flame should be only a bead 3/3?" In diameter. CAUTION: 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. MQNS 046207 XX. SPECIFICATIONS AND TEST METHODS, oontd. XX - 83 Test Methods 10,123-53 Plash and Wre (Burn) Point Teat for Aroolors. Pyranols. Inerteens, and Trl-Tetrachlorobensene Blenfts, Method Mo. 10,123-53, contd. A. Complete Procedure, oontd. 5. When visible vapors start to rise from the product under the test carry across the surface or material the small bead flame (Step A). The test flame should hever be allowed to get anjr 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 Plash Point. 8. Continue to pass the flame head across the sample (Step 5) ever five degrees Fahrenheit until the vapors flash down to the material and continue to burn for at least 5 seconds. 9. Reoord this temperature as the Fire (Burn) Point. NOTH: 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 (Bum) Points to the nearest 1*0. B. Abbreviated Procedure: 1. Fill the cup with the sample to within 3/8" of the top and heat to boiling under a well ventilated hood. 2. As the material oomes to a boll pass a test flame (see Step 4,Com plete Procedure).across the top of the sup(Step 5,Complete Proce 3. Note if the sample bums for five seconds or more. dure) 4. If the material does not bufn for 5 seconds, report the Fire (Bum) Point as) B.P. (abova boiling point). 5. If a positive result (the sample bums for 5 seconds or more) was obtained, a test for Flash And Fire (Bum) Point should be run on the same materia, using ihe procedure described above under "Complete Procedure". HONS 04620B ' ' IX. SPECIFICATIONS AMD TEST METHODS, contd. IX - 84 Test Methods 10,124-53 Date: 2-26-53 By: AEB.NPA:SMK Material: Aroelors, Pyranels, Method No. 10,124-53 Inerteens, and Trl-Tetrachloro- bentene Blends WOK Dept.No.233/246 Test: Iron (as Fe)* 1 Iron Is determined In Aroelors,,Pyranols, Inerteens, and Trl-Tetrachlorobenzene Blend on occasional samples only. 1. Weigh on a beam balance a $0 (+0.05) g. sample In a casserole. 2. Add 20 ml. C. P. HsSO^ and digest the mixture on the hot plate. 3. Ignite the carbonaceous mats In the muffle at 800*C. 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 S0s 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 10O-ml. low form Nessler tube. 8. Add 3 drops HaOs, 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^, H*0* and NH.SCN. Follow the procedure described In Qeneral Method No. 8 (Method No. 10,199). Add eMttgh Standard F solution to match the color of the sample. Calculation: t ( ) m * ron ' e " (rcl- 3td. ye solution x 0,000025) x 100 Weight of Sample (step 1) x Aliquot 100 Report the results to the nearest O.OOOljg HONS 046209 ' IX. SPECIFICATIONS AND TEST METHODS, eontd. IX - 84a Teat Methods 10,125-53 Date: 2/26/53 By: AEB, NPA SMK Material: Aroolora, Pyranols Method No. 10,125-53 Inerteens, and Tri- Tetradhlorobenzene Blends Test: Refractive Index WOK Dept. No. 233/246 1. Determine refraotlve Index of Aroolora, Pyranols, Inerteens, and Trl-Tetraohlorobenzene Blend according to Oeneral Method No. 28 (Method No. 11,784) with the following modifications: 2. Take refraotlve Index at 251c. 3. Clean the Abbe prisms by flushing with Trichlorobenzene. Then follow with benzene and "Meraol" washes. NOTE: BO NOT TOUCH TUB POLISHED SURFACES OP TIE ABBE PRISMSI Report Refractive Index ( N. 25 ) to the nearest O.QpOl unit. HONS 046210 l IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 85 Test Methods 10', 126-53 Dates 3-9-53 Material: Aroclors, Pyranols Method No. 10,126-53 Inerteetis, Trl-Tetra- ohlorobpnzene Blend WOK Dept. No. 233/246 By: SB,NPA:SMK Test: Corrosion and Chemical Stability* 1 2 3 4 5 6 7 8 9 10 Procedurei 1. Roll a rectangular (2" x 4") piece of aluminum foil so that it will pass through a 9 24/40 Joint of the corrosion test flask. CAPTION: Be careful that after rolling the specimen does not touch Itself at any point. 2. Nash the aluminum foil (Step 1) scrupulously with acetone, distilled water, acetone, benzene, and chloride-free ether. 3. Then place the foil on a clpan watch-glass and dry In an oven at 110*0. 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 fpll Into the chloride-free corrosion flask of the "0. . Corroslpn 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-lnch 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. MONS 046211 T IX. SPECIFICATIONS AND TEST METHODS, eontd. IX - 86 Test Methods 10,186-55 Test for Corrosion and Chemical Stability on Aroolors, Pyryols, Inerteens, Trl-Tetraohlorobenzenie Blends, Method Ho. 10,126-55, eontd. 11. At the end of the heating period, detach condenser from the flask before removing it frpm 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) Chlorideb - Apply Method No. 10,118 c. Aoldlty (Acid Number) - Follow Method No. 10,087 14. With a pair of clean, straight nlchrome tongs remove the alumi num foil specimen (Step 6), wash thoroughly, dry and weigh accurately on an analytical balance in the same manner as before (Steps 2, 3, 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: - 0. E. Corrosion Apparatus consists of the following: a) A Corrosion Flask - It is a 300-ml. Pyrex flask with a 6 g.g. 24/1*0 Joint equipped with a 12-lnch straight tube as an air cooled condenser. The Hr-condenser is painted on the out side with aluminum. b) The Corrosion Apparatus!! A translte box 32" long x 8" wide x 5" deep. The top f the box represents a split transits board with holes cut to fit the flasks. The box is heated by . ' two 500-watt, 15 volt Q.. Strip heaters with off-set terminal* ; 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" thlak. The temperature Is controlled by an automatic thermostat with tempera ture setting Indicator. MONS 046212 T ' IX. SPECIFICATIONS AMD TEST METHODS, contd. IX - 87 Test Methods 10,127-53 Date: 2-26-53 Material: Aroolors(Crystalline) Method No. 10,127-53 By:EAB,NPA:SMK Test: Hold(Grystalllzing)Point WOK Dept. No. 246* 1 2 3 4 Introduction: The cyrstalllzlng point of the crystalline AroclorB is defined as the highest temperature noted after crystallisation begins when the sample la cooled slowly In an insulated container. This Is iK referred to as the "Hop.d Point". Procedure: 1. Pill a 1" x 8" test tube to within 2 Inches of the top with molten Aroolor and heat sufficiently to Insure complete fluidity. 2. Insert an 0-360*0. range, 3-Inch Immersion, thermometer through a oork 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. 3. Place the test tube In a suitable Dewar flask (tube form-evacuated). 4. Allow the sample to cool to pbout 3'C. below the expected crystal lizing point wlthaat stlrrlnje. After the temperature is 3 to 5*C. below the expeoted crystallzlng point (material supercooled 3-5 "C.) start to stir the Aroolor carefully with the thermometer and note the highest temperature rise of the Aroclor. This point Is taken as the Hold (Crystalllzlng)Fpint.. NOTH: If a material of unknown qjuality is to be tested and the approximate cyratallizlng point lp not known, a preliminary test is made in order to determine at wha|t temperature the stirring of material should start. CAUTION: The material must not be supercooled more than 3 - 5C. below the expected crystallizing point. Duplicate tests should check within l'C. Report the Crystallizing (Hold) point to the nearest 1*C. HONS 046213 , . IX. SPECIFICATIONS AMD TEST METHODS, contd. IX - 88 Test Methods 10,194-55 Date: 4-5-55 by: WWX:WJQ Material: Aroolor-Toluene Mixtures Test: Composition Method No. 10,194-55 WOK Dept. No. 246* 1 Introduction: Certain customers require a mixture of 900 by weight of Aroolor (1254, 1260, or 1262) with 100 Toluene. A rapid method of determining whether or not the required amdunt of Toluene la present In the sample of the mixture has been devlseq and Is described below. Procedure: 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. Prom the supervisor's file obtain the specific gravity of the Aroclor used In the mix. 5. Warm the sample to about 50*C. by placing It next to a hot plate. 4. Four the sample Into a cleqn, dry hydrometer Jar and determine the specific gravity at 40/15.5*C. according to Oeneral Method No. 13 (Method No. 10,497), NOTE: The gravity must be taken at exactly 40*C. 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 Aroolor used In the mix the ordinate on the following graphs on pages XX-89, IX-90, and IX-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 absolssa and ordinate Intersect on the graph. If this point falls within the shaded portionof the chart, the mixture oontalns 9*5 - 10.50 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*C. and whether or not the material passes the specification limits. Report the gravity to the nearest 0,001 unit. MONS 046214 HONS 046215 IX - 90 '  nt>* co. 3 HONS 046217 IX. SPECIFICATIONS AMD TEST METHODS, contd. Date: 8-25-54 Material: General Method By: AEB,NPA:WJG Teat: Iron (Pe) Traces (Colorimetric) IX - 91 Test Methods 10,199-54 Method No. 10,199-54 WOK O.M. No. 8 Introduction: Quite frequently Iron la 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 colorlmetrlcally 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 proportional 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: .* 1 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 q solid: 1. Weigh accurately on an analytical balance a 1 to 10 grams (more for extremely low Fe content). 2. Dissolve the sample In dilute HsSO^. 3. Oxidize the Iron by adding 3-4 drops of 3# HaOa solution. If the material to be tested Is a liquid: 1. Acidify the sample with C.P. HaSOjj or C. P. HC1. 2. Oxidize the Iron by adding 3-4 drops of HaOa solution. The procedure Is continued for solid and liquid material In the following way: -- MONS 046218 . . ' IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 92 Test Methods 10,199'y* Oeneral Method, Iron (Pe) Traces (Colorimetric), Method No. 10,199-54, contd. A. Add to the prepared sample (Step 3 - solid material: Step 2 liquid product) 10 ml. N MH^SON 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 Pe solution until the tints of the two tubes match. Record the number ml. of Standard Pe solution re quired to make the match. Calculations: $ Iron (as Pe) iul.Std.Pe Sol'n.x 0,000025 x 100 Weight of Sample The test will easily detect 0.00001$ Pe. Important: In the event that a sample contains sufficient Iron to require a titration of more than 10 ml. Standard Iron (Pe) solution, the prepared sample should be diluted to a larger volume (500 or 1000 ml.) and the Iron (Pe) should be determined on a suitable aliquot. Reagents Used: M NHijSCN Solution: Dissolve 76.1 g. NH^SCN In distilled water and dilute to one liter. - 3$ HsOa 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 (Pe) Solution: Plpet 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. Pe/ml. * Clean wire with emery cloth to remove any oxide and wipe clean before weighing. MONS 046219 IX. SPECIFICATIONS AMD TEST METHODS, oontd. IX - 95 Test Methods 10,252-52 Date: 7-25-52 Material: Biphenyl (Diphenyl) Method No. 10,252-52 By: AEB,NPA:SMK Test: Appearance and Colour* 1 WOK Dept. No. 246 Biphenyl (Diphenyl: Xenene) la 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 WOK Plant"but 14 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. Heport observations as none, veiy 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. ' HONS 046220 IX. SPECIFICATIONS AND TEST METHODS, contd. XX - 9*1 Test Methods 10,298-52 Date: 7-23-52 Material: Biphenyl (Diphenyl) Method No. 10,298-52 By: ABB, NFA SMX Test: Crystallizing Point WOK Dept. No. 246 1. Melt completely the sample. Avoid overheating. 2. Kill 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* - 90*C. range, 3" Immersion thermometer and a plungertype metal stirrer. 5. Cool the material with constantstirring to crystallization. After slight Buperooollng of the molten sample, the temperature will rlBe 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. MONS 046221 IX - 95 Test Methods 10,299-52 IX. SPECIFICATIONS AND TEST METHODS, oontd. Dates 7-24-52 Material: Biphenyl (Diphenyl) Method No. 10,299-52 By: AKB.NPA: SMK Teat: Distilling Range: WOK 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: 2. Measure 100 ml. of the molten sample Into an asbestos covered benzene distilling flask. 5. Use a 230* - 265*C. 3" lmnerslon thermometer and set up the distillation apparatus using a translte 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 0.1*0. First Drop Dry Point 100# Range (First Drop to Dry Point) The results are precise to + 0.1*C. MONS 046222 IX. SPECIFICATIONS AMD TEST METHODS, contd. Date: 11-17-53 Material: Qeneral Method By:LO,DKL,NPA:SMK Test: Specific Gravity by Hydrometer1 IX - 96 Test Methods 10,497-53 Method No. 10,497-53 WOK O.M. No. 13 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: Pour 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 teBt that Is free from air currents. Place the Jar on a level surface. 3. Insert a 0 to 110*0. 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 walla of the cylinder. 6. Read the Specific Oravlty as the point at which the surface of the sample apparently cuts the hydrometer scale. Record the reading after applying the hydrometer correction (If any). MONS 0A6223 XX. SPECIFICATIONS AND TEST METHODS, oontd. IX - 97 Test Methods 10,497-53 Oeneral Method, Specific gravity by Hydrometer, Method No.10,497-53 oontd. IMPORTAMT; 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: CAPTION: These calculations apply only to those hydrometers whose specific gravity scales are numerically higher at the bottom of the soale 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.Or. at specified temperature = Sp.Qr. at observed temp.+ Sp. Or. temp, correction. b. If the observed temperature Is below the specified temperature: Sp.Gr. at specified temperature Sp.Or. at observed temperature - Sp.Or.temperature correction Report the specific gravity at the specified temperature to the nearest 0.001 units. MONS 046224 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 90 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*0. Specific gravity 25/15.5*0. Specific gravity 60/60*F. Specific Gravity 20/4*0. The meaning of the expression given in this example can be easily seen from the following definition of specific gravity and of density: A Speolflc gravity 1b 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 substanoe per unit volume at any definite temperature. Then in the expression "Specific gravity 25/15.5*0. 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/y*C. are lnversly proportional to the absolute densities of water at x*c. and y*C. NOTE: Absolute densities 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/y"C. instead of x/x"C., the following calculation is sufficient: Specific gravity x/y*C.=(Sp.0r. x/x*C.) x density of H0 at xC. density of H*0 at y*C. M0NS 046225 .. IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 99 Test Methods 10,510-54 Date: 6-7-54 By: ABB, NPA: WKO Material: Arcelor 1270 TeBt: Foreign Odour Method No. 10,510-54 W.O.K. Dept. No. 2461 1. Place approximately 2 or 3 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. 3. 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 AwjClors. 4. Material showing sharp odours will be rejected. Report the Foreign Odour according to the General Method No. 5 (Method No. 10,06.0) definitions of odours (none, very faint, faint, distinct, or strong). HUNS 046226 IX - 100 Test Methods 10,511-54 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 6-7-54 By: AEB, NPA NJO Material: Aroclors 1270 and 1271 Method No.10,511-54 Test: Colour of 5% Toluene 3ol'n. WOK Dept. No. 2461 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. 3. Place on a hotplate and stir until all the Aroclor has dis solved. Do not overheat the solution. 4. Transfer the hot solution to a warm 50-ml. tall form Nessler tube. 5. Determine coloulvof the material according to Oeneral Method No. 2 (Method No. 10,007). The method is precise to + 5 units. Report the APHA Colour to the nearest 5 units. MONS 046227 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 101 Test Methods 10,576-54 Date: 6-18-54 By: ABB, NPA WJO Material: Aroclor 1271 Method No. 10,576-54 Test: Appearance and Colour WOK Dept. No. 2461 Aroclor 1271 (Decachlorodlphenyl) 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), Buch as rust, wood, Mnt, black specks etc. Report observations as none, very slight, slight, moderate, or considerable. Describe appearance of Impurities briefly. MQNS 046228 ' XX. SPECIFICATIONS AND TEST METHODS, oontd. IX - 102 Test Method 10,577-54 Date; 6-18-Material: Arcelor 1271 By: AEB, NPA: WJ0 Test: ^Moisture (Haft) Method No. 10,577-54 WOK Dept. No. 246 1. Tare accurately on an analytical balance a wide mouth drying bottle. Record tare. 2. Weigh accurately on the same balance a 10( + 0.0005) g. sample into the tared bottle. Record weight of the sample. 3. Place the bottle in an oven at 120"C. for 2k hours. 4. Cool the sample in a desiccator. 5. Reweigh the bottle. Record loss in weight of the sample. Cal culate percent moisture. Calculation: % Moisture (H*0) jt Loss in weight (Step 5) x 100 wt. of Sample (Step 2) The method js precise to + O.Ol# Rupert the result to the nearest 0.01$. MQNS 046229 IX. SPECIFICATIONS AND TEST METHODS, ocnt.i . IX - 105 Test Methods 10,578-52 Date: 3-26-52 Material: Aroclcr 1271 Method No. 10,578-52 By: RK,WJQ:SMK Teat: Melting Point WOK Dept. No. 2461 1. Fill a 400 mi. tall-fcrm beaker with Dow Corning Fluid. 2. Fill one capillary melting point tube to a height of 3/4" with sample and another with the standard Aroo.lor 1271. Attach both capillary tubes to a 300-335"C. y immersion thermometer with two short lengths of thin wire, adjusting the lower end of the tubes level with the mercury bulb. 3. Immerse the assembly in the bath and clamp the thermometer stem in position 3/4" from the side of the beaker. (A desk lamp placed near the bath will facilitate observations). Adjust the initial bath temperature to 250-60*0. 4. After the apperenua is in position, heat at such a rate that the bath temperature will increase 0.5 + 0.1/m.in. 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 end the temperature of complete: melting of both the sample tested and the du Pont standard. The first meniscus is taken as the temperature at vrttlch the first liquid meniscus in the tube Is observed. The complete melt 13 taken as the temperature >' which all crystals have disappeared. The method is precise to + 0.2*0. Report the melting point. (M.P.) (first meniscus) and the complete melt (C.M.) on bob', the standard and sample tested to the r.earest. 0.10.*C. MOWS 046230 IX. SPECIFICATIONS AND TEST 'HODS, cor,id IX - 103a Teat Methods 10.579- 41 and 10.580- 52 Date: 3-4-41 Material: Aro|clor 1271 Method No. 10,579-41 By: AEB.MJW Test: 5# Toluojl Solution Color WOK 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 Aroolor has dissolved. Now transfer the hot solution to a warm 50 ml.tall form Nessler tube ar^d 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 -quits. -------------------------:---------------------------------- j-----------------Date: 6-24-52 Material: Aroqior 1271 By:AEB,WJ0:SMK Test: Crystal (Structure1 Method No. 10-580-52 WOK Dept. No. 246 1. Spread a small amount of the sample on a glass slide and place It on the stage of a mlcroscotle which magnifies from 75 to 300 diameters. ~ 2. When the sample has been bifoyght Into the field and is ir. f-ous, slowly move the slide fromleide to side and observe the kind? of crystals present and the proportion of eaan. 3. Estimate roughly the percent of Jagged crystals. Report the amount of sharp eagqd crystals to the nearest 5j. Two analysts observing the 10JS. material will usually agree within MONS 046231 IX, SPECIFICATIONS AND TEST METHODS, contd. IX - 104 Test Methods 10,620-53 Date: 3-9-53 By:SE,NPA:SMK Material: Arocloris, Pyranols Method No. 10,620-53 Inerteemi s, Trl-Tetra- chlorbe:mzene blends WOK Dept.No.233/246 Test: Moisture (I,e0 Water Content) Introduction: Because of the varying solubllltiy of Aroclors, Pyranols,Inerteens, and Trl-tetrachlorobenzene Blend, different proportions of a mixed solvent are required. However, the analfysis Itself Is the same for all listed products. Procedurei 1. Determine moisture (water content ) in Aroclors, Pyranols, Inerteens, and Trl-tetrachlorobenzene B1end using Karl Fischer (K. F.) reagent. Apply the "Dead St;|op" method described In Oeneral Method No. 7, (Method No. 10,100) wjl th the following modifications: 2. Place the solvents. In the proportions Indicated below, into the titration flask: Material Anhydrous Benzene Anhydrous Methanol Pyranol 1476 ~ Pyranol 1488 Pyranol 1467 Pyranol 1470 Pyranol 1481 Pyranol 1495 Inerteen P.O.P.O. Tri-Tetrachlorobenzene blend: All Aroclors 0 ml. 100 ml. 100 ml. 100 ml. 100 ml. 100 ml. 100 ml. 100 ml. 110 ml. 300 ml. 200 ml. 200 ml. 200 ml. 200 ml. 200 ml. 200 ml. 200 ml. 190 ml. Titrate the solvent with the K. F. reagent until It is "blanked". HONS 0A6232  IX. SPECIFICATIONS AND TEST METHODS, eortd. IX - 105 Test Methods 10,620-53 Test- for Moisture (HaO Water C ohtent ) for Aroelors, Fyranols, Inerteens, Trl-Tet.r-achlorober.z&r.e Mends', Method No. 10,620-53. ocr.td. NOTE! The solvent Is "blanked" when the tube shadow remains fully open (oa. 100) for 30 seconds. *. Refill the burette with K. |F. reagent, to the zero mark. 5. Weigh on a beam balance a ipo (+ 0.05) & sample by difference, Into the "blanked" solvent |an-d allow the material ir. i-tr flask to mix well. 6. Titrate the solution with Kj. F. reagent r-r- the end-point described In Step 5. Record the vclijne of K. F. reagent used. Calculation; % Moisture (H0) ml K.j F. Reagent \ UgO factor x 100 : Sample Weight The method Is precise v.o + yjk of the water present. Report the result to the nearest O.OOOjjt or equivalent p.p.m. NOTE; 1 ppm le equivalent- to q.000i;<. * If required by a specification... report, as "Water Content" in p.p.m. equivalent to per-' nt; moisture. MONS 046233 IX. SPECIFICATIONS AND TEST [OPS, contd. IX - 106 Test Methods 10,670-53 Pat*1 4-13-53 By: DBH,NPA:SMK Material: Pyr^nols 1488 and , 1495 Test: Trlchliorobenzene (TCB) Method No. 10,670-53 WOK Pept. No. 246 Introduction: Aroolor 1260 (Q.E. Compound No. |l482) and Trlchlorobenzene (TCB) (0. E. Pyranol No. 1478) are blended together to make transformer Pyranols for the General Electric Company. Two blends are made: Pyranol 1488 (600 Aroolor - 4056 TCB) and Pyranol 1495 (9058 Aroclcr - 100 TCB). 1 Sixteen ounce sampleeof the Aroolor 1260 and the TCB used for blending In the department are brought tej the laboratory for the analysis. Procedure: 1. Tare accurately on an analytical balance two conical ground glass stoppered weighing bottles. 1 2. Add 10 (+ 0.0005 ) 6. of warm|(60 - 70C.) Aroclor 1260 to each bottle. ' 3. Cool and rewelgh on the same {balance. 4. Add TCB to each weighing bottile from an eyedropper until the desired composition is obtained. NOTE: The following proportions are used: Pyranol No. TCB Added Sample No. 1 Sample No. 2 1488 390 410 1495 90 110 5. Heweigh the material accuratejly on the same balance. MONS 046234 IX - 106a Teat Methods 10,670-53 IX. SPECIFICATIONS AND TEST MEjTHODS, oontd. Test for Trlchlorobenzene (TCB)i In Pyranols 1488 and 1495, Method No, 10,670-53, contd. 6. Put the stoppers In the welching bottles and place them on a covered steam bath. : Swirl the materials occasiojially to facilitate thorough mixing. 7. After the blends are thoroughly mixed, determine the refractive Index at 25*C. with an AbbefRefraotometer according to Method No. 10,125. 8. Plot NDgj versus % TCB on coordinate paper and connect the two points obtained with a straight line. 9. Determine the refractive inAex at 25C. of the sample under test according to Method No. 10.J.25. 10. Determine the percent T.C.Bj present from the graph (step 8). Report T.C.B. to the nearest O.lji. M0NS 046235 IX. SPECIFICATIONS AND TEST t^THOPS, oontd. IX - 106b Test Methods 10,723-51 Date: 5/16/51 Material: General Method By: HOH,DKL:SMK Operation of Fisher Test: Eleotrpphotometer Method No. 10,723-51 WOK 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 ofi functioning of the instrument consult your supervisor. b. Be certain that the proper! filter is in the instrument before depressing the lamp buttonl and that the filter is clean. c. Always adjust the galvanometer needle at the beginning of a series of measurements. I d. See that the Intensity control is in the proper position. e. Use only absorption cells jin the instrument. The matched pairs will be engraved with the bame number by the Service Section. Be sure the cells are cleafi and free from fingerprints. f. In filling the absorption bells, 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 befolre 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) whep placed in the adaptor. i. Always close the compartment when making measurements or setting the initial null. J. In changing the position o|f the sliding platform, push the platform gently but flrmlyj against the proper stop. Do not slam the platform against he stop. MONS 046236 IX. SPECIFICATIONS AMD TEST OPS, contd. IX - 106c Test Methods 10,723-51 general Method, Operation of Flpher Electrophotometer, Method No. 10.723-51, contd. f PRECAUTIONS: contd. 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. 1. Do not keep the lamp buttor( depressed longer than necessary. 1. Place the proper filter In position. 2. Set the Intensity control (lower left switch) to "ADJ. OAL" and turn the "ADJUST ZERO" ^cnob (above the galvanometer) so that the galvanometer needlp coincides exactly with the Index line. 3. Set the Intensity control tjo that position designated by the letter engraved on the handjle of the filter holder. ^. Place one of the matched pajir of carefully cleaned 23 mm Plsher cylindrical absorption celljB containing the reference solution In the rear position In the adapter platform In such a manner that the label fapes front l(towards the operator) and place the other cell of the pair, containing the unknown solution In the front position in the adaptjer holder with Its label also facing front. 5. Close the cell compartment door. 6. Pull the platform knob forward until the catdi is In firm contact with the front stop In order to bring the rear absorption cell containing the reference sojlutlon Into the light path. HONS 046237 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 107 Test Methods 10,723-51 Qeneral Method, Operation of Posher Electrophotometer, Method No. 10,723-51, contd. 1 Adjust the dial control td 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 lamij button, push the platform knob until the platform is firmly in Icontact with the rear stop to place the absorption cell with tjhe unknown solution in the light path. 9. Still holding down the lanjp button, bring the galvanometer needle back to the Index l|ine by turning the dial control. 10. Record the A-Soale or B-Sc|ale reading as indicated in the specific method. 11. Without releasing the lamp! button, reoheck the initial null adjustment as before (Stepb 6 and 7). If not in adjustment, repeat steps 6 thru 11 untp.1 there is no change in null adjustment. 12. Empty the cells, rinse thoroughly, fill with distilled water, and return them to the adapter^, /---------,----- / HONS 046238  ; IX. SPECIFICATIONS AND TEST MKTtjODS, oontd. IX - 107a Test Methods 10,733-53 Datet 5/21/53 Material: Bolder Water By: HOH,NPA:SMK Teat: Chloiflde Method No. 10,733-53 WOK Dept. No. 3501 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 30 H0 solution and mix well. 3. Add 3 drops phenolphthaleln, then follow with 0.5 N H*S0^ until pink oolor Just disappears. ; NOTE: If the sample is acldito phenolphthaleln, add 0.5 N NaOH until pink, then 0.5 N HaSO^ dropw^ae until the color Just disappears. 4. Add 1 ml. Chromate Indicator (NagCaOh) and titrate with standard Silver Nitrate solution (O.Otto>5 g. Cl/ml) to the first appearance of a permanent red coloration Record ml. AgNOa 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. 30 HeO* solution and mix well. b. Add 3 drops phenolphthaleln and 0.5 N NaOH until pink. o. Add carefully 0.5 N HeSO^ until the color Just disappears. d. Add 1 ml. Chromate indicator and titrate with standard Silver Nitrate solution to the samefend-point as for the sample. Record ml. AgNOe used. Calculation: Chloride (as ppm Cl) ml. AgNO^ for sample (Step 4) - ml. AgNOa for blank (Step 5;) x 5 The method is precise to + 5 ppm. Report the ohlorlde to the nearest 1 ppm. MONS 046239 i IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 108 Test Methods 11,147-53 Date: 8-27-53 By: SE,NPA:SMK Material :Arocloij s, Pyranols Inerteens, TCB,and ^ri-Tetrachloro- benzen^ Blends Test: Sampling procedure Method No.11,147-53 WOK Dept. No.233/ 246 Samples of the listed products are taken in the following way: A. Batch Samples (taken by men jin Dept.) Three 16-oz. wlde-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, Bc[kelite-screw-cap, bottles. Samples to be taken as per tableibelow: Material Reserve iSample Pyranol 1467 S.T. Lot - 3 X 5-pt. Bottle Car - 2 X 5-pt. II D. Lot - 2 X 5-pt. II Pyranol 1470 O.E.Compound No.1476 (Aroolor 1254) Pyranol No. 1478 S.T.Lot -'3 X 5-pt. Car -*2 X 5-Pt. D. Lot - 2 X 5-pt. S.T.Lot -i3 X 5-pt. Car - 2 X 5-pt. D. Lot -[2 X 5-pt. S.T. Lot -13 X 5-pt. II II (1 II ll V (Trlchiorobenzene) Car -i3 X 5-pt. O.E.Compound No.1482 S.T.Lot -13 X 5-pt. (Aroclor 1260) Car - 2 X 5-pt. Pyranol No. 1488 D. Lot - 2 X 5-pt. S.T.Lot -|3 X 5-pt. II (60f Aroolor - 40J<TCB Car -j2 X 5-pt. Tri -Tetrachlorcbenrane Blend Car(only)-j 3 X 5-pt. Inerteens S.T.Lot -! 3 X 5-pt. Car -12 X 5-pt. II II II D. Lot -|2 X 5 Pt. * Advance samples to be sent on!request only. Advance Sample 1 x 5-pt. Bottle 1 x 5-pt. " 1 x 5-pt. " 1 x 5-pt. 1 x 5-pt. " " 1 x 5-pt. " 1 x 5-pt. 1 x 5-pt. " " MONS 046240 IX, SPECIFICATIONS AND TEST 'HODS, contd. IX - 109 Test Methods 11,147-53 Sampling Procedure for Aroclors^ Pyranols, Inerteens, TCB. and TrlTetraohlorobenzene Blends, Method No. 11,147-53, contd. Osneral 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 pottles are returned to the carton until needed. 2. Whan ready to sample, remove a bottle from the carton and wipe off with a clean, dry towel (aep Note 1 at the end of method). Procedure for Car Sampling; 1. Attach bottle to the clean Stainless steel sampling rod (see Note 2 at the end of method). NOTE 1 The bottle Is attached fisniy so that It can not swing, to one end of the rod, with the nepk toward the handle of the rod. 2. After the department man hap opened the car dome, remove the cap from the bottle and Immediately plunge the bottle, neck up, at least 12 to 18 Inches beneath tpe surface of the material in the dome. Allow the bottle to fill1 completely. 3. Withdraw the bottle and empty the contents Into a bucket. NOTE; The bucket oontent is laper thrown away . 4. Repeat the filling of the; bottle from the car and emptying into the bucket three timeB (Step 2 pnd 3). 5. Plunge the bottle again lhto the car, fill it completely with the material, remove from the car, pour out few milliliters of its contents to rinse the Inside ofi the bottle cap, allowing the drip pings to fall into the bucket. 6. Cap the bottle 'with the rlpsed cap and remove from the rod, wipe clean and label. > MONS 046241 \ \1 f IX. SPECIFICATIONS AND TEST* 1 2 3IOPS, oontd, ix - no , *Test Methods 11 1 7-53 Sampling Procedure for Arcclors,! PyranolB, Inerteens, TCB., and TrlTetrachlorobenzene Blends, Method No. ll,1^7-53 eontn ' Procedure for Storage Tank (S.T.j) 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 oar 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) Rampling; 1. Sample directly from drumB{designated by the department. Take a composite sample of the ^ot. 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 BOTtatS for the standard 5-pint, narrow- neck, amber sample bottle fltte<p with the factory metal-lined screw oap. - NOTE: 1: In Dr. R. L. Jenkins) memo to Mr. D. L. Uynon, 9/26/47, In which Clegom's method of sampling is Included, "diaper cloth" Is used. Mr. J. P. Stickley 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 Clegom's method of sampling Is included, "a clean hardwood etick about 1" x 1" x 4'"is use|l. Mr. J. F. Stickley has approved the method as here modified. HONS 046242 IX. SPECIFICATIONS AND TEST [QDS, contd. IX - 111 Test Methods 11,321-54 and 11,323-54 Date: 2-25-54 Mate.v.u.. : Montars Method No. 11,321-54 By:SE,NPA:SMK Test: Appearance WOK Dept. No. 246 Montar Is usually brown to blacl<j lumps or chunks. 1. Examine the content* of the sample bottle and describe Its appearance. Report as blaok chunks or otherwise if appropriate. 2. Observe the sample for visible foreign bodies, such as rust, wood, lint, etc. Report as none,j very slight, slight, moderate, or considerable. Describe appjearance of impurities briefly. Date: 2-25-54 Material: Months Method No. 11,323-54 By :SE,NPA;SMK Test: Non-Volatile Residue at! 800'C.1 WOK 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 800*p., 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 r.o longer given off. 3. Place the crucible In the muffle and heat at 800Cc.for 45 minutes. 4. Cool the sample In a desiccator and rewelgh accurately or. an ana lytical balance. Record weight of the crucible. Calculation: H Non-Volatile Residue at 800*0 f - ' Weight of Crucible {step 4) - Tare (Step 1) x 100 Weight of fample (Step l) " Report the result to the nearest;0.01#. MONS 046243 IX. SPECIFICATIONS AMD TEST METHODS. contd. Date: 9-21-54 Material: Gejneral Me-.tod By: WMK, LJW, WJO WWKsWJQ Test: Visdoslty IX - 112 Test Methods 11,433-54 Method No. 11,433-54 WOK O.M. No. 251 Part A: Saybolt Universal VlBcoalty by Saybolt Viscosimeter, 1. Take a scrupulously clean, dry 60-ml. viscosity receiving flask from the oven and allow It t|o 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 i 2. Clean the vlscosimeter/as fallows: A. Insert the cork, which should be clean and in good condition, in place in the bottom qf the tube. B. Carefully pour enough benzene into the tube so tl at 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 I 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 through C Inclusive. E. Permit the viscosimeter tube to drain and dry. ABSOLUTELY DO NOT INTRODUCE A CLOlTf OR KLEENEX INTO THE TUBE OR GALLERY KOF. BLOTTING UPj RESIDUAL LIQUID. HONS 046244 I r ' IX. SPECIFICATIONS AND TEST METHpDS, oontd. IX - 113 ,Test Methods 11 433-54 General Method, Viscosity, Methodj No. 11,433-54, oontd. F. Plush oa. 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 a|bove. 0. Drain this out, and'again flush with a fresh portion of sample to make certain arjy 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 orlfl|ce should be free of fibers or any other obstruction. If tlpeae are present, they should be removed by flushing wlthlsample only, not by use of wires. If flushing with sample fall8, Inform the supervisor. ADDITIONAL PRECAUTIONS; A. See that the bath oil, when hot. Is not less than 1/4" above the level of the overfloijr rim of the gallery of the tube. B. The bath oil should be algrade of light-coloured mineral oil which has a viscoslti of 40 + 5 Saybolt seconds at 210P. and should be replaced wlpen It displays a definite darkened colour. C. For viscosities^ to be ruiji at 100F. the bath oil temperature shall not exceed 100.25? (+ 0.05"F. for 10 Min.). For vis cosities determined at 1I0*F., the bath temperature shall not exceed 130.30F. (+ 0.05PF. for 10 Min.). For viscosities determined at 210F, the'bath shall not exceed 212.0F. (+ 0.10*P. for 10 Min.) D. Use only thermometers standardized to the nearest 0.01F. against a National Bureap of Standards thermometer. E. Use only the st.cpwatch provided for timing purposes, which should be accurate to within 0.1 percent when tested over a 60 minute period. Eleptrical timers must not be used unless the available power sourjce Is known to be of sufficiently HONS 0462A5 l IX. SPECIFICATIONS AMD TEST METHpDS. contd. IX - 114 Test Methods 11,*33-5* general Method,Vlsooslty, Methodj No.11,433-54, contd. E. Contd. i accuratefrequency. The(stopwatch must be left in the holder provided, since variations in its position can cause error, : F. Never use the plunger, eimmonly provided, for cleaning the instrument and never expose the viscosimeter to a draft during a determination, j 3. Blot the cork dry with a lin ree cloth and insert it in the tube. Pour ca. 150 ml. of s le into a scrupulously clean beaker which has been rinsed _th sample, and heat the contents to not over 7*P. hotter than the temperature of test. Do not use a sample which has overheate|d, even if it is then cooled to with in the prescribed range. i I 4, Four 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 + 0.02*F. of the desired temperature for one full minute (with constant stirring). ; NOTE! Stirring is-a very critical point, especially in the case of more viscous liquids sucp 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. MUNS 046206 ' IX. SPECIFICATIONS AND TEST METHCjDS, contd. XX - 115 Test Methods 11,*33-5* Oeneral Method, Viscosity, Method iNo. 11,455-54, contd. 5. contd. Regulate the temperature of trie sample while stirring, by adjusting the oil bath until the desired reading holds constant within + 0.02P 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 li Inserted at one point In the gallery without touching the (ver-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 ijhe 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 sam4 Instant that the bottom of the meniscus of the sample reached the mark In the neck of the receiving flask. - 10. Examine the end of the cork t6 see If It has become moistened with sample. This would denote an Incomplete seal and a pre mature seepage of sample though the orifi ce which would produ< c erroneous 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 HONS 046247 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 116 Test Methods n.'tJJ-S't Oeneral Method, VlBcoslty, Methoiji Mo. 11,433-54, contd. OPERATION OP THE TAP 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 befori making a test. This will allow the metal parts of the viscoslmeier 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 polrlts 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 deem 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 ami 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 qablnet. 2. Adjust the constant temperature bath to the desired temperature. holding the temperature within + 0.05"F. 3. Place a 1 x 6 inch test tube; Inside a 500-ml. suction flask. Insert a medium porosity Sel^s glass crucible into the rubber adapter. Place the adapter [In the top of the flask with the MONS 046248 I IX - 117 Test Methods 11,433-54 IX. SPECIFICATIONS AND TEST 'HODS, contd. general Method, Viscosity, Methjid No. 11,433-54, contd. 3. contd. glass tube extending Into thfc test tube. Filter, by suction, enough of the sample to fill!the 1x6 Inch test tube ca. 3/4 full. Have the sample hot ejiough 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 plabe the capillary side into the filtered sample contained In the test tube. C. Using gentle suction dr^w enough filtered sample to fill both bulbs and Into the'capillary up to the mark etched on It. D. After loading, the tubeiis turned right side up, vacuum removed, and the excess!sample Is wiped off the viscosi meter tube. Modified Ostwald Viscosimeter Approximate Viscosity Range Centlltokes Saybolt Universal Seconds Series 50 Series 100 Series 200 Series 300 Series 400 Series 500 0.8- 3 3 -10 10 - 70 25 - 175 120 i- 850 800 ;-5600 ------------ 1------------- 35 - 65 60 - 325 120 - 800 550 -4000 3600 - 25,000 MONS 046249 IX. SPECIFICATIONS AND TEST METHODS, oontd. general Method, Vlsooslty, Met; No. 11,433-54, oontd. ix - u8 ,^Test Methods 11 53-54 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 tj-o come to temperature equilibrium in the bath. 10 minutes wijll be the minimum time required for this. 7. After the sample has attained bath temperature, apply vacuum to the capillary arm and draw the sample 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 menlaous to pass from the vjpper to the lower mark. This is efflux time, t, in seconds< 9. A oheck 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 samble 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 SemPerature bath to 100 + 0.05F. B. For the standard oil I use API or NBS oil. C. Repeat Steps 3 through 9 above. MONS 046250 IX. SPECIFICATIONS AMD TEST ME] [ODS, contd. IX - 119 Test Methods 11,433-54 general Method, Viscosity, Methpd No. 11,433-54, contd. D. Using the viscosity (Vi), In centlstokes, marked on the standard oil lable, calculate the tube constant (C) as follows: where C - Calibration constant at 100`F.for the tube i tested. V - Viscosity of the oil In centlstokes, and t - Efflux time In seconds. E. Determine the constant: in duplicate. Duplicate efflux times should be within! 0.2 seconds. F. To determine the calibration constant on a tube at other temperatures use the fallowing equations: Calibration constant ajt 210*F. (98.89C.) = 0.996 x calibration : constant at 100'F. (37.T8*C.) Calibration constant a|t 130F. (54.44*C.) - 0.999 x calibration constant at 100'F. (37.78'C.) Calibration constant ajt 60*F.(15.56*C.) 1.001 x calibration constant at 100F. (37.78*C.) 12. To convert from kinematic piscoslty in centlstokes to Saybolt viscosity in Saybolt Universal Seconds consult either the attached graph B-7781* or [aSTM D-446-39. 13. The following equivalents pre frequently used In connection with viscosity conversions: Poise Centlpolse Stoke Centlstoke Centlpolse Reyn (1 lb > c.g.s. Unit of absolute viscosity 0.01 poise c.g.s. unit of kinematic viscosity - 0.01 stpke - oentistpkes x density (at temp, under con - sideratlon) sec. per s|q. In.) - 69 x 103 centlpolses. Reference: ASTM D-445-46-T and (>-446-39. See page IX - 6lb, above. HONS 046251 I IX. SPECIFICATIONS AND TEST METHODS, contd. 1 Date: 9-25/52 Material: Trlchlorobenzene IX - 120 Test Methods 11,505-52 Method No. 11,505-52 By: LDP, DKL, NPA:3MK Test: Stability1 2 * 4 WQK Dept. No. 225-246 1. Rinse a clean, dry, 500-mli, g.g.s wlde-mouth Erlenmeyer flask twice with a few ml. of the Triohlorobenzene (TCB) sample. Weigh on a beam balance the flask and add 290 (+ 0.05) g. of the sample. Set the dlp-plpe Into the flask making sure the dlp-plpe Is not touching tjie 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 water, 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 dlp-plpe, 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. 5. The Dewar bottle space is [filled with dry Ice and methanol around the condenser trap.j Use ca. 5" of methanol, then orushed dry Ice to the ton. 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 tap 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, oJ 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, 5/16" I.D. l/l6" wall -- dc 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|trierssyl phosphate. HONS 046252 IX. SPECIFICATIONS AMD TEST METHODS, contd. IX - 121 Test Methods U.503-52 Stability Test for Trlchlorobenzene. Method No. 11,303-52, oontd. 5. Cover the parts of the assejmbly (excepting the absorber bulb) that are above the bath top with aluminum foil to exclude light, whloh 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 varlac operatinjg the main bath-heat souroe and adjust heat to approximately 210*C. with this source alone. The stirring motor for the bathf 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-lraner- slon heater: syateiv is''plugged In and the bimetallic thermo- regulator Is adjusted as follows: Loosen locking screw In the base and rotate the Bakellte head until the pointer Indicates the temperature desired on ie graduated scale. Relock the head by tightening this loc ng screw. At the Instant the desired temperature is obta ed, the red contact screw-governing setting should be turned so hat It Just touches Its contact arm button. Usually only a sma part of a turn of the adjuster will be sufficient. : NOTH: This thermo-regulatbr 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 11he 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 mil alr/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 beiused to make small changes. Usually, however. It should not be necessary to change the setting of the regulator. MONS 046253 l IX. SPECIFICATIONS AND TEST MEI' fHODS, contd. IX - 122 Test Methods 11.505-52 Stability Test for Trlchlorobenzene. 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 appearingjlater In this method on use of electrode, care, and source^ of trouble). Occasionally (every 2 or 5 days) It Is necessar^ to clean the silver wire electrode by dipping It In dilute nitric acid and sanding with fine sand paper. CAUTION; Do not use emery dloth. Emery cloth contains impurities whloh will affect the electrode potential. 9. Rinse off electrodes by placing a 100-ml. beaker of distilled water under electrodes and t|urnlng 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 50-78 ml. of the methanol, placing the beaker under the electrodes, turning on the agitator, ana 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 AgNOs reduce the potential to 60 mv. or less, and methanol Is good enough to use. Dlsqard the beaker contents. NOTE: If the methanol Is ndt 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 example Is two 8-hour periods. At the end of the first 8-hour period, remove the first absorber without turning off the air, and poujr Its contents Into a 100-ml. beaker which has been cleaned by rinsing with 1:4 HNOs, then distilled water. Rinse Into beaker, apdlng a total of 50-75 ml. of methanol, and titrate to a potential off 60 mv., using 0.005 N. AgNOs. j 12. The absorber must be rinsed Iwell with distilled water, 20 ml. of water then being added to the flask, and water removed from Joints with tissue, as before. Thej absorber Is then placed back on the dlp-plpe for the second 8 hojur period. MONS 046254 l  IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 123 Test Methods 11.503-52 Stability Test for Trlchlorobenzene. Method No. 11.503-52. contd. 13. The contents of the otherjabsorbers are then treated as des cribed In Step 11. 14. At the end of the second ^ 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 dlp-plpes with alcohol and distilled water and place in the oven to dry. The Dow Coming fluid levql should be maintained 1 inch from the top of the bath. , During any run where onlyjone or two flasks and assemblies are In use, the remaining positions are occupied by dummy flasks to maintain the proper bath }evel. Calculation: Parts per million chlorides - ml. 0.005 N AgN03 x 0.61 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 anothe*. Report results to the nearest (p.l ppm. NOTE: If the chlorides on batih samples are greater than 1.0 ppm determlnealso Stability by Metaod No. 10,126 (O.E.) on the sample filtered through Attapulgus eafth. Preparation of Solution and Apparatus: 0005 N AgNOa: The sliver nltfate solution is made up by adding 50.00 ml. 0.01 N AgNOs from a JO-ml. volumetric flask (painted black), to a 100-ml. volumetric flask (also painted), and diluting to the mark with distilled wat^r. This solution Is prepared by the Analytical Section. Moms 046255 ` IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 124 Test Methods U.503-52 Stability Test for Trlchloroben^ene, Method No. 11,503-52, oontd. Checking the electrode system: j Standard chloride solution may be prepared to check the electrode system in case the cell exhibit* abnormal behavior. To make 1.00 ppm standard, add i.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 AgNOs. Calculate the parts per million chlorides indicated by the titration and oompare with the standard value. Fresh standards should be prepaid from time to time. Calculations for 1.00 ppm std; ml. AgNOs req d. ,, 1.00 ppm 1.64 ml. ; 0,6l Use of mercurous sulfate electri le t 1. Do not place electrode too near the heating bath. Evaporation changes the normality of th| KaSO^ solution. 2. Before refilling electrode ilrlth potassium sulfate from the volumetric flask, pour a srn^ll amount over the lip to avoid contami nation. 3. Remove all air bubbles from I 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. Som4i times potassium sulfate crystallizes around the plug, preventing good electrical contact. Remove rubber stopper before looseiiilng plug to allow solution to drain freely. 6. Make certain mercury In outir arm is In contact with platinum wire which connects outer aipn with Inner electrode system. MONS 046256 IX. SPECIFICATIONS AMD TEST IOPS, oontd. IX - 125 Test Methods 11.505-52 Stability Test for Trlchlorobenzene. Method No. 11,503-52, oontd. 7. Always keep stop-oook open ljhlle electrode Is being used. 8. Always keep rubber stopper l|n place when making a run, and never leave stopper off very long.! The atmosphere may contaminate the electrode. 9. Always leave electrode tip Ip a beaker of distilled water when not In use. NOTH! A second electrode has beien prepared In case the first one should be broken. This electronje Is kept In a labeled box in the Aroclor Room. It Is advisable to drain out the KeSOjj solution and refill the new electrode with f:'besh solution before using. Preparation of a New Mercurous Sijlfate Electrode: Before filling the new electrode, clean thoroughly with dilute nitric acid and rinse with distilled wqter followed by potassium sulfate solu tion. Reagent grade meroury is added to outer am with an eyedropper. Make sure the mercury is In contact vpth platinum wire at the bottom of am. Punch a hole In a rubber policertan and fit ever arm of electrode. In sert a piece of clean copper wire about 3 Inches long. One lead wire from potentiometer Is connected |to wire. Other lead wire Is connected to sliver metal electrode. Add enough reagent grade mercury to Inner electrode bulb to cover *the platinum wire. Add about 1, Inch of mercurous sulfate, reagent grade, which has previously been washed with normal potassium sulfate solution. Rill the electrode wj| th normal potassium sulfate. CAPTION: Mercuric sulfate Is a Ipolson to the electrode. Mercuric Balts can be reduced by leaving |ln prolonged contact with mercury and KgSO^ solution. Methanol Still: Using methanoljfrom the can, fill a large round- bottom flask full. Add ca. I5 grams Sodium Hydroxide pellets. MQNS 046257 IX. SPECIFICATIONS AND TEST METHODS, oontd. IX - 126 Test Methods 11,503-52 Stability Test for Trlchloroben^ene, Method No. 11,503-52, oontd. Methanol Still: oontd. : Use a distilling column packed ilrlth glass helices and a waterjacketed condenser. All Joints are glass-to-glass. Do not use rubber. A bulb-shaped funnel oif receiver end of condenser protects methanol from air contaminationj 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, j Discard first 100 ml. distillate. Run a blank test on the next 50 ml, of methanol; 0.02 ml. or less of 0.005 N AgNOs 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 npck, as bad air In the bottle will spoil the methanol. Use either p 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 en|d point of the titration. When bottle Is full, cover cap w)Lth aluminum foil. When bottle of distilled methanol . is put Into use, uBe Blphon arrangement on shelf In Aroclor 1 loom. The system consists of two empty traps with "breather" bottj ,e between containing alcoholic caustic to absorb chlorides and J 'CB vapors. It is necessary to occasionally refill the alcohollj caustic bottle with fresh solution, If good distilled methanol Is no available, undlstllled reagentgrade methanol from MalUnckrodt ihemlcal Company can be used. The methanol must be tested before ul e, however. MQNS 046258 XX. SPECIFICATIONS AND TEST 'HODS, contd. IX - 127 Tea*: Methods 11,503-52 Stability Teat for Trlchlorobehzene, Method No. 11,503-52. contd. A. Bath B. Stirring Motojr C. Main Heat Varjiac, 20 amp. cap. D. Dewar flask containing cold trap. E. ThermoregulatOr F. Bubbler (Air). 0. Flask, 300 ml. H. Dip Pipe I. Absorber Bulb J. Relay (Amlncc^ # 4-37 OB) K. Reserve D-C ifluld L. Mercury Manonjeter M. Clamp adjustnjent for air flow. MONS 046259  IX. SPECIFICATIONS AND TEST METHODS, contd. Date! 5/24/54 Material! Arojslors: 1142, 1148 By: IDF,NFA,QWM: WJO Test: Acid Number IX - 128 Test Methods 11,532-5* Method No.11,532-54 WOK Dept. No. 246* 1 2 3 4 5 6 This method is used for all dar^c-coloured Aroclors (mainly crude Aroclors). 1. Weigh accurately on a beam balance a 10(+ o.05)g. sample by difference into a clean, dr|r 400-ml. beaker. Record weight of the sample. 2. Add 100 ml. of Carbon Tetrajshlorlde (CClj,) and 100 ml. distilled water, previously Just neutralized with 0.01 N KOH, using Phenol Red indicator. 3. Stir 4he solution with a glkBS rod until all the Aroclor is in solution. Transfer the concents of the beaker to a 850-ml. separatory funnel. Shake apd allow the layers to separate. 4. Draw off the lower (Aroclorj-CCl^) layer into another 250-ml. separatory funnel, and the water layer (containing free add) into a clean, dry 400-ml. bpaker. 5. Add another 100 ml. of neutralized (as above Step 2) distilled water to the seoond separatpry funnel, shake and collect the water layer in the same-beaker as' before (Steps 3 and 4). Combine water extracts. ' 1 6. Titrate the combined water Extracts with 0.01 N KOH solution to Phenol Red end-point. Reoopd ml. KOH solution used. CALCULATION! Acid Number (mg. KOH/gram of sample )= ml. 0.01 N KOH (Step 6) x 0.56 Sample Weight (Step 1) Upon request only, convert Acid; Number to mg.NaOl^.ln 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. 1 MONS 046260 [ IX. SPECIFICATIONS AMP TEST MfTOODS, contd. IX - 129 Test Methods 11,533-53 Dates 2-26-53 Material: Pyifanol 1467 and 1470 Method No. 11,533-53 By;Se,NPA:SMK Test: Tin Tetraphenyl1 2 3 4 WOK Dept. No. 246 f CAUTION: This method Is not a.;pplloable to product containing more than 0.00355* water. Determine results on two separately weigheu samples. Blow the funnel with dry air 10 minutes. Procedure: 1. Weigh on a beam balance by[difference a 15 (+ 0.05) gram sample (approx. 10 ml.) at 25*C. from a 10-ml. graduate Into a 125-ml. separatory funnel. 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 separatory funnel so that any spatter drops are washed down. NOTE: A tube drawn to an ^lmost capillary tip Is desirable for the bubbling. 3. Leave the capillary tip InI the funnel and bubble dry air through the sample for 30 min. to sweep out excess HC1. Dry the air over Drlerlte. Occasionally rotate the separatory funnel so that any spatter drops ar washed down. Check for complete removal of HC1 by odour. Do not remote air line from funnel. 4. Plpet 25 ml. of distilled irater into the funnel, allow to blow for 1-2 minutes and then!withdraw air line. 5. Stopper funnel and shake vigorously for 2-3 minutes. 6. Allow separation of layers; and decant bulk of water layer Into a clean, dry 100-ml. beakef. 7. Plpet Into the funnel anot visr 25-ml. portion of distilled water, shake vigorously as before, allow to separate, discard the Fyranol layer and combine the water extracts. HONS 046261 l IX. SPECIFICATIONS AMD TEST METHODS, eontd. IX - 150 Test Methods 11,535-53 Test for Tin Tetraphenyl In Pyranol 1467 and I*>70, Method No. 11,555-55 eontd. 8. Mix the water extracts and Jlpet a 20-ml. portion Into a 250-ml. Erlenmeyer Flask. 9. Add 50 ml. distilled water And 5-5 drops of alcoholic phenolphthaleln Indicator solution (1 g. Indicator to 100 ml. 95# ethanol) and titrate with ojoi N NaOH until pink colour remains for 5-10 seconds. 10. Determine a blank titratlonjwith 0.01 N NaOH on 70 ml. of dis tilled water. NOTH: The distilled water used|for the blank and samples must be taken from the same containers.1 Calculation: # Tin Tetraphenyl - (ml. NaOH.Step 9 x Normality)-(ml.NaOHaStep 10 x _________ Normail-.lty) x 40 x 2.5______________ Sample Weigh?(Step 1) x Empirical Factor (last page of method) Report the result to the nearest 0.001# t Determination of Bnplrloal Factor for Tin Tet,raphenyl Analysis In Pyranols 1467 and 1470? I Introduction: In the prooess of blending Pyraiol 1467 (or Pyranol 1470), the manu facturing department will send a 1/2-gallor. sample of Pyranol 1488 (or Trl-Tetrachlorobenzene Blena-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 faot a pilot run for the manufacturing department, all materials must be the same as proposed to use In the plant production. MGNS 046262 l IX. SPECIFICATIONS AND TEST METHODS, contd. IX 131 Test Methods 11,533-53 Test for Tin Tetraphenyl In Fyrjthol 1467 and 1470, Method Wo. 11,533-53 oontd. Procedure: 1. Weigh on a beam balance a cjLean, dry 16 oz. wlde-mouth bottle. 2. Rinse the bottle twice with!about 100 ml. of Pyranol 1488 (or Tri-Tetra-Aroclor 1260 Mixture for Pyranol 1470) sample. 3. Pill the bottle approximately two-thirds full. 4. Rewelgh the bottle with tr cj sample and obtain the weight, of Pyranol 1488 (or Trl-Tetra-|roclor 1.260 Mixture) being used. Record the weight. 5. Calculate the necessary amount of Tin Tetraphenyl powder to give a 0.130j< solution of Pyranoj 1467 (or Pyranol 1470). Tlr. levraphenyl (grams) g. at Pyranol l488(or Trl-Tetra-Aroolor 126^ Mixture) x 0.00130 Reoord calculated weight of Tin jTetraphenyl. 6. Weigh accurately on an analytical balance, using a watch glass, the amount of Tin. Tetraphenyl calculated in Step 5. 7. Brush the powder from the watch glass into the bottle containing the Pyranol 1488 (or Trl-Tet|ra-Ar-sclor iP6o Mixture). 8. Effect complete solution byjheatlng to approx.60*0. w!rb constant agitation. This should take about 1 hour and is minutes. 9. Analyze Pyranol 1467 (or Pyranol 1470) prepared by the above procedure, for Inorganic ,F(ee) Chlorides according to Method No. 10,118. Report the result 1[o Department a-246. 10. Analyze the Pyranol j. e 67 (pjf Pyranol 1470) in the regular manner (Procedure at- the beginningjcf this method) as for Tin Tetraphenyl content. Calculation: Expiries! factor ml. NaOH x Normalityx 100 Sample Weight used x 0.130 Report the result to the nearest 0.001. MONS 046263 IX. SPECIFICATIONS AND TEST METHODS, eontd. IX - 132 Test Methods and U Date: 4-22-54 Material: Tin (Tetraphenyl Method No. 11,565-54 By: SMK,NPA:WJQ Test: Appearance and Colour WOK Dept. No. 246 Tin Tetraphenyl Is usually a white to light cream colored powder. 1. Bxamlpe the sample and describe its appearance noting any unusual characteristics. Report as white powder or otherwise if appropriate. 2. Examine the sample for vlBlble foreign bodies such as rust, lint, wood, etc. Report as| none, very slight, slight, moderate, or considerable. Describe appearance of Impurities briefly.1 3. Report presence of lumps and moisture also. Date: 4-22-54 By: SMK.NPA WJQ Material: Tlr: Tjetraphenyl Test: Meltihg Point Method No. 11,566-54 WOK Dept. No. 246 1. Place 2 g. of the sample in an agate mortar and grind to a fine powder. 2. Pill a melting point tube, Iwhich has beer, sealed at one end, with the sample to a height of ,y4 inch. 3. Place the melting point tutje In the melting point apparatus, fastening the tube to a 125 t0 235C. thermometer. 4. Determine melting point according to Qeneral Method No. 3 (Method No. 10,052) with thje following modifications: 5. Regulate the temperature tcj give a rise of 0.25*C. per minute. 6. Report Bettering Point, Meeting Point, and Complete Melt. 7. Duplicate determinations sfy>uld check to within + 0.25*C. Report the result to the nearesjt 0.5C. MONS 046264 ` IX. SPECIFICATIONS AMD TEST METHODS, contd. IX - 133 Test Methods 11,568-5^ Date: 10-6-54 Material: Tin;Tetraphenyl Method No. 11,568-54 By: WMK,WJQ,NPA PLD,RPS:WJOTest:ChjtorldesWOK Dept. No, 246 1. Weigh a 20 t 0.1 g. sample;Into a 500 ml.g.g.s.Erlenmeyer flask. 1i 2. Add 350 ml. CP monoehlorobknzene and heat on the steam bath until the sample dissolves. Occasional swirling of the contents will speed solution. 3. Transfer solution to hot, 00 - 100C., 1-11ter separatory funnel. 4. Rinse flask with 100 ml. hk>t water Into funnel. Shake for one minute venting carefully through stopcock. 5. Transfer bottom layer (mon^chlorobenzene - TTP) to second hot 1-llter separatory funnel. 6. Add 50 ml. hot water and ejctraet as before. 7. Draw off bottom layer and discard. 8. Combine H*0 extracts and transfer to 250-ml. beaker. 9. Cool to room temperature, hdd 3 drops oono. HNOs and 50 ml.2-B alcohol. : 10. Chill in Ice bath and titrkte potentlometrically using 0.0333 N AgNOs from a 5-ml. mlcropurette. NOTE: Add AgNOs In 0.10 mjl. 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 AgNOs vs. emf (mv) as follows (see Plg.l): HONS 046265 ' , IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 1}4 Test Methods 11,568-54 Chlorides Test for Tin Tetraphenpl, Method No.11,568-54, oontd. 12. oontd. . a. Draw line AA1 through the top plateau. b. Draw line BB' through the bottom plateau. c. Draw line CC' through the step. u. Draw lines DD' and EE'I through points 0 - N and parallel to the horizontal axis. e. Draw lines FF' and 00'j through points 0 and N and parallel to the vertical axis, i f. Draw line HH' through bolnts M and P. g. Draw line JJ1 through point of Intersection L and parallel to the vertical axis.i>.0335 h. Read the volume of 8XU N AgNOs from the intersection >of line JJ1 with(he horizontal axis. Calculation: ppm Chlorides {ml. AgNOs (sample) - ml. AgNOs (b lank ))x. H x 0.035457 x 10*** * 106 - 1,000,000 ' MQNS 046266 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 135 Test Methods 11,605-54 Date: 10/2/54 Material: Arodor., Pyranols, Inez 'teen, Tri-tetra- By: CM, UW, MPA ohlc:robenzene Blend WWK:WJQ* 1 2 3 4 Test: Dleleot;rlc Strength + Introduction: Method No. 11,605-54 WOK Dept. No.246/233 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 lndloate the presence of contaminating agents suoh 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. Ascertain that temperature I of the material under test Is 25 (0.5) *C. Exception: For Arooler 1260 only the temperature of the material under test will be 50 + 1*C. 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 cu. NOTE: This operation is even more Important with used than new oil as the impurities may fettle 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 tested. 4. Immediately after final rinse, fill the cup to a height of not less than 20 mm. (0.787 in^) above the top of the eleotrodes. MONS 04626 7 IX. SPECIFICATIONS AMD TEST METHODS. contd. IX - 136 Test Methods 11,605-5* Test for Dielectric Strength ofi Aroclor, Pyranols, Inertsen. Trl-tetraohlorobenzene bland. Method No. 11,605-54. oontd. 5. Rook the oup a few times ljn order that any entrapped air may escape. Close cover over pll test cup. 6. Allow to stand 3 minutes. \ CAUTION: THIS 18 IMPORTANT! 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 glojw. NOTE 8 The green signal ljlght Is connected across the 113 volt ln-put and denotes that line voltage has been applied to operating control circuit. Amber light Is connected lh 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. 6 Turn voltage control (largfe knob on front) to extreme counterelookwise position. 9. Depress red botton on fronk.d This energizes high voltage trans former and olrcult breakeivls Indicated by amber light going out and the red light dlrectlyf 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 rlscj at a rate of 3 K.V. per second. 11. Note and Record the voltmejter reading at breakdown. IS. Repeat the test until two (successive breakdowns occur on each .of two fillings of the teat cup which do not differ by mere than 100 Report the average value of th^se two readings (Step IS) as the Dielectric Strength. If the limit of the Instrument |ls reached before breakdown, report the Dielectric Strength as/ 50 K.V. at 25*C. or^50 KV. at 50*0. for 1260 Aroclor. HONS 046268 IX. SPECIFICATIONS AND TEST [OPS, oontd. XX - 137 Test Methods 11,605-54 Teat for Dielectric Strength of Aroc lor, Fyry.ols. Inerteen, Trl-tetrachlorobenzene blend, Method Mo. 11,605-54. oontd. Cleaning of the teat cup: 1. After the teBt- la completed, drain the cup. 2. Flush the cup with benzene. Use warm benzene after the 1260 teat. 3. Then fill with Aroolor 1240 land let stand until the next analysis. MOTE! 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 the lhoh with Index notches on both the electrodes and the lock nuts. To set the Oap; 1. Arrange one of the electrodes; and the lock nuts with the index marks in line. ^ 2. Move the other electrode until 1 it, comes in firm contact with the first electrode and lock It. 3. Now unscrew the electrode with the index marks In line (Step 1) two complete turns and look At. This will leave a gap of C.1 Inch between faces of the electrodes. Cleaning of the electrodes and tKe*~teat. cup free of carbon coating; The following ASTM method of cleaning shall be followed when it is apparent from visual inspection phat the electrode discs of the cup are coated with carbon. HONS 046269 1 IX. SPECIFICATIONS AND TEST [OPS, ocntd. IX - 138 Test Methods 11,605-54 Test for Dielectric Strength of Aroclor, Pyrands. inerteen, Trl-tetraohlorobenzene blend. Method Mo. 11,(505-54", 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 |f the tissue paper whioh have been In contact with hands. . 2. Rinse the electrodes and cub with dry lead-free gasoline, Stoddard Solvent (or dry, water white Kerosene) until they are entirely clean. Care should bp taken not to touch the eleotrodes or the Inside of the cup after cleaning so as to avoid possible contamination. ! Apparatus; general Information: The eleotrloal equipment necesaaby to provide high voltage to permit the determination of dielectric ^trength of liquid dielectric at commercial power frequencies is basically quite simple. The equipment was assembled In the W.C.K. Plant laboratory and con sists of a high voltage transformer of good design and with a current oapaclty 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 open tar. It la enclosed In a steel grey cbacfcle finished cabinet measuring 42" high, 22" wide 17" deep and set pn 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 oil 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 cup: Transfers***. Voltmeters, and Accessories HONS 046270 I . ; IX. SPECIFICATIONS AND TEST METHODS, oontd. IX - 139 Test methods 11,605-54 Test for Dielectric Strength of Aroclor, Pyryiols, Inerteen. Trl-tetrachlorobenzene Blend, Method No. 11,605-54. contd. The oil testing cup type No. 224009 supplied by Oeneral Electric Co. Is mounted on the top rear of the cabinet. It is protected by a heavy plastic cover, hinged at tjhe rear for acceasablllty to the reeeptloal. It Is equipped with safety contalotor so placed that the circuit energising the high voltage contractor can not be completed unless the protective cover Is completely lowered and In place. It Is Impossible for the operator or sjnyone 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 atj 400 mlllampers. It was recovered from a used X-ray machine, puroljaaed quite Inexpensively. An auto transformer from the seime X-ray machine Is connected so as to limit the output voltage of t[he high voltage secondary to 50,000 volts. The primary of the auto transformer Is connected to the secondary of a 2i KVA powerstat variable aute transformer supplied by the Superior Electric Company. ' power to the powmtat Is controlled by a 4 contact 30 amp. solenoid olroult breaker. The voltmeter mounted on top neir 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 coll of the solenoid cir cuit breaker Is wired through tpe contacts of this relay. HONS 046271 IX. SPECIFICATIONS AND TEST tODS. oontd. IX - 140 Test Methods 11,605-s'* Test for Dielectric Strength of Aroclor, Pyranols, Inerteen, Trl-tetraohlorobenzene Blend, Method Mo. 11,605-54, oontd. Safety and Operating Controlsi (a) Door Interlock switch located on rear door. (b) Oil test cup cover interlock switch. (c) Powerstat switch moiknted on rear or unit arranged so that high voltage contactor can not be closed unless powerstat is at zero position. (d) Main power switch 01^ front panel. Fowerstat voltage control on front panel. I (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. /-------------------- 1-------------------- / MOMS 0*6111 IX SPECIFICATIONS AND TEST contd. Dates 5-24-54 Material: jAroclors, Pyranols By: CM, UV, NPA Test: and Inerteens Resistivity* I OWM:WJO________________________ _____________________ IX - l4l Test Methods 11,607-54 Method No.11,607-54 WOK Dept.No.246/233 Introduction: Consult Method No. 11,752 for this sequence of electrloal 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 re allstlvity Indicates high resistance to the passage of electrloal cuirrent and normally, but not necessarlly, establishes the absence of conducting contaminants. Procedure: 1. Assemble the test cell. Place the recently cleaned (within the last 8 hours -- see Method J4o. 11,751* Step electrodes In an 800-ml. beaker. , 2. Measure the capacitance of Ithe test cell (C ) according to Method No. 11,608 (Dlelectijlc Constant and ?ower Factor measure ments ). 3. FI11/fthe oell assembly untijl the liquid level Is 3/4 Inch above the top of the electrodes, i 4. Heat the assembly on the ho|t plate to 100 (+ 0.5 )*C. I-- 5. Plaoe the assembly Inside ojf the testing oven. 6. Attach top lead (+) on the fnegohm bridge to Inner electrode. 7. Attach other lead to outer jslectrode. 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. MONS 046273  i IX. SPECIFICATIONS AMD TEST METHODS. eontd. IX - 142 Test Methods 11,607-54 Test for Resistivity of Aroolorat, Pyranols, and inerteens. Method Mo. 11,607-54, contd. I 9. contd. DANOERt Make sure control ^nob Is In "CHECK" position. Otherwise painful shock will result. 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 lmob to "CpAROK" position for one minute. 12. Turn the oontrol knob to "OPERATE" position and return the galvanometer pointer to zerjo by adjuetment of the "MULTIPLY BY" swltoh and the megohm dial.; 13. Read after one minute. Calculation! Resistivity* - megohm dial readlnlg (Step 12) x "Multiply By" readlng(8tep 11) x capacitance offcell (Step 2) In uuf. x 11.29 x 0.001 Report the result In units of 109; ohnv/cm3 . NOTE! It Is important -that the pfoduot under test, electrodes, and beaker be at uniform temperature for this determination. Temperature variations In different parts of the sample will cause the galvanometer zero to ohange constantly aid give misleading results. CAUTION i In as muoh as measure: its must be made at a potential of 500 volts DC a shook hazard exla In the handling of thlB apparatus, With the oontrol knob In the < and operate position full voltage of the bridge (500 volts) is app: .ed to the + and low terminals and through the test leads to the eli itrodes. Do not attempt to handle the eleotrodes or the test leads iless the oontrol knob Is in the "CHECK" position. Possible penall ;y for failure to observe this are- caution -- Painful Shook. * Values of resltlvlty are qualified by designation of temperature and voltage. These are for thjj.8 test, 100*0. and 500 volts DC. MONS 0462 74 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 14? Test Methods 11,607-5* Teat for Resistivity of AroolorsL Pyranols, and Inerteens, Method No. 11,t>07-54, oontd. Apparatus: general Radio Co. Megohm Bridge type 544-B. This la a combination of Wheatstone bridge and vaouum tube voltmeter for Indicating null. The direct measurement of resistance!up to 1,000,000 megohms Is made possible by the use of a vaouum tube detector whloh 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 oondltlon Is necessary to measure resistance properly. The accuracy of the Instrument lh the range encountered In the measurement of Aroclor resistivity, 100 to 1000 megohm Is + 6ft. The Instrument Is equipped with k 115 volt A.C. power supply which supplies all operating voltages Tor the bridge Indicating olroults and In addition supplies 500 V DC tor application to the material under test. The Instrument Is completely enclosed In a waxed finish shielded oak oablnet measuring 8i" wide, 22$ " long and 8" high. Approximate weight -- 26 pounds. Test Electrodes; Two oonoentrlc nickel cylinders Ifith feet, obtained from general Bleotrlo Company. The inner electrode has outside diameter of 2.8" and a height of 3.25" with area of 184 eq. cm. The outer eleotrode has Inside diameter of 3" and height of 3.25" with area of 198 sq. cm. The distance between electrpdes is, therefore, 0.1" or 0.25* cm. I By theory, eleotrode constant (k|) area/length is 191/0.25* or 752 where average area Is 191 sq. cm|. Also K - 36IT x IP11 x C (in farads with air as dielectric)- 11.29 x C (in uuf. with air as dielectric)!. glass Plate! Pyrex about 3i" dikmeter with concentric grooves to assist m spacing electrodes. Obtained from general Electric Company. Heating Unit: Assembled in the laboratory and Is the same unit described In Dielectric Constant Apparatus! (see Method No. 11,608; equipment). MONS 046275 IX. SPECIFICATIONS AMD TEST [OPS, contd. Date: 5/17/54 Material: Aroclprs, Pyranols, Inerteens, and fri-Tetrachlorobenzene Blends By: CM,NPA,QWM:WJQ : Test: Dielectric Constant and Power Factor* I IX - 144 Test Methods 11,608-54 Method No. 11,608-54 WOK Dept. No. 246 I. Adjustment of Controls on Electrical Apparatus I A. On Panel No. I (Top Pane|L, 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 6o cycles. b. Allow the equipment to warm up 10 minutes. e. Turn "OAIN CONTROL" to 6. d. Depress "NULL DET." button. e. Depress "INPUT> 0.03V." button i B. On Panel No. 2 (Oscilloscope) a. Turn "INTE1T." to aboujt the 12 o'clock position. CAUTION: Do not allolw a high Intensity spot to remain stationary on the screen for any length of time. b. Using "HOR. POSITION" and VERT. POSITION" control oenter the image or. the screen. c. Adjust "FOCUS" for sfiarp line. d. Turn "FREQ. SELECTOR" to 100 KC. e. Turn "FREQ VERNIER" to 80. f. Turn "VERTICAL <JAIN"j to 5- HONS 046276 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 145 Test Methods 11,608-54 Test for Dielectric Constant and Power Factor of Aroclors, Pyranols, InSrteens. and Trl-Tetraohlorobenaene Blends, Method No. 11,608-54, contd. S. Turn "VERTICAL INPUT'I to "10 VOLT MAX.". h. Turn "HORIZONTAL OAllj" to about 20. 1. Turn "SYNCHRONIZINO" ;tc + 20. Turn "SYN. to "EXT. sjyN." J. k. Turn "OEN." to "SWEElj OEN." C, On Panel No. ? (Capacitance Bridge) a. Turn "RANGE SEIECTOR'j switch to "100c" for 60 cycle measurements and to 1; KC" for 1000 cycle measurements. b. Turn "METHOD SWITCH" jto direct. c. Turn "DISSIPATION FACTOR" selector switch to "0". .t D, On Panel No, 4 (Osclllatejr) a. Disregard this panel |for measurements at 60 cycles. b. On 1000 cycle measurebient.e, depress the No. 10 "MULTIPLY BY" button. C. Set "FREQUENCY DIAL" to 100. d. Turn "OUTPUT" dial soi that pointer Is at the end of the arrow. e. Depress the "UNBAL. 5(X)0 OHMS" button. When all cf the above ad.Juets.eKts are made, the electrical apparatus Is ready for measurement of Dielectric Constant and Power Factor. MANS 046277 IX. SPECIFICATIONS AMD TEST METHODS, cond. IX - 146 Test Methods 11,608-54 Test for Dielectric Constant and Power Paotor cf Aroolore, Pyranola, Inerteens.and Trl-Tet,rachlorobc|zene Blends, Method No. 11,608-54, oontd. II. Determination of Constantsjfor the Apparatus. 1. Carefully assemble the cell which has been cleaned and dried within the last 8 hours.1 Refer to Method No. 11,751 for the procedure to use In cleaning the cells. 2. Place the cell assembly ).n the Fisher oven which has been ad justed to 25C. 5. Connect the back: wl re inhide the oven to the lead on the Inner cylinder of the cell and the front wire to the lead on the outer cylinder of thp cell. 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 f.ron|t terminal. 5. the oven before going 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. 3 until the wide vertical band on the oscllllBcopej 1b adjusted to a minimum width. 8. Record the sum of the readings on the "CAPACITANCE" dial and vernier and call this vs|lue A. 9. Remove the teakar containing the cell from the oven and fill It with C. P. benzene to; a level 0.737 Inches (ca. 3/4 inch) above the top of the conjoentrlo cylinders of the oell. 10. Adjust the temperature cjf the benzene to 25*C. while stirring with a thermometer. HONS 0462 76 IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 147 Test Methods 11,608-54 Test for Dielectric Constant and Power Faotor of Aroclors, Pyranols, Inerteens, and Trl-Tetrachlorobei zene Blends, Method No. 11,608-54. contd 11. Replace the cell in the ovpn (at 25*0.) and make the same electrical connections as in Steps 3 and 4. DO NOT Interchange connections. 12. Balance the bridge again aj In Step 7. 13. Record the sum of the readings on the "CAPACITANCE" dial and vernier and call this yalue B. 14. Calculate the cell constant by the following equation: Cell Constant, K B A, (this is usually around 2.$7 - 1.0 70 uuf). ,i 15. Remove the cell from the o|en 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 7. (capacitance of connecting cable). 17. Calculate the Cell Lead Capacitance by the following equation: CELL LEAD CAPACITANCE, 0 - A - F - K (this Is usually around 3 uuf.) WHERE: A - CAPACITANCE OF ENTIRE {SYSTEM IN AIR (SYSTEM CONSTANT) Q * CAPACITANCE OF THE CElj, LEADS (CELL LEAD CONSTANT) F - CAPACITANCE OF CABLE ARD WIRES WHICH CONNECT THE CELL AND CELL LEADS TO THE {iRlDQE. (CONNECTOR CONSTANT). K - CAPACITANCE OF THE CEL^, ALONE (THE CELL CONSTANT). MONS 046279 IX. SPECIPICATIOMS AND TEST METHODS, oontd. IX - 148 Test Methods 11,608-54 Test for Dielectric Constant andj Power Factor of Aroclors, Pyryiols. inerteens, and Trl-Tetrachlorobenzene Blends, Method Ho, 11,608-54, oontd. Tabulate the System Constant (A)|, the Cell Lead Constant (a), the Conneotor Constant (P), and the bell Constant (K) on a piece of stiff paper and post them near the Instrument where they oan be easily referred to for comparison and cjalculations. These oonstants must be checked at least once every three months and in all oaseB where the Dielectrijc Constant and/or Power Factor are out of specification. III. Measurement of Dlelectrl onstant and Power Factor on Aroclors. Pyranola, Inerteens, and 1-Tetraohlorobensene Blends. A. Test Run on Cell to Properly Aligned. ermine Whether it is Clean and 1. Carefully assembly a cell which has been cleaned and dried within the past 8 hoirs. NOTE: Refer to Method No. 11,751 for procedure to use in cleaning cells. 2. Adjust the oven control to hold at a temperature ef 100*C. for all materials except Tri-Tetra Blends. If a Trl-Tqtra blend as to be tested, adjust the oven to hold a temperatur^ of 25 "C. 5. Place the empty cejll assembly in the oven and connect the hack wire inside tpe oven to the lead on the lnner cyllnder of the cejll, and connect the other (front) wire to the lead c(n 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 (groujnd) goes to the front terminal. 5. Allow 15 minutes for the cell to reach temperature equilibrium lnsidej the oven. HONS 046280 IX. SPECIFICATIONS AMD TEST KgjjHODS, eort-d. IX - 149 Test Methods 11,608-54 Test for Dielectric Constant and Power Factor of Aroclors, Pyranols Inertsens, and Trl-Tetranhlovobe^sene Blends, Method No. 11,608-54.oontd. 6. Remove the thermonjeter from the t.op of the oven before taking any measurements on the bridge. This Is Important. 7. Make all the adjustments on the electrical apparatus aB direc.te;'. in Parjt 1 of this method. 8. Balance the bridge, by rotating the "CAPACITANCE" and "DISSIPATION FACTOR" dials or. Panel No. 3 until the wide vertical band on tpe oscilloscope screen is adjusted to a minimum, width. 9. Record the sum of the readings or. the "CAPACITANCE" dial and vernier add compare this value with the SYSTEM CONSTANT determined In Part II of this method. IMPORTANT: If the! value obtained m Step 9 does not agree with the System Constant- A (Part 11) within 5 uuf, the cell roust, he re-cleaned, re-dried, re-assembled, and the test run 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 calcLlat-lons but Is to be used only as a check ovrthe cleankinasE and alignment of the cell. B. Procedure far Teat-Ins Materials. 10. Remove the cell frh the oven end fill the beaker with the material, to be> tested to a level 0.737 inches (ca 3/1* ir.'.ih) ahe-v^ the cylinders of t.he cell. 4.1. AdJus t the tMr.peivfeure of the sample to 100*0. (use hot piste) for all materials except. Tri-Tetra blends. For Trl- Ter.ra blends, adjust the temperature of the sample to P5*C. us|tng an ice-water bath If necessary. NOTE: Sl-'.r sample:: continuously with a thermometer while adjust-.lRg the ..eapjsra bure. MONS 046281 IX. SPECIFICATIONS AKD TEST METHODS, contd . IX - 150 Test Methods II,608-54 Test for Dielectric Constant and;Tower Factor cf Aroclora, Pyranols Inertsens, and Tri-Tctraohlorobehzenc Blends, Method No, ll,6o6-54,contd. 12. Place the ceil and! sample In the. oven and make the same connections from the cell to the bridge as in Steps 3 and 4, DO NOT interchange connections. 13. Allow fifteen minutes for the cell to reach temperature equilibrium inside) the even. i 14. Remove thermometer! from the oven before taking a measure ment." This 18 in'pjortar.t. 15. Make the adjustment- of controls on the electrical appa ratus as directed [in Part I of this method. 16. Balance the bridge, by rotating the "CAPACITANCE" and "DISSIPATION FACTOR" dials nr. Panel No. 3 until the wide vertical bard on the oscilloscope screen is adjusted to a mini mum width. 17. Record the sum of Ithe readings cn the "CAPACITANCE" dial and vernier, end call this value X. 18. Record the arm of jth* readings or. the "DISSIPATION FACTOR" dial and switch. iCall this value D. Calculationr.: Dielectric Cor.stsf.t it - F - G i "k--------- Where.: X Cat del banco readir^ from Step 17. P * Cer.i.eotor Constant (Determined in Part 11) if - (Jell lead Constant (Determined In Part II) K > Cel| Constant. (Determined in Part II) HONS 046282  IX. araOIFICATIOHa AND TB3T MBTgODa, contd. ix - 151 Test Methods 11,608-54 Test for Dlelsotrlc Constant andjPower Factor of Aroelors, Pyranols Inertsens, end Trl-tetraohlorobeazene Blends, Method Wo. Il,6o8-54.oontd. % Power Vector ff l0 _ XD Where: f - Test Prequenoy (60 cycles or 1000 cyeles) f - frequency of "Range Selector" on Panel Mo.3 D1 Dissipation Factor reading from Step 18. i 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; (Referencej General Radio Manual for Model 716-C Oapaoltance Bridge). a. Capacitance readings are precise to + 2 uuf x multiplier reading (+ 0.2% of full soale for each range) when the dissipation factor la less than 0.01. b. Dissipation Faotoif (Power Factor) readings are precise * to + 0.0005 or + of the dial reading whichever is larger, for valuer less than 0.1 for D (Dissipation Factor). XV. Apparatus A. Osolllosoope: Heathkltj Model 0-6. S, Constant temperature Heating Unit: Fisher Isotemp oven. Model 13-245A, modifier to Include inter-wall connectors. 0. A. C. Generator: General Radio type 1302-A. MQNS 046283 IX. SPECIFICATIONS AND TEST 10D3, oontd. IX - 152 Test Methods 11,608-54 Test for Dielectric Constant and Power Factor of Aroclors Pyranols, Inerteens. and Trl -tetrachlorobenzene Blends, Method No. 11,6o6-54, oontd.[ IV. Apparatus, oontd. ; D. Amplifier and Null Detector: General Radio type 123I-B with type 1261-A powpr supply. E, Capacitance Bridge: General Radio Company Capacitance Bridge type 716-0. P. Test Cells: Q. E. type, concentric cylinder electrodes Catalog # 1,559,663.! 0. Class B driver transformer: This Is UBed for 60 cycle measurements to excite t.he bridge directly from the domestic power line.! It has 50 volts outphfc 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. /--!----------/ HONS 046284 IX. SPECIFICATIONS AND TEST IODS, contd. IX - 153 Test Methods 11.732-5* Date: 4/22/5* Material: Qeheral Method Method No. 11,732-5* By: DKL, NPA:WJO Test: Color j(N. P. A. soale) WOK O.M. No. 11 1. Fill a 1-5/16" X 5" N. P. |A. glass test Jar (N. P. A. tube) half full of the liquid (ojr molten) sample. 2. Plaoe 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). *. Turn the knob that brings jthe various colored glass standards Into view. 5. Match the sample as nearljt as possible with the color standards. ' The method is precise to ^ 1/* N. P. A. units. Report the ooloP to the Rarest 1/* N. P. A. unit. Reference; ASTM Union Colorimeter and the N. P. A. Color Standards are given In ASTM Designation: D-155-*5T (see 1952 Book of ASTM Standards, part 5, pages86 to 90 Inclusive). MONS 046285 IX. SPECIFICATIONS AND TEST HODS, contd. XX - 154 Test Methods U, 751-53 Data: 2/26/53 Material: Aroblors, Pyranols, Method No. 11,751-53 Inerteens, and Trl-Tetrachloro- benpene Blends WOK Dept.No. 233/246 By: CM, HOH, Test: Procedure for Cleaning of LJW.WJO, NPA: Electrodes, 0. E. Cell, and Accessories SMK______________________________ |___________________________________________ A, The Electrodes Cleaning Procedure: 1. Remove the electrodes from the tested material while hot and allow them to drain. 1 .I 2 Place the electrodes In h{ot TCB for 10 minutes. 3. Wash with unheated TCB. i 4. Rinse twice with methanolj and twice with tap water. i 5. Place the electrodes in hbt lOjt T. S. P. solution. Soak and heat for 10 minutes. ' .6 Wash thoroughly with tap ^ater. CAUTION: After Step 6 ~ j)0 NOT TOUCH THE ELECTRODES WITH HANDS! 7. Wash with distilled water! twice. .8 Dry In drying oven for atj least two hours at 120 *C. B. The 0. E. Cell Cleaning: ! 1. Reolean the Cell before ube, If more than 8 hours have elapsed since the previous cleaning. 2. Follow the procedure for jbhe electrodes starting at Step 4. C. Cleaning of the Aacessorle^: MQNS 046286 1. Apply the same cleaning procedure as given for the electrodes (Steps 1 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. ; 3. Place the wet thermometerj (after Step 7) directly In position In the Temperature Heating Upit (Modified Fisher iBotemp Oven) and allow to d'-y. , f IX. SPECIFICATIONS AND TEST oontd. IX - 155 Test Methods 11,752-53 Date: 2/26/53 By: CM, LJW Material: Arodlors, Pyranols, Inerteens, ana Tri-Tetrachlorobenzene Blends Test: Electrical Measurements Method No. 11,752-53 WOK Dept. No. 233/246 Introduction: Some of the Aroclors, Pyranol* , Inerteena, and Tri-Tetraohlorobenzene Blends have important lndustrlal uses based on their eleotrlcal properties. There;fore, tests for certain electrical properties are made on these products. Oeneral Information; The testa should be run in th* following order: Test 1. Dielectric Constantj Method No. 11,608 2. Power Factor (if needed) 3. Resistivity 4. Dielectric Strength] 11,608 11,607 11,605 The terms, which are used in bonneotion with the above listed electrical measurements, are defined as follows: 1. Dielectric: A dielectric is an insulating or non-conduotlng material. 2. Dielectric Constant: i The dielectric constant jls the ratio of the equivalent parallel capacitance of ja capacitor in which the material MQNS 0402b7 7 ; ; IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 156 Test Method 11,752-53 Kleotrlcal Measurements for Aboolora, Pyranols, Inerteens, and Trl-Tetraehlorobenzene BlendaL Method Mo. 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 vaouum as the dieleotrlc, and Is represented by the symbol X. The K of air may be considered eqiial to that of a vacuum. 3. Capaoltor; A oapacltor consists of bn electrical oonductor upon which an electric oharge can be stored. In practice, a condenser consists of two or more petalllc plates separated by a dielectric. 4. Resistivity: In the metric system, this volume resistivity of a material Is the resistance between two electrodes which cover opposite faces of a centimeter eupe. It Is expressed in ohms/om*. 5. Dieleotrlc Strength: ; Dielectric Strength is the rupturing strength of an insulating material when subjected [to voltage stress, under specific conditions and expressed In volte/mllllampere. Breakdown varies with the shape of, the electrodes and does not Increase In proportion to the thljokness of the dielectric. 6. Power Factor: The power factor of a dielectric Is the ratio of the energy less in the dieleotrlc tjo the "apparent power" In the di electric. | HONS 04628B i IX - 157 Test Methods ' 11,784-53 IX. SPECIFICATIONS AMD TEST METHODS, eontd. Date: 10/7/53 By: WRB.DKL DTM:SMK Material: General Method Method No. 11,784-53 Test: Refractive Index WGK 0. M. No. 281 1. Study the attached diagram to familiarize yourself with the principal parts of the Refrkctometer which will be referred to throughout the method. ! CAUTION; The glass from which the prisms in this instrument are constructed ib necessarily somewhat unstable and Is very easily scratched or corroded. It ks, therefore, necessary to exercise extreme caution In using th|em by following these 3 rules: a. Do not wipe the glass wilth any rough material or with anything in which there may be specs or grit. b. Never touch the surface^ of the Abbe Prisms. c. Clean the prisms only by flushing them with alcohol. Xylol, TCB or water. 2. Make sure that the surface^ of the prisms, between which the fluid Is to be placed, are perfectly clean. This can be aooompllshed by flushing them with alcohol and allowing to dryin air. 3. 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 25*C.|or other specified temperature as registered on the thermometer. This is done as follows: If the temperature Is above 2(*C., 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 25"C., flip the toggle switch ir. the upper right comer to the "Medium" position. This should bring the temperature to 25*C. 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. 5. Place several drops of purfe distilled water on the auxiliary (lower) prism and lmmedlat|Bly bring the prisms together and clamp them m position. MONS 046289 IX. SPECIFICATIONS AND TEST [OPS, contd. IX - 158 Test Methods 11,784-53 General Method, Teat 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 bhe refractometer and adjust the mirror until light Is reflected Into the lower prism. 7. Release the "Hand Positioning Control Clan" 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 tills position by means of the hand positioning control clamp.! 9. Move the mirror slightly. Ilf the dividing line moves It Is spurious. The mirror should be moved to clear the spurious dividing line from the flefd and the true dividing line sought again. 10. The border between the light and dark portions of the field will usually be ooloured. 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 orosses the Intersection of the cross-wires. 12. The refractive Index Is thin read by observing the scale of the "Alidade Arm" through the rSeale Magnifier", the fourth decimal place being estimated. HONS 046290 13. If the reading of the distilled water at 25 *C. varies from 1.3325 (the true index of distilled water at 25<IC.)record the correction and apply this same correction to the sample reading when It is ; observed. NOTE: Corrections at othei temperatures than 25C. may be made with suitable conversion -{ see your supervisor. 14. Repeat Steps 2 to 12 Inclusive substituting the sample In place of the distilled water In ^tep 5. 15. Apply the correction from itep 13 and record the reading. 16. Repeat Steps 2 to 15 excluding Step 14 twloe more, using fresh samp.ie each time. The readings should agree within 0.0001 units. Rep'rt Refractive Index atj25"C. to the nearest 0.0001 unit. 'I IX. SPECIFICATIONS AND TESTjMETHODS, contd. IX - 158 a Test Methods 11,784-53 ABBE TYPE REFRACTOMETER Soale Magnifier Line Reticule Alidade Scale Movable Leve Arm Hand Positioning Control Clamp Tangent Screw Line Adjustment Auxiliary (Lower)) Prism _) Mirror Eyepiece Telescope ____ Compensator iControl Knob Heating Chamber Clamp Thermometer Detachable Hinge A-7751 HONS 046191 IX . SPECIFICATIONS AND TEST METHODS, c o n td . [A-7752] tCMIMr 7IHUIim HUM ? 6 ? 9 V 0 SNOW I IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 159 Test Methods 11,788-53 Datei 7/30/53 Material: Oenerpil Method Method No. 11,788-53 By:DKL,WJO:SMK Test: Turbidity; ----------------------------------------------------------------1---------------------- WOK O.M. No. 15 The turbidity of WOK 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. Compare the sample lnmedlate|L;y to the appropriate turbidity standards In sample bottles 3f the same size and similarly shaken. Report' the turbldlt|f to the nearest standard number, e. g. Turbidity, Standard (Jo. 5. NOTE: A helpful procedure Is to borapare the eaBe 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 4i 51 62 75 84 9 -- 10 5 Preparation of Standards: APHA Turbidity ppm Suspended Matter 2 4 8 16 30W .60 125 250 500 1000 Turbidity stock solution, 1000 ppid Puller's Earth In accordance with AFHA 6th Edition, obtained from th}s Hartman-Leddon Co. (Harleco) Philadelphia, Pa. MQNS 046293  IX. SPECIFICATIONS AND TEST METHODS, oontd. IX - 160 Teat Methods 11,788-53 Teat for Turbidity, general Method, Method No, 11,788-53, oontd. The stock solution Is Standard Wo. 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' 30 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 3 8o 2 4o 1 20 Add 50 ml. of a 5% mercuric chloride solution containing l 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. MOWS 096294 1 IX. SPECIFICATIONS AND TKST METHODS, oontd. IX - 161 Test Methods 11,861-54 Date! 5/6/54 Material: Phenoiypropene Oxide Method No. 11,861-54 (Olycidyl Phenyl Ether) By:WOM,NPA:WJ0 Test: Crystallising Point WOK Dept. No. 246* 1 CAUTION: Phenoxypropene Oxide |Olycidyl Phenyl Ether) Is a toxic Irritant. Handle with oare and'avoid contact with the skin. Wear your Safety Glasses. 1. Prepare a dry lee-acetone bath In a 4oo-ml. beaker. 2. Prepare an ice-water bath J.n a second 400-ml. beaker. 3. Fill a 1" x 4" test tube 3/4 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 loe-aoetone bath. Stir constantly with the thermometer. 5. Upon cooling of the sample to -2* to 5C. remove it from the bath and Bead with previously prepared orystals 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 -15*C. IMPORTANT: DO NOT COOL BE^OW -15*C. 7. Immediately plaoe the sample In the loe-water bath and continue stirring until the temperature reaches a maximum point. Record this temperature. 8. This maximum temperature lp the crystallizing point. The method Is precise to + 0.1*p. Report the result to the nearest 0.1'C. HONS 046295 l IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 162 Test Methods 11,862-54 Date: 5/3/54 Material: Phendxypropene Oxide Method No. 11,862-54 (PPO) By:NN,NPA:WJO Test: Distilling Range WOK Dept. No. 2461 CAUTION: Olyoldyl Phenyl Ether (Phenoxypropene Oxide: P.P.O.) Is a toxlo 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. }.0,006) with the following modifi cations : 2. Insert a 250 to 260C. raAge, 5" Immersion thermometer. 5. Use a transits board with a 2-lnch opening. 4. Distill at the rate of 2 i^ropa per second. 5. Apply the thermometer and[barometric correction. Report the following temperatures: First drojk 95)* (1-96 ml.) range 100)* (Fir^t Drop to Dry Point) range Dry point Report the results to the nearest 0.1'C. MQNS 046296 l XX - 163 Test Methods 11,863-54 IX. SPECIFICATIONS AMD TEST MBTjlODS, oontd. Date: 5/3/54 Material: Phenojcypropene Oxide Method No.11,863-54 By: NN,NPA:WJQ Test: REFRACTIVE INDEX AT 25 *p.1 WOK Dept. No. 246 CAUTION: Qlycidyl Phenyl Ether (Phenoxyprppene Oxide: P. P. 0. ) Is a toxic irritant. Handle with care and Avoid contact with the skin. Wear Your Safety glasses. 1. Determine the refractive Index of PPO at 25*C. according to General Method No. 28 (Methpd No. 11,734) with the following modifications. 2. Clean the Abbe prisms by flashing with Trlchlorobenzene. Then follow with benzene and "Mersol" washes. IMPORTANT: Do Not Touoh the Polished Surfaces of the Abbe Prisms! Report the Refractive Index (N^2^) to the nearest 0.0001 unit. /' -/ M0NS 046297 ' IX. SPECIFICATIONS AMD TEST METHODS, contd. Datei 7/23/54 By: NN, NFA, OWMiWJO Material: Phenfoxypropene Oxide (PPO) Teat: Specific Oravlty IX - 164 Teat Methods 11,864-54 Method No.11,864-54 WOK Dept. No.2461 CAUTION: Olyoldyl Phenyl Ether (Phenoxypropene Oxide: PPO) la a toxic Irritant. Handle with care and avoid contact with the akin. Wear Your Safety Pleases. 1. Determine the Specific Oravlty 25/15-5*0. according to Oeneral 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 50*C. range thermometer. 4. Adjust the temperature of #P0 between 20 - 30*C. 5. Apply (if any) the hydrometer correction. 6. Use Specific Oravlty Coefficient 0.0008 unlt/*C. Calculation: A. For Specific Oravlty t 15.5*C^L5.5*C. Temperature Correction - (Temp.of Sample - 15.5*0.) x 0.0008 Add this correction t the reading obtained If the tempera ture of the sample wap above 15.5*C. subtract if below 15.5*C. B. For Specific Gravity pt 25*C./15.5*C. Temperature Correction - (Temp.of Sample - 25*C.) x 0.0008 Add this correction tp the reading obtained If the tempera ture of the sample wap above 25*C. subtract If below 25*C. The method is precise to + 0.001 unit. Report the Specific Oravlty 15.$*C./15.5*C. and 25*C./15.5*C. to the nearest 0.001 unit. HONS 046298 l I IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 165 Test Methods 11,865-52 Data! 7/8/52 Material: Transformer Inerteen (PPQ) By: NN, TT:SMK Test: (Phenoxypropene Oxide) ---------------------------------------------------------------------------------> -- NOTE; Run this analysis In duplicate Method No. 11,865-52 WOK Dept. No. 246 Preparation of Reagents: Indicator - Mix 1 part of a 0.1$ water solution of cresol red with 5 parts of a O.ljf water solution of thymol blue. Pyrldlnlum Chloride Reagent; - Completely mix 16 ml. of cone. HC1 with 1 lltejr of Baker's C. P. pyridine. 1. Weigh (+ 0.05 g.) a 100 +15 g. sample Into a 500 ml. Erlen- meyer flask. 2. Add by pipette 20 ml. of the pyrldlnlum chloride reagent. ?. Attaoh to a reflux condenser and reflux for thirty minutes. NOTE: Measure reflux tlme|from the start of boiling. 4. Turn offthe heat at the en4 of the reflux period, and add 50 ml. of distilled water at t|he top of the condenser. 5. Detaoh the flask from the dondenser and wash the end of the condenser with a few ml. of distilled water. 6. Cool the flask and content^ to room temperature In Ice water or under the tap. 7. Add 1 m}. of the cresol reij-thymol blue Indicator. 8. Swirl .the flask rapidly so 4hat there Is a thorough and violent mixing of the contents whl).e titrating with 0.1 N NaOH to a dlstinot blue colour. MOWS 046299 l IX. SPECIFICATIONS AMD TEST METHODS, contd. IX - 166 Test Methods 11,865-58 Test for (Phenoxypropene Oxide)lh Transformer Inerteen (PPO), Method No. 11,865-52, oontd. HOTBi 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. Erlenmeyw flask, weigh, on a beam balance, a 100 + 5 e- 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 fl Phenoxypropene Oxide (PPO) - (A - B)(Normality NaQH)(15.0) Oram Sample Report to the nearest 0.00l. Referencei Westlnghouse Research Report No. 60-94602-9-48. MONS 046300 f '' IX. SPECIFICATIONS AMD TH3T MgTftODS. oontd. IX - 167 Test Methods 12,03-3-53 Date 1 5/12/53 BysNPAtSMK Material! Trl and Tetrachloro - Method No.12,033-53 benzene Blend ' Test: Last; Crystal Point WOK Dept. No.. 2461 1. Pill Pour-Point test Jar wl{th sample to a depth of two Inches. 2. Insert the thermometer-stlrper assembly so that the mercury bulb of the thermometer is hear the center of the sample. . 3. Cool, while stirring, until sample is at about -15*C. 4. Seed with a few crystals of 1,2,4,5 Tetrachlorobenzene and con tinue stirring and ooollng until the sample crystallizes forming a Blurry. 5. Continue stirring at the rate of one to three strokes per second, while exposing Jar and contents to room temperature. NOTBi As the last crystal point approaches, the mercury meniscus of the thermometer under thp liquid Is Invisible, but it Is within a range of 0.2 - 0.3*C. 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 1 The visibility does hot appreciably change during the next 0.5*C. rise in temperature. Report the result to the nearest 0.1*C. Apparatus: A Pour-Point, test Jar (see Sectlbn 3 a, ASTM D97). A -15 to 20*C. range thermometer accurately calibrated and having 0.1*C. subdivisions. A loop stirrer of a heavy gauge Wire. A rubber stopper with holes to accomodate thermometer and stirrer. MQNS 046301 IX. SPECIFICATIONS AND TEST METHODS, contd. Date: 2/6/53 By:NPA:SMK Material: Trl-Te trachlorobenzene Blend Teat: Distilling Range1 IX - 168 Test Methods 12.034-53 Method No. 12,034-53 WOK Dept. No. 233/246 1. Determine the distilling range of the sample aooordlng to Oeneral Method No. 1 (Method No. 10,006) with the following modifications: 2. Use a translte board with a 2" opening. 3. Use a 0 - 360*C. range 3-indh Immersion thermometer (corrected at 200* and 250*C.) with 1*0. 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 900 by volume 95% by volume Dry point. NOTE: The distillate Is collected "by vplume" and not "by weight" as In the case of Pyranol distillations. MONS 046302 * IX. SPECIFICATIONS AND TEST METHODS, contd. IX - 169 Teat Methods 12,036-53 Date; 2/10/53 Byi TT,NPAsSMK Materials Trl-ietrachlorobenzine Blend Method Mo. 12,036-53 WOK Dept. No. 233/246 Teat: Composition by Distillation1 Use a beam balance for all weights. 1. Weigh a "heel" of 200 ( + 0.<)5) g. of Aroclor 1248 Into a 2-llter 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 Trl-Tetra-blend to be tested 3. Connect the still-pot to th+ 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.): Colleot distillate ` from 204* to 220*C. (the distilling head temperature). Into a 500-ml. Erlenmeyer flask (tared). b. Fraction 2 (1st Intermediate Fract. - Trl-Tetrachlorobenzene): When the distilling head temperature reaches 220*C. 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 245*c. NOTE: To prevent possible "Freezing" during this stage of the distillation, turn an electrical current In the circuit to the distilling head when the head temperature reaches ca. 230*C. o. Fraction 3 (Tetrachlorobenzene Fract.): Collect the distil late at the head temperature 245-255*C. Into a dry, tared 500 ml. Erlenmeyer flash. MONS 046303 l  IX. SPECIFICATIONS AMD TEST METHODS, oontd. IX - 170 Test Methods 12,036-53 Test for Composition by Distillation of Trl-Tetrachlorobenzene Blend. Method No. 12,036-53, contd~l ' NOTEi An additional heat on the distilling head may be required during part of this fraction. d. Fraction 4 (2nd Intermediate Fraot.) - Tetra-Pentachlorobenzene Fract.): Collect all distillate from 255-275*0. in a dry, tared 250-mlt Erlenmeyer flask. NOTHi If the Pentachlorobenzene:content is not required, the dis tillation may be terminated at tfcis point. If the "Penta" is desired then proceed as follows: e. Fraction 5 (PentaohlorSbenzene Fract.): When the head temperature reaches 27**C., replace the fourth fraction reoeiver with a dry, tyred 250-ml. Erleneyer flask and collect all distillate until the head temperature Is 277*C. 6. Stop the distillation. Tumi 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 20-55*C. range, 3" immersion thermometer. Record the highest temperature reached after crystallization has taken place. Determine from Dwg. No. A-5p38 on page IX - 17? below the 1,2,3,A-' . 'aHd'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 dpwn, determine weight of the residue as follows: wt. of Residue (gms) > [wt. of Pot - (wt. of "Heel" + still-pot Step 1)J HONS 046304 1 XII. BCPIPMBNT LIST, oontd Closed Tanka, oontd. XII - 53 Equipment List CT-0968 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/J7. Heq. 81458 on 8/2/37 Price $575.00. CT-01013 #1A scrubber liquor pump tank made by Leader. Dwg. C-4616. 81ze 4>6" IP x 5'6" vertical, steel, flange quality, all welded Jacketed. Order B 4164 on 4/29,1/38, Req. 87029 on 3/9/38. Prloe *582.00 On 38 level SB comer CR. ' CT-01014 Scrubber tank made Heintz. Dwg. C-4845. Steel 12" dla. std. brought steel pipe 10'10" high, i" dished end and oth<er end fitted with 3/4" faced and drilled fig. wit 1 5/8" cover plate. Steel plate, and distributor. Us 1 5 ou. ft. 1" Cl Rasohlg rings pkg., Order B3933 on 3/4/3 I Req. 86921 on 3/4/38. Price *139.00. On top of 6r-01013, #1A sorubber. CT-01162 Scrubber tank made bT Heintz. Dwg. C5743. Welded steel scrubbed size 12" ID x 5'. Order B19519 on 9/27,p9, Req. 1977 on 9/19 Prloe *102.00. Vent line to CT-0848. CT-01163 Catch Tank 55 gal. speel drum. Por CT-0762. Mate to CT-01164. *11.40. 11/27/39. Chg. out (*) (*) Both CT-OII62 and CT-01163 are on vents of CT-01321 and 02621, Pyri anil Plant. CT-01164 Catoh Tank. Same as CT-01163. Por CT-01162, PyranoL Plant. HONS 046403 XII. EQUIPMENT LIST, contd. Closed Tanks, oontd. XII - 34 Equipment List CT-01258 01279 CT-01258 Monel gas chamber made by Nooter. Dwg. C-5825. 4' dla. x 4' high constructed of Monel. Order B7835 on 4/3/40, Req. 8061 on 3/27/ 40, Req. 8061 on 3/27/40. .Chg. out 4867.00. on gas exit from fire heated chlorlnator. This monel vessel is at the lowest point of the gas exit line from the gas-heated ohlorlnator. Solid Aroclor which collects In It Is removed by hand and returned to the ohlorlnator with a subsequent batch. CT-01259 Cyclone Tank made by Helnts. Dwg. B5821. 2'6" dla. x 6'7" high constructed of 3/16" steel plate, order B7345 on 4/27/40. Req. 8062 on 3/27/40. Price 492.00. Hang from ioof of Bldg, on 38' level. CT-01259,01279, 01280, 01281, 01282, cyclones on ohlorln ator off-gas, follow the scrubbing towers CT-0759 eto. Drain through S. O'a 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). See drawing |b-660. CT-01263 Monel condenser madq by Nooter. Dwg. C-6144. 42" dla. x 63" high cone bottom condenser constructed of 3/16 Monel metal jwelded construction throughout. Order B-8364 on 4/9l,/40. Req. 8198 on 4/1/40. Price 4928.00 This vessel is obsolete. CT-01279 Cyclone separator mi le by Nooter Dwg. 5821. 2' dla. x 6'7" high cyclone s< parator made of steel and welded throughout. Order 1 13177 on 6/12/40. Req. 10232 on 6/5/4C . Chg. out 486.25. For use at CT-0968. MONS 046404 XII. EQUIPMENT LIST, contd Closed Tanka, oontd. XII - 35 Equipment List CT-01280 - 01321 CT-01280 Cyclone separator mi ide by Nooter. Dwg. B-5821. 2' dla. x 6'7" high oyclone separator made of steel and welded throughoit. Order B13177 on 6/12/4o. Req. 10232 on 6/5/40. pf:loe $66.25/ At CT-O762 east scrubber. CT-01281 Cyclone separator. Same as CT-01279 and 1282. At CT-0759. 2nd from I scrubber. OT-01282 Cyclone separator. Same as CT-01279 - 1280 - 1281. Used at CT-0760. 3:M from E scrubber. CT-01283 Chlorlnator made by Leader Iron Works, Inc. Dwg. B6209, 3' x 161 steel vert:4al chlor. welded const. Order B-14119 on 6/21/40, Req. 10408 on 6/11/40. Price $720.00 Bast of CT-0833. #4 chlorlnator. S*e CT-0744. CT-01310 #5 Aroclor 1260 St$irage Tank made by Leader Iron Works. Dwg. C-609. Horlsoi4tal 10' OD x 26' long on str. shell. lnold. colls, etc Omitted 2 - 3" nozzles changed 18" nos. to 24" and add$id covers for 24" noz. Tanks, colls, ooll supports, lnslq,1e of noz. and manholes and manholes and nos. and Inside covers must be sprayed with jinc ' 0.005" thick follow^Id by a sprayed coat of 0.003" tin. Order B13240 on 6/1i/40, Req. 10432 on 6/11/40 Price $2200.00. umqerground s of CT-0848. Pump P-0929. CT-01321 Pyranol Mixing Tank made by Nooter. Drawing D6455. 14' OD x 10' hi,gh steel tank with 3/8" shell, 1/2" std. knuckle reidlus heads, entire Interior sprayed with min. t:hickness of .015" tin. ' 42" Quadruplex turbo mixer complete Including Turbo adaptor assemilply -- off set from centre. (1) Order B20976 on 9/27/40. Chg. out $2930.00 (2) Order B21762 on 10/8/41, Req. 13664, Cost $740.00 MONS 046405 XII. EQUIPMENT LIST, oontd. Closed Tanks, contd. XII - 36 Equipment Llet CT-01321 01397 CT-01321 contd. Driven by MSC-01286J Motor M01718. 1$" steam coll, 45 (umi, 18" diameter,through the cover. 9600 imp. gallons, Outdoors. Bverdur or galvanized piping. Bronze valjries. Bottom outlet to Tatr pump P-01540 delivering to filter press F-0159. Cappj}d Inlet on cover for Attapulgus Earth. Manlld. Steam coll Dial thermo. Vent to soda-lime vent box. Beat insi'lilatlon (gone). CT-01377 CT-OI378 Still reoelver tank made by Nooter. Dwg. C-795, B-7082, like CT-0771. PA #| 45. 5'6" x 5'6" Monel metal treoelver, complete 1th cover, coll, eto. Insulation 2" and ij finished coat. Glass wool Order B4137 on 6/27/'41, Req. 18315 on 2/17/41. Prloe $3295.00. NE corner of 12' level platform In Bldg. CR. is used' Ion #2 still S-062. Condenser tank made| by Nooter. Dwg. B651. 12" ID x 5' long.I,Moh<tel metal. Order B4137 on 10/ Req. 18315 on 2/17/41. Price $650.00 W of bT-01413 on 20'6 level platform, Bldg. CR. Like CT'-D770. Used on #2 still. CT-01396 Vacuum scrubber p'urteihased from Combustion Engineering Co. Drawing C-807. 3 tlD x 10' high, steel construction including grating and screen. Order B8360 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 exohangi;4r made by Leader Iron Works, Dwg. B-483. 6" dial x 10' long, 12 tube. Order B8324 on 4/4/4:1, Req. 19993, Price $119.00 North of CT-0831. On #2 still. Spare. HONS 046400 XII. EQUIPMENT LIST, contd Closed Tanks, contd. XII - 37 Equipment List CT-01398 01491 CT-01398 CT-01399 Cooler tank made byj Leader. Dwg. B644. 2'6" ID x 3' high sjteel cooler tank complete with coll. Order B8324 on 4/Vr*1, Req. 19993. South one on 29' p Iktform Used on #2 still Vented. Price $152.00 E-6839 and #2 blending tank maUiie by Nooter. Dwg./D-10290, general arrangement. 7' II} x 7' high, complete with coll, agitator, and drive support, zinc and tin lined, seams to be chipped and _ground smooth. Order B8325 on 4/4/|4;1, Req. 19990 on 4/4/41 Chg. out $930.00. |Drlven by M-02170. Kiddle one of 3, north end of 12 level platform, Vertical bearing fidr agitator shaft, A-6853. Compare CT-0779. Newport experience phows the need for adequate heating and agitation In biltendlng higher Aroclors. ' CT-01400 #2 filtrate receive;r,made by Nooter. 7' ID x 7' high lnql coll and supporting legs, Inside of tank zlnq sprayed, all seams chipped and ground. 1" glass vjool Insulations 2$" fin. coat. Order B8323 on 4/4/4:1, Req. 19992, Price $925.00 Msstone of 3 north end of 12' level platform, CR. Dwg. C-6863. See 0T-O78O. CT-01413 Separator tank madej by Heintz Steel. Used on #2 still, Dwg. C6957. 3' ID x 6' high tangential separator with Integral vapor pip4 complete. Order B10722 on 5/%1/41, Req. 20429 on 5/1/41. Chg. out $382.50. North one on 29' level platform Bldg. CR. CT-01432 5th chlorinator. See CT-0744. Nooter. Drawing E6209. CT-01491 Heat exohanger tan$ made by Leader Iron. Dwg. B483, CABI #217. 6" dla x 10' long, all steel, 12 tubes Order B21479 on 9/i:9/41, Req. 24894 on 9/19/41. Chg. out $140.00. Used on #2 vaouum still system. MONS 046407 XXI. EQUIPMENT LIST, contd Closed Tanka, contd. XII - 3B Equipment List CT-02086 -02621 CT-02086 Air blowing tank. Like CT-0750. CT-02404 This store tank ha been set up outdoors to hold the tri-tetra-ohloro bk nzene mixture, which Is bought in rail oars and unlol led by pump P-Ollll. The tank is a vertical cylindrl cal vessel 13'0" ID, 20'0" high on straight side with dome top and bottom. Total capacity 20, 00 U.S. gallons. It has a bottom outlet, with a str|| ner box, to pump P-02077 delivering to either of the ranol blending tanks. The tank has a Varec depth lndl :ator with stainless steel exposed parts, a vent pipe a dip pipe for air blowing, an Internal steam ool and external heat Insulation. 1 NOTE: Mr. Barbre, 1947, said that a batch tank to hold filtered Pyfanols, 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 cyclindrloal steel tank 10'6" IP 23'0" high with flat top and bottom. Total capacity 14,600 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. 1 The tank has a 7i B .P. Llghtnln 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 coll with T.I.C.iltem 1-01094,set at 50*C. (tin-sprayed thermo well), and external heat insu lation. There Is also a dip pipe through which dry air from the Leotrodryer PC-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. [ HONS 046408 XI1 EQUIPMENT LIST, contd. X71 - 59 Equipment List Note: In MCC manuals the CT ant. OT Items of equipment are listed under "T", e. f;. Closed Tanks and Open Tanks. HONS 046409 xii. ; SQUIPMBNT LIST, eontd XII - 40 Equipment List D-012 Dryers D-012 Plaker, Devine, 48" dla. x >0" long, drum 5/8" thick, rolled steel, machl^ied and polished. Housing to be of #16 ga. monel. Order B 7378 on 4/1^/36, Req. 69124 on 4/14/36. Price $1668.00 quot 3/17/56. In lean-tc on floofr on found, of concrete. Driven by M-0827 - ! HP Wagner motor thru MSC-0639. Jones Speed Reducer The pan is heated by gas flames. Sketch showing drum side-knife, dip pan and essential dimensions on 48" dj am. x 30" long steel drum, monel hood flaker -- drg. B-675, chutes for finished product. Drg. D-518. See drawing B-374. General arrangement, and C-827, weighing truck. Dryer for Attapulgus Barth In 1946 a vertical iteel tank with Internal steam colls was Installed at the Krusanrlch plant. It was still the only equipment for drying earth at the Krummrlch plant In 1955, but reliance was placed mainly on supplies drawn from Anniston With the Krununrlch 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 3" 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. HONS 046410 XII. EQUIPMKNT LI3T, oontd. | XII -4l Equipment List Dryers Dryers, oontd. Dryer for Attaplugus th, oontd In 1947 at the Krunmrlph plant the Attapulgus earth was being dried In a vertical oylindrloal steel vessel, with oone bottom, and an Internal steam ooil. The earth was fed in through a hand hole in the oover and withdrawn as wanted through twin dajnpers in the bottom. See the sketch sent to MCL with the drawings oolleoted in 1947. The oover of this dryer had a vapour vent, but there was no positive movement of air through the vessel, and the eleotrloally heated shelf dryer used at Anniston (see page 5 of the report "Notes on the Anniston Aroolor plant" Haveroroft and Mather, September 1947), would appear more likely to give thorough drying. The steam heated dryer was still in use at the Krummrloh plant March 31, 1954. The referenoe of Sehwarting and others, November 12, 1953, page 10, to an eleotrloally heated dryer refers to a still earlier unit-which had been abandoned. HONS 046411 XII. BttPIPMENT LI8T, oontd. XII - 42 Equipment List P-0106 - 0172 Pllters P-0106 Steel filter purohasipd from Nooter. Dwg. C-3775, Size 12" die. x 3'1d-3/4" high. leg supports, glass wool packing. Order B35U on 2/19/36. Req. 67729 on 2/14/36. Price *56. pO quot. 2/5/36. Pormerly used on chl>t:rine gas, but used In 1946 to filter out iron eto. Impurities froei the HC1 gas coming from other department;s through a long steel line.. P-0113 Sperry 24" bronze flJL.ter press. Cover for electrlo oven heater for prei Drg. B-685. Replaced by Sparkler press P-Ol/p Steel support and for Sperry filter B-7121. 3/4" pipe coll for liter catch pan -- A-7136. P-0159 Oeneral Electric PI] ter Press. Serial #6166966. Type PP30. Aooessoi les Included. 3 HP motor ahd 4 compartment drying ven. Pom 0, Cap. 25/30 gal. per min. Size 12", 20 chambers. Heated and insulated steel oover*wlth pul lies, oable, oounter weight and strip heaters, Pyrar 1 plant. Order B18935 on 9/21/39, Req. 1991 on 2/20/39. Chg. out $984.00 on JL1/30/39. P-0178 Sparkler filter, rial 484. Model l8-dl2 all bronze construction with li proved Scavenger plate, plates to be arranged so entli set can be removed. Steam tracing inside the lagging, then a metal shield over all. Steel legs and flooi flanges for bolting to floor. Served by pump p-09t Order B10302 on 4/2/ Req. 20430 on 4/30/41. Price $830.00 per qi 3/19/41. On ground floor center of Bldg. CR. Installed for Aroclars, but later transferred to use on Pyranols. Chain hoisst, MSC-01495, provided for lifting out the nest of planes. * MSC-02108. MONS 046412 XII. EQUIPMENT LIST, eontd. XII -43 Equipment List P-0172 - 0239 Filters, eontd. P-0172> eontd. Samples of filter p4p] er for the Sparkler press P-0172, which was then being used on Aroclors, bought under the reference "#21-18 Pi Iter paper", $2,753 per 100 sheets, Sparkler Mfg. Co. Nandei leln, were sent to London, April 9, 1947, P-0238 P-0172 was moved to the Pyranol department and replaced by a 33" Sparkler, See Operating Instructions 8/10/54, and Mr. Harden's notias of August 1950. 8parkler Filter, 334i-12 cell type,304 Stainless ateel, with Jacket for 30 $slg. P-0239 33" Sparkler press for Aroclors Installed In place of P-0172, P-0172 b^lng used for Pyranols. Sweetland. Size 10 EH, 5^ leaves. 523 sq.ft. C.I. body, lined with th:iick nickel. Nlokel valves and outlet line, with piamp P-01757. Out of use In 1955. (Pyranol plant). MONS 046413 XII. EQUIPMENT LIST, contd. XII - 44 Equipment List FC-045 Furnaces 70-045 Qas heiter for No. 1 till. Steel ahell 3/16" x 3'9" dia. x 4'10$" long, l[lned with lnaulatlng fire brick, etc. 1 ooll 2" xHy pipe, V turns formed into a 2' dla coll with apare blooks and| legs. Drawing S-886. Req. 69859 on 5/14/56, 0i:rde r B9665 on 5/29/56. Used to heat material in S-045, pvWi]ped thru coil by P-0593. Vent stack drawing B 4689 (oould not be found In 1946.) Piping detallB, draw:'ling C-8l5, was sent to London April 24, 1947. At plant B In 1946, tfhere were two natural gas burners aimed tangentially liftito the bottom of each furnace, and there was some evldenice of damage due to overheating of the lowest pfcrt of ttyie coll. The central "dummy" Inside the coil was made as solid cylinder of firebrick and plastic refractory mS<Serial built up on a circular plate suspended on a centra:il steel lifting bar. Head room and a suspension hook aw| required over eaoh furnace, for maintenance work. The material from thS still Is pumped downwards through the ooll In the fumty,ee of the new still, but upwards In the old still. The lain reason for this Is that this arrangement enables ijlhe coll of the deep still to be on the same level as thty,t of the shallow one. At Anniston the material is pumped upwards beoause this puts the coldest Aroolor In at the bottom where the ooll Is most In dangqr of overheating. This can have little advantage, ex^i ept towards the end of the run, when the temperature sprei between the Inlet and the outlet Is greater. There Is a thermo-reqorder pocket In the inlet of each coil, and another In the outlet. There are valves on the circulation lines, bj) which the coil can be sucked empty. See Section VI, page 18. These also help In locating any blockage In the clrcElation system. MQNS 046*114 , . XII. EQUIPMENT LIST, oontd. t uraaoea, oontd. j XII - 45 Equipment List PC-045 -066 FO-045 PC-046 PC-066 oontd. Mr. Purzey reported! December 5, 1951, that the coils last about 12 months, but may require cleaning every 3 or 4 monthB to remove plugs. At Newport the still coll is Interchangeable with that of the diphenyl department still, A,temperature difference recorder controller was Installed on the heater coll fit Newport, and a CO* 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. Electric, Air Drying Purnace purchased from Lectrodryer Corp. Serial 270, Size BWC-250, dual-absorber type. 40# pressure. 440 voltB, single phase, 60 cy. 4-8 hours operation. 300 amp[. heater on each side thermostati cally controlled, at 270*F. See T-014. Order B7403 on 4/14/36, Req. 691191 on 4/14/36. Price $1,350.00 on 6/30/36. Has blower with Motor M-01486 for scavenging. Selves the alr-blowing tanks CT-O750 and CT-02086, and the melter CT-0763, In the latter case at pressure enough to blow the charge to the chlorlnator. Brings the dew point of the air to between - 10*P. and + 10*P. ! 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 ^ year. Steel Heater Fumade for No. 2 still. Drawing C-3479. Brick lining, coll, burners and stack. S. W. comer of the 20'6" level plareforai. Bldg. CR. Generally like PC-045. Drawing C-3479 (missing April 1946). HONS 046415 XII. EQUIPMENT LIST, contd. XII - 46 Equipment List 1-016 - 0441 Instruments 1-016 Taylor Temperature Cl^ntroller. Drawing D4417, Size 1, #36JR523. n rect acting, self acting, with std. double seated v'^lve lncl. steam strainer. Range 110*P. to 170*P., Set 122*, 25' tubing 3/4" union hub connection placed 7 from bulb end. Order B3443 on 3/10/B'7, Req. 76979 on 2/15/37. Chg. out 3/51/31, $76 57. On CT-0848, Pyranol blender. 1-0108 Rotameter Instrument! purchased from Eoonomy Equipment Co. Serial #10166. Por scrubber TW-0182. No. 6, Pig. 25 bronze with ptalnless steel float calibrated for max. cap. of 300 gph{ water. . Order B19959 on 11/lb/37, Req. 83079. Price $66.70 1-0204 Poxboro. DP cell. Stainless Steel body. Ni diaphragm. 1-0244 1-0581 TIC, LAN. 2 point Mloromax. Range changed to 0-600*C. Used to replace j MSC-0668. Palmer Superoar Dlall Thermometer, 8" oone Mercury actuated. Range 0-150*C., 25' stainless steel oonneoting tubing with adj. damp, fig. to be located 91 from end of bulb. Order B18385 on 8/23/40, Req. 12533 on 8/23/40. On 1269 stg. tk. CT-D1310. Price $56.50 1-0598 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-190P. to 25O*P. Size 1, pbess N. 0. on CT-0748 diphenyl stg. tk. Order B23310 on 10/28/40, Req. 14583 on 10/28/40. Price $69.05 1 1-0441 L & N 6 point temperature recorder. Serial #389329, #40352M, Model S, mlbromax strip chart temperature recorder. Type DC potentiometer - multi point curve printing, record numbered and color dot for each HONS 046416 XIX. EQUIPMENT LIST, eontd. XII - 47 Equipment List 1-0441-01118 Instruments, eontd. 1 -0441 oontd. thermocouple. Time cycle - 30 Bee. normal for each point. Order B13260 on 6/18/J1, Req. 21072 on 6/17/41. Price $395.00. In second floor control room. Bldg. CR. 1-0*43 Watt hour meter Instrument purchased from Oeneral Electric. Serial 21-220-743. #fe * 905. Type V3A, 220 to 5 CT use. Order B 9118 on 4/15/ii. Req. 20313 on 4/14/41 Chg. out $51.40 on 6/30/41. In cabinet outside E vail Bldg. CR. 1-0507 Palmer Dial Thermometer. CABI #217, Range 0-150eC. In Pyranol Mixing Tank CT-01321. 15 ft. stainless steel special armor flexlbl* tubing plain bulb. Order B20438 on 12/1/41, Req. 24426 on 9/9/41. Chg. out $49.59 on 12/27/41. 1-0835 Bailey Integrating ant Recording Plow Steam Flowmeter. Serial #13996R. Order BII589 on 9/25/45, Req. 67905 on 5/II/45. Price $348.00 In control room B wall. For steam from the 200 lb. main. Supplies the ejectors^ the high pressure colls In the air-blowing tanks, and melter. See MSC-0682 for the low pressure Bteam meter. Taylor Fullscope recoiling controller on the No. 1 still vacuum system. 1-01118 Chlorine flow recorder controller on No. 5 chlorinator. See also MSC-0663, paje 6l. 0668, pa,(e 61. 0675, pate 61. 0682, paje !";3. 0705, pa je 63. Foxboro steam flow controller, 0 - 2000 lbe. per hour. HONS 046417 XII. EQUIPMENT LIST, oontd. XII - 43 Equipment List 1-01547 - 02045 Instruments, contd. 1-01547 Taylor PR, 2 pen, wish alarm and shut off valve. Chlorine lines. 0 - 100 pslg. 1-01894 1-01941 1-02019 1-02045 Taylor Fulscope TI Cj 0-150*0. working at 50*C. Tin-sprayed thermo wbll. On blender CT-02621. Controls Fisher diaphragm valve on steam to coll in CT-02621. Pyranol blender. Foxboro. D.P. cell tor chlorine liquid in store tank. Taylor Fulscope LRC. Worthington meter, gallons, well water. See also MSC - 0663 0666 0675 0682 0705 0770 01395 I MQNS 046418 XII. BgJIPMENT LIST, oontd. XII - 49 Equipment List L-031 Elevators L-031 Bucket elevator from general Conveyor It Mfg. Co. Drawing K-870. Lg. ti be 22'4-11/16" OA c to c take up shafts and 20'6" oaising and head section 3/16" and boot 1/4". 6" belting 4 ply H covered pinched 10-7/32" for buokets *f 4g" x 3" chrome steel. Order B10455 on 5/15/i16, Req. 70140 on 5/25/36. Price 4491.20. Drlveg by M-0834. Drive drawing B-661 Solid Aroclors (dismantled 1952). See also V44, 45, 46 onveyors from flaker D-012 to Jelevator L-031, and ol am hoist MSC-01495 over the Sparkler filter B-017g and electric hoist HSC-O655 for solid Aroclors. A chain hoist Is used also to lift bags of lime to the still operating platfd:irm. MONS 046419 1 XII. EQUIPMENT LIST, contd. XII - 50 Equipment List M-0790 - 0834 Motors Note! The motors ere changed to other duties from time to time, but the following details will serve to indicate the types of motors used K-0790 Westlnghouse Motor 3 HP-1750 RPM. Serial 7435. Type CS, sq. cage Induction notor, horlz., frame W225, 220/440 v, 3 ph,, 60 oy., 8/4 sunp., 55*C. temp., rise, style 801068V, class 1, total enolbiaed, ball bearing. Rac'd. 8/20/35. (#6058-5077) *78. On pump P-0346. ' M-0827 Motor 3 HP 1200 RPM from Wagner Electric Co. Serial #1718199, horizoni'tkl Induction motor, totally enclosed, fan oooled, bail be|ikring, 3 ph, 60 oy, 220/440 volts, 8.2/4.1 amp., type CPI, f:rami 254, model W425198. Order B8184 on 4/23/36, Req. 69P76 on 4/23/36. Chg. out $94.16 Also drives V-046 t]hru second chain on link belt; drives 0-012 flaker thru MSC-0639 speed reduoer and chain. M-0830 Motor 2 HP 1800 purshased from General Electric. Serial HK-1407, Horizontal induction, totally enolosed, fan oooled ball bearing, frame 225, 2HP 1740 RPM, 220/440 volts, 5.61/2.81 amp., typ> K, 3 ph., 60 oy., model SK-225-A715. Order B8169 on 4/23/36, Req. 69377 on 4/23/7(6. ' Chg. out $73.84 on 5/30/36. Drives P-0565. M-0832 Motor 3 HP 1200 RPM purchased from Wagner Bleotrle. Serial 1714954. Horizontal Induction, totally enolosed, fan oooled, ball bearing, 220/440 volts, frame 254, 3 ph., 60 oy., type CPI, model W42J198, 8.2/4.1 amp. Order B8178 on 4/23,^6, Req. 69378 on 4/23/36. Chg. out $94.16 on ii/30/36. On blower B-094. M-0834 Seared head motor 2 HP 1200 RPM purchased from Master Electric Co. Serial. HE-975, air Jacketed, totally enolosed, fan oooled, 1140 to 220 RPM single reduction parallel geared head, 220/440 volts, 3 ph., frame 254, type PA, style 47476, 55* coot, rating, 6.2/3.1 amp. Drives L-031. Order B8156 on 4/24,^36. Req. 69373. Chg. out $109.14. MONS 046420 XII. EQUIFHENT LIST, contd. XII - 51 Equipment List M-0835 - 0848 Motors, contd. M-0835 Reeves vertical motodp;lve 14 HP 1800 RPM purchased from Bates Co. Motor seri 41 1914691, motodrlve unit serial MD-1136. Size 4253-E 18, model V 34J223, 3ph, 60 cy., 1.9 amp., frame 224, to 1 speed variation and 30 to 1 gear reduction, hand dhain control and chain In place of standard hand wheel. Order B 7376 on 4/l4/}6 Req. 69123. Charged out $300.96 iDrives V-044. M-0836 Reeves vertical motodrlve, same as M-0835. Drives V-045. M-0841 Oeared head vertical niounted motor 5 HP purchased from Master Electric Co. ferial HE-988. 220,440 volts, 3 ph., 60 cy., totally encloi fan cooled, ball bearing, type PA, frame 11230 # 254 |DP - 1725 to 80.2 RPM Style 47478 - cont. 53 c. Order B 8155 on 4/24/36 Req. 69375 on 4/23/36. Chg. out $211.84 on 6,/feo. Drives stirrer in blerldlng tank CT-0779. M-0846 Vertical mounted Induction motor. 1 HP 1800 purchased from Oeneral Electric. Serial EP-2773. Totally enclosed fan cooled, ball bearing, thrust type with ring base and drip cover, 3 ph 60 ksy., 220/440 volts, 1720 RPM. Model 5K204A1550. Prakne 204y Order B 8175 on 4/23/36, Req. 69371. Chg. out $55.44. Drives P-0573 M-0847 M-0848 Vertical mounted mdu.eft.Ion motor 1 Hp 1800 purchased from Oeneral Electric Co. rial EP-2779. Totally enclosed, Kfan cooled, ball bearl| , etc. same as M-0846. Drives P-0909. Vertical mounted lndu<ict:Ion motor 1 HP 1800 purchased from Oeneral Electric Co Serial EP-2777. Totally enclosed, fan cooled, ball bearl|ng, thrust type with ring base and drip cover, 3 ph., 60 py. 220/440 volts, 1720 RPM, model 5K204A1550, frame 204y| Order B8175 on 4/23/36| Req. 69371. Chg. out $55.44 Drives P-0674. MONS 046421 XII. EQUIPMENT LIST, contd. XII - 52 Equipment List M-0849 - 0871 Motors, contd. M-0849 Wagner horiz. induction motor 5 HP 1800 Serial #1714362, totally enclosed, fai cooled, ball bearing, type CPI, frame 254, model W-30J195, 3 ph., 60 cy., 220/440 volts 1750 RPM, 12.6/6.3 aup. Order B-8177, Req. 69372, chg. out $97.08 6/30/36 Drives P-0578. On pump P-0578, on No. 2 chlorlnator. M-0850 M-0851 Horizontal induction Wagner motor 5 HP 1800 Serial 1718376. Same as M-0849 and 01'$51. Drives P-0579. On pus P-0579 on #3 chlorlnator. Motor same as M-0849 and 0850. Serial 1718377. M-0853 M-0854 Vertical mounted lndik<ictlon motor 3 HP 1800 0. E. Makers, Serial PP-1104. Totflly enclosed, fan cooled, ball bearing, thrust type with ring base and drip cover, 3 ph. 60 cy., 220/440 volt^ 1730 RPM, model 5K225A2430, 8.54/4.27 amp.,frame 225Y, type K. Order B 8174 on 4/231, /36, Req. 69367. Chg. out $95.92. Dri ves P-0583 Motor Serial FP-3898 same as M-0852 and 3, on CT-0768. M-0856 Vertical mounted induction motor 3 HP 1800. Made by 0. E. Serial FP-2457I Thrust type and drip cover, ring base, class 1, groupJd, underwriters #5474727. Explosion proof, ball bearing,j1720 RPM, 3 ph., 60 cy., model 5K225A2446, 220/440 Volts, 8.42/4.21 amp., frame 225Y, type K Order B8172 on 6/26/36, Req, 69368 on 4/23/36. Chg. out $115.58 on 7/13/36. Drives P-O585. M-0871 Vertical induction motor 5 HP - 1750 RPM from 0. E. Serial PP-3177. Toti.lly enclosed, fan cooled, ball bearing, thrust type with ring base and drip cover. 220/440 volts, 13.9/<.95 amp., frame 254 y, type K, 60 cy., 3 ph., model 5K254B1930. Order B8173 on 4/23/; 6, Req. 69369. Chg. out $124.21 on 7/31/36. Still pimp drive, drives P-0593. HONS 046422 XII. EQUIPMENT LIST, o6ntd XII - 53 Equipment List M-0873 - 0914 Motors, oontd. M-0873 M-O875 Vertical mounted Induction motor 5 HP - 1750 RPM. Purchased from 0. E. Serial FP-3I07 . 220/440 volt, 60 oy., 3 ph., totally enclosed, fan cooled, ball bearing, thrust type with ring base and drip cover. Model 5K254B1930,! 13.9/6.95 amp., frame 254y, type K. Order B8176 on 4/23/36, Req. 69370. Chg. out $124.21 pn 7/31/36. Drives P-0592 In tank outside. Horlsontal Induction motor 1 HP 1200 made by 0. E. Serial DP-5227, totally enclosed, fan cooled, 60 oy., 1130 RPM, model 5JC204A1036, 220/440 v., 3/45/1-73 amp., frame 204, type K, 3 phase. Order B13188 on 7/2/36, Req. 71152, ohg. out 7/21. Drives P-0595. ! M-O885 M-0904 Vertloal 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 oover. 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, Ren. 71147 on 7/1/36. 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 vblts, 1150 RPM, 55* cont. rise, type NF 254, 8.4/4.2 Order B17431 on 9/1/36, Req. 72637, Chg. out $90.40 on 10/24. Drives B-bl05 in Bldg. CR. M-0914 Blaokmer motor 7y HP 1800 made by Louis Allis. Serial 217543. Totally ^enclosed, fan cooled, type JX, 3 ph. 60 cy., 220/440 ' Its, 1750 RPM, frame 284, class 53d, form B, 18.4/9.2 lamp. Order B21241 on ljo/22/36, Req. 74034, Chg. out $133.12 Drives Naphthalene pump P-0617 for CT-0347. MONS 046423 XIX. EQUIPMENT LIST, oontd. XII - 54 Equipment List M-0955 - 01229 Motors, oontd. M-0955 Portable "Llghtnln-JiMlxer" 1/4 HP 1725 purchased from Mixing Equipment Co Mixer Serial 37108, Motor Serial HK-4536. CABI 106/:'1956. Model C-4, 3" folding monel metal propeller moitiiel shaft, 4/2 amp., 110/220 volts, single phase, 60 0/ class 1, grpup d, explosion proof, underwriters P-519(;$72, extension cord and attachment plug. Order B1340 on l/l|3/37, Req. 76212 on 1/18. Chg. out $109.42 on 2/27/37 Used for drum shipments. M-0975 Motor 5 HP 1800 pu[i^chased from Wagner Electric Co. Serial 1725358. T(Otally enclosed, fan cooled, ball bearing. Induction motor, type CPI, frame 254, model W30J247, 3 ph, 60 4y. 220/440 volts, 12.6/6.3 amp. oont. rating 95*C. Order B2834 on 2/91, /37, Req. 76765 on 2/5/37. Cost $95.61. On P f0629. On No. 1 ohlorlnator pun P-0629. M-0905 Wagner Vertical Motor 7$ HP - 1800 RPM. Serial #1728961. Totally[enclosed, fan oooled, ball bearing, type CP-2, frame 234y, 440V, 60 oy., 3 ph., 18.4/9.2 amp. 1750 RPM, model W40V143. Order B3323 on 2/12/ 37 and Req. 76927. Chg. out $133.98. [inst. to drive submerged pun In TOB stg. tank CT-0$48. On P-0346. M-01229 Vertical mounted li kductlon motor 1 HP 1800 purchased from Louis Allis [serial 269797. Totally end. fan oooled, ball bearli thrust type with ring base and drip cover, weathe: iroof conduit connection box, type IS, frame 204v, oil isa L, form B. 220/440 volts, 3 ph, 60 oy., 3/1 5 amp. oont. 55*C., 1730 RPM. Order B3853 on 3/4/38, >q. 86889 on 3/3/38. Chg. out $55.20 on 4/29/38. On pump P-0731. HONS 04642'* XII. iUIPMBNT LIST, contd. XII - 55 Equipment List M-01377 - 01573 Motors, contd. M-01377 0. B. Motor 2 HP - 1800 RPM. Serial MR-8969. Totally enclosed, fan cooled, sq. cage, induction motor, type K, ball bearing, 220/440 V, 60 cy., 3 ph., frame 254, 1760 RPM, model 5K254B91. 5.44/272 amp. Order B15B55 on 9/26/38, Req. 91711, Chg. out 475.00. On P-01111. M-01456 Westlnghouse horizontal motor 3/4 HP 1200 Serial 4139. Totally end. ffn cooled, low starting current, 440 volts, 3 ph., 60 cy., 1160 RPM. Type CS, frame 204, 2.6/1.3 amp., style 1707136.. 55*C. rise, ChL out mach.`441.03 on 12/29/39 Order B17367 on[l2/l8/39i Req. 1357 on 8/31/39 on Blower B-0148 M-01469 0. 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, 9.06/4.53 an., oent. 55*0. rise. Order B10935 on 9/21/39, Req. 1991 on 9/20/39. Chg. out 472.47 on 11/30/39. On gear pump to P-0159. M-01486 M-01501 M-01573 Qeneral Eleotrlt Motor 1/4 HP 1800, totally end., model 5 KH47AB9$4, type KH, 110 volts, single phase, 3.4 amp., 55* cint. Order B17923 oml0/l7/39, Req. 1531 on 9/8/39. Cost 424.25. On Leotrodyer pf-046. Replaced by M-Oj.706. . Motorized car spotter 5 HP 1640 RPM purchased from Link Belt Co. motor ferial 307939, spotter serial 5252, 220/440 volts, $0 cy., 3 ph, type IK, frame 225 VY, class 3, form Bl 17.2/8.6 amp. 55*0. Order B26741 onll2/29/39 Req. 5128 on 12/29/39. Chg. out 4373.8s. On track 11 at load dock. HONS 046425 xii. a 3UIPMKNT LIST, oontd. XII - 56 Equipment List M-01622 - 01660 Motors, oontd. M-01622 General Electric mi or 7i HP, 3600 RPM, Serial BU7108. Totally enclosed fi 1 cooled, type KP, model 5KP254C25, frame 254, 220/440 ., 3 ph., 60 cy., 3435 RPM, Drives ML-045. Order B4lllJB on 2/20/40, Req. 6737 on 2/fO. Chg. out $114.96. M-01629 Vertloal motor 7$ HP purchased from Turbo. Made by Meetinghouse. Serial 2640. Totally enclosed, fan cooled, frame 284, class 1, RPM at full load 1735, cont. rating at full load 55 *C. Use, 220/440 volts. 3 ph, 60 cy., 18.8/9.4 amp., style 1071192. Order B8337 on 5/20/40, Req. 8441 on 4/9/4oL chg. out $112.66. On MSC-01205. Driving agitator lnT CT-0808, final chlorlnator. M-01650 M-OI656 M-01660 Louis Allis motor f HP, serial 258334, 1750 RPM, type JS, frame 254, class 43h, form B, 220/440 v., 3 ph, 60 cy., 13/6.5 amp., full load 55*0. cont. Order B26263, Req. 85432 on 12/24/37. On Sparkler press pump. Wagner Electric Motor 5 HP 1800 RPM Serial 1758959. Horlsontal totally enclosed, fan cooled, ball bearing, less base and puller, type CPI, frame 254, 220/440 v., 3 ph., 60 cy., 1750[ RPM, cont. rating 55*CP, model 1B8J247B, 13.2/6.6 Up. Order B12802 on 7/8/40, Req. 10231 on 6/5/40, chg. out $87.92. Drives P-OIO56 Taber Horlsontal pump. General Electric Motor 1 HP 1800 RPM purchased from Taber Serial OU1902. Totklly 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. 55*0. rise I Order B13111 on 6/10/40, Req. on 6/10/40, chg. out $50.19. Drives new Taber sub. pump P-0909. MONS 046426 XII. B tUIFMENT LIST, oontd XII - 57 Equipment Li at M-01697- 01772 Motors, oontd. M-OI697 Motor made by Waliiner 1/5 HP, CABI 169, 50" dla. type S-60WS, style 1241;9-4622 portable circulating fan, single ph., 60 cy , 115 volts, complete with guards, 'Jloor column, and cord. B16528 on 7/26/40. Req. 11797 on 7/26/40 Chg. out $60.58. Used on operating platform near chl<lorlnator. ' M-01706 M-01718 Vertical mounted Induction motor 5 HP 1800 made by 0. E. aerial JU3498. Totally enclosed, fan cooled, ball bearing, thrust type with ring base and drip cover, " frame 225VY, type K, 220/440 v., 5 ph., 60 cy., l|50 RPM, 8.54/4.27 amp., cont. 55*0. rise. Order B18445 on 8/25/40, Req. 12560 on 8/25/40. Chg. out $92.24 on 10/51/40. On P-0929 Taber. Replaced by M-01601. Loula Allis Motor 7$ HP-1800 RPM, Serial 555985. Totally enclosed] fan cooled, weatherproof conduit. connection box. jType JX, frame 284, 220/440V, 5 ph., 60 cy., 1750 RPM, Class 0, form R, 19.6-9.8 amp., full load temp, vise 55*C.. trine hours cent. Order B21071 on S/50/40, Req. 15674. . Chg. out $115.00 on 10/51/40. . Drives (Falk Reducer MSC-01288) on Turbo Mixer for CT-01521. I . 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 B26350 on 12/4/40 and Req. 15856. Chg. out $36.98. I On B-034. M-01772 Lewis Motor 1/2 HP 3600 made by 0. E. Serial J33, CABI 169, totally end., model 5K49BC756A, type X, rise 55*0., 440 v., 3 ph., 3450 RPM, amp. 7. Chg. out $25.00, Req. 16663 on 12/30/40. Use with P-0378 1 n 0T-0640. . HONS 0^6427 XIX. EQUIPMENT LIST, contd. XII - 58 Equipment List M-01811 - 01995 Motors, oontd. M-0I811 Louis Allis Motor 2 HP 1800 RPM Serial 385335. Totally enclosed, fi cooled, normal starting current, Cl oondult oonneotl box, less bass and pulley. 220/440 volts, 3 ph., 60 oy 1750 RPM, type JS, frame 225, class M, form R, code H, 5. '2.8 amp. Order B4136 on 3/7/V1, Req. 18313 on 2/17/41 Chg. out $65.36 on 00/41. . On ground floor N. of P-0172 on P-01037. M-01850 Louis Allis Motor 1 HP 1800 RPM Serial 395205 Totally enclosed, fi4 cooled, ball bearing, 220/440 v. 3 ph., 60 oy., 1740 RPM, type IS, frame 204, class L, form B, 3.1/1.55 am$ Order B7411 on 3/26/4l, Req. 19634 on 3/26/41. Chg. out $36.98. Of ground floor. M-OI856 Louis Allis motor 5 HP 1800 RPM Serial 391009. Totally enclosed, tk,n cooled, vertical flgd. mounted (Cl oondult connect^on box) normal starting current, 3 ph, 60 ey., 220/440 v., 1750 RPM, type JS, frame 254 VB, class N, form R, oo$,e H, 1.3/6.5 amp. full load temp. rise 55*C. Order B6380 on 3/13,/u, Req. 19213 on 3/13/41. Chg. out $109.74 on 6/30/41. On P-0997 top of 3-062. M-OI859 Unit heater from Am Blower Corp. Serial 1939. Order B8936 on 4/11/'41 and Req. 20240. Chg. out $48.73, In MSC-01393. M-01995 Motor 1/3 HP 1800 RPIM made by 0. E. Explosion Proof, clkias 1, group d, underwriters No. FA352-094. Totallyf enolosed, fan oooled, ball bearing, type K, frame 45A, (nodel 5K45AC1024A, temp, rise 55*C. trine rating cont.. 440 v., 3 Ph, 60 oy, 1725 RPM, 55 amp. Order B4625 on 2/21/'41, Req. 18520 on 7/21/41. Chg. out $29.75 on P/30/41. On P-01054. MONS 046428 XII. EQUIPMENT LIST, oontd. XII - 59 Equipment List M-02170 - 0514 Motors, oontd. M-02170 Oeared head motor 5 HP 1800 RPM. Made by Master Elec. Serial PD-9. Parallel, air Jaoketed, fan cooled, totally enclosed, frame # 254, 80 RPM on mixer shaft, barrel mounting for Vertical operation, style 10354J, 220/440 v., 3 ph., 6p cy., 1725 RPM, type PA, amp. 13/6.5, 3 Ph, trine nours cont. FI/TR 55*C. Order B3580 on 4/8/4E, Req. 30060 on 2/10/42. Chg. out $259.25. oti CT-01399. #2 blender. M-02175 M-02877 Office ] Drives 1 M-03133 Drives ] M-04592 Drives ! M-0469I Drives 1 M-04817 Exhaust M-04025 Drives : M-0514 Drives : agitator In #2 mix tank CT-02621. MONS 046429 XXI. EQUIPMENT LIST, contd. XII - 60 Equipment List ML-045 Mills ML-045 "Helix-Seal" Impact filll purchased from Williams P. C. & Pul. Co. Serial #9 >>! 94. Size #1. Less drive pulley.OrLven at 5500 RFM thru V belt drive furnished by Monsant). Order B2371 on 2/1/37. Req. 76578. Price $420.00. West lean-to. Hand fed. Por solid Aroclors. Dismantled 1952. 046A30 mons XXI. EQUIPMENT LIST, eontd. Miscellaneous Equipment XII - 6l Equipment List MSC-0639 - 0675 MSC-0639 Speed reduoer made by W. A. Jones Foundry, Serial 83957, #105W, assembly #1 style 4, 36 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. OR, lean-to.'. MSC-0655 Shepard Electric Lijf tabout Holst. Serial 36306. 440 volte, AC, 3 pb|, 60 cy., single speed oontrol with motor drive ttrolley. Holst speed 18' per min. lift 19'. Holst motor 3 HP. Travel motor 3/4 HP. order B7405 on 4/1V36, Req. 69120. Chg. out $906.70. MSC-0663 Multiple temperatu* recorder 40112-291 Micromax Model S strip ehartj 2 prints, surface panel $300.00. Made by Leeds and Northrup, Serial 276758. Order B9975 on 5/1:i/36, Req. 69970. In lean-to. Bldg. CjR. MSC-0668 M8C-0675 LAN Temp. Reoordefir made by Leeds and Northrup. Dwg. B-666, Serial 1276807. (1) #40354-291 Mlc:nomax model S strip chart, multiple temp, reoorder, 4 point. (Multiple colored dots Instead of numbers on prlnlj wheel). Surface panel mounting $465.00. (2) Extra for high Contact for operating alarm $20.00 Order B9976 on 5/1!a/36, Req. 69969, Chg. out $491.82. South wall, west 1instrument, Bldg. CR.(See note on next pg.) Replaced by 1-0244 Temperature Record^:r purchased from Leeds and Northrup. Serial 276784. #4<;1353-291 Mlcromax, model 3, strip ohart multiple poll it temperature recorder for 3 prints. (Multi-colored doti Instead of numbers on print whsel.) Surface panel mounr' ising $400.00. Extra for high contact for operating alarn} $20.00. 3 thermocouples to fit wheels. Our Dwg S-666. Order B9977 on 5/1!9/36, Req. 69968, Chg. out $324.05. South wall, east ii.instrument. Bldg. CR. (See note on top of next page.) MOWS 046431 XII. EQUIPMENT LIST, contd. ! XII - 62 Equipment List MSC-0668 - 0676 Miscellaneous Equipment, oontd. MSC-0668 -0675 Mote: Reoord the following temperatures: Batch temperatires In chlorlnators: CT-0744 0745 0833 j 01283 0808 Goods temperatire In diphenyl store tank CT-0748 Coll Inlet temperature on the stills S-043 and 062. " outlet " " .................................................. Vapour temperature entering the condenser. Goods temperature in receiver. Goods temperatire In blending tank, CT-0779. Goods temperatire In finished product receiver,CT-O78O. MC8-O676 Drawing B-666 shows thermo-couple wells. Drawing B-6868 shows monel thermo-oouple wells as used In distilled Aroolors. Gas Electric Water Booler for drinking water. Made by 0. E. Compressor 6541356, cabinet 6600807. Model RM-51, pressure type, 110 v., single phase, 60 oy. Order B14045 on 7/14/36, Req. 71432. Chg. out 7/31/31, 176.00. On 12' level. Bldg. CR. I MONS 046432 XII. EQUIPMENT LIST, contd. XII - 63 Equipment List MSC-0681 - -734 Miscellaneous Equipment, oontd MSC-O681 Rail truck purchased from Nutting Truck Company. Dwg. C-827. Welded construction, wheels equipped with Hyatt Roller Bearings. Used as weigh truck for still pots on SC-095. Includes traok. Order B11134 on 6/1/36, Req. B70395. In lean-to Bldg. CR MSC-0682 Brown mech. flowmete:r. Serial 115969. Recording and Integrating steam at 65# ga. press. Dry sat. orifice monel In 4" std. hoy:'lz. line, (used on 80 lb. main). Max. flow 4000#/hr. Model 2221-x40. 2 lgs. 25' of i" copper tubing an^l conneotors - Monometer valves, Elec, clock for 110 v - 60 cy. Order B14604 on 7/2$!,/36, Req. 71548 on 7/20, chg. out $280.00 MSC-0705 Palmer Industrial Tinermometer CABI #89. #249 - 45* reollnlng Industrial therm. 12" scale, steel separable socket - 30" long wj th 1" std. pipe thread. Range 0-200*C. No nlokel plating. fcase painted reg. lacquer. Order BI8261, chg. $ut $28.05 on 10/31/36. On Buffer tank CT-0|50. MSO-0718 Lab and Office of D>:ipt. CABI #89 - 1936. 20' x 10' x 10' high Includes partition and elec, lights on NW corner of CR. MSC-0725 Laboratory testing Equipment. See reports on 0. E. testing. MSC-0734 Electric drying ove$ CABI 89-1936. Cat. 7764, 3 heat oven with one shelf and 9525 thermometer for* 110 v., AC current. Belong! to the Pyranol Dept. Order B23080 on ll/li6/36, Req. 74628. Chg. out $26.60. HONS 046433 XII. EQUIPWMT LIST, oontd. ni - 64 Equipment List MSC-0760 - 0903 Miscellaneous Equipment, oontd M8C-0760 Vacuum Jet made by Vjprthlngton. #2i JFD-S std. 3s tag<;e steam Jet ejector with 2nd stage condensing andl fitted with Jet type Intercooler, Jet to be Cl bronze pozzies, heads, monel nozzles. Order B7404 on 4/14,\ke Req. 69211 on 4/14. Chg. out $796.00 on 6/30/36. - N of MSC-01392 Bldg. CR. Ejectors NSC-0760, 01392, and 01686 are In a row running north and south In t tie building, and they are Inter connected so that th im oentre one can serve as a spare for either of the ot tier two, to serve the vacuum stills 8-043 and 062. Cast Iron bodies with monel Jets. Karbate ejectors were to be tried. (Anniston were using ejector* with two stages of Karbate Jets, then a wet oondenser, and then two more Karbate stages.) Faulty behaviour, due to erosion or corrosion, or to wet or dirty steam, |Ls very objectionable as allowing water to get baok Into the goods. Karbate units have to be very carefully supported to prevent strains from the pipe lines. More reoently procelaln units have been Installed at the Krummrioh plant. MSC-0770 Super Tank Gauge mads by Varec. Fig. 68, Oastlght Use on tank aooordlng 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-0848j. TCB store tank. MSC-0903 Steel cabinet made Medart. CABI #139* 1 unit 48" wide and 24" deep x '3" high 9" ledge,bln fronts, dividers and 2 doore on lower part with lock. Order B3013 on 2/18/ 38, Req. 86579 on 2/17/38. Chg. out $50.51. HONS 046434 XII. EQUIPMENT LIST, contd. XII - 65 Equipment List MSC-0971 - 01392 Miscellaneous Equipment, contd MSC-0971 10 steel box lockers made by Medart. CABI 139. Olive green steel arrange! 2 wide x 5 high. Complete with looks, 2 keys for each look x 3 master keys oomnon to all. Lockers 12 x 12 x 15" deep. Order B15781 on 9/23/38, Req. 91603 on 9/21/38. Cost 25.75. MSC-01061 Two loading ramps made by Monsanto. For one ton chlorine cylinders, using I tyeam supports and concrete footings with I-beam rallB. East side, outside Bldg. CR. MSC-01094 Drying Oven purchaseid from 0. E. Used with P-0159-In the Pyranol plant. 4 compartment elect^:lc drying oven with 115-230 volt heating elements. 3 HP motor. Order B18935 on 9/2 ,/39, Req. 1991 on 9/20/39. MS0-01191 Metal Desk and Stoo Desk 36-5/32" wide, 42" high front, 54" high back, 31" (Jeep. Stool 30" high. Order B5169 on 3/4/4'0, Req. 7148 on 2/29/40. MSC-01205 Speed reducer made P Falk. Serial M0127-928. Size 28DZX, RPM 175* to 180, ratio 9.7. Order B8337 on 5/20,f40, Req. 8941 on 4/9/40. Chg. out 169.94. Driven by M-01629 on CT-0808. MSC-01286 Falk Motor Reducer i HP. Serial M0131-842. #44DZX, output spee! 1750 to 41.9 RPM, service factor 1i, ratio 41.9. Order B21071 on 9/3<j>1, /40, Req. 13674 on 9/30/40. Chg. out 4341.94 on 10/31/40. On CT-01321, Pyranol blender. MSC-01392 #2i Worthington vaci|i North of MSC-0760. Same as MSC-01686. Jet 3 stage. Type 9-10-11. MONS 046435 XII. EQUIPMENT LIST, oontd. XII - 66 Equipment List MSC-01393 - 02108 Miscellaneous Equipment, oontd MSC-01393 Control Room. Drag:lng C-9646. Structural steel, f}'oor plate. Bldg, tile 12 x 12 x 3. Pyrobar roof, door $nd Instrument panel for 1-0441. MSC-01495 i ton Peerless holsl| and trolley. Model C, 11' lift. Model J trolley. Order B17508 on 8/6/f'J41, Req. 23095 on 8/6/41. Chg. out $72.74 on }l/27/4l. Used to remove platiis of filter P-0172 for cleaning. MSC-01686 #2$ Worthington 3 s$iage vacuum Jet. Type 9-10-11. North of M8C-01392. Same as MSC-01392. NSC-01699 Lookers (4} made by Medart. CABI 152,1939. 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/J9 MSC-01877 Canvas tent for tang oar. Approx. 7' dla. 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 co:>#ner CS. Also elec, light In tent. order B20696 on 9/7/'43, Req. 48441 on 9/4/43. MSC-01879 South dock, wood, mug: latlc loading. Also swing plank and wood decking. On track 11 west of CS. 5' x 516". 1943. MSC-01916 North load dock mads of steel with swing plank. 5' x 7' long, 9'6" high. 5 x 5 angle columns with 6" channels to support {" steel deoklng. l" pipe railings. North of NSC-01879. SW of CS on track 11. 1936. NSC-02071 Stoneware sink. NSC-02108 Steel Hood and Duct 2' x 4' oounter balanced with 6" dla. steel duct to 4utslde of Bldg. Hood located over F-0159 0. E. Filter Press. HONS 046436 XII. EQUIPMENT LIST, contd. XII - 67 Equipment List MSC-02426 - 04442 mBoellaneous Equipment, contd. MSC-02426 Ducts, hoods, dampers. MSC-03417 Air cond. unit. MSC-03523 Vac. ejector. Worthington, Porcelain, Karbate. 10" Porcelain condenser. 10 lb. hr. air at 2 mm cbs. 150 pslg steam. S5*F. well water. MSC-03611 Duct and hood. MSC-03689 Haveg sink. 4' 8" x 19" x 18". M8C-037O6 Water cooler. Drinking water. MSC-03741 MSC-03835 MSC-04018 1/2 T chain hoist above P-0172, j 1/2 T chain hoist #2 mix tank.] Work bench Pyranol plant MSC-04109 MSC-04132 Llghtnln mixer (only - not motor) 7i HP side entering metallized with ojoi5" Al. See CT-02621. Water cooler. ! H8C-04442 Hand hoist. Heaters for plant office and for Instrument and control Oas supply and melering. room. Water hose with steam mixing Jet for cleaning the floor. Desks. Clothes lockers. Test bench. Phone. Clock. Pramed Instructions for special pieces of equipment. Drinking water supply. First aid cabinet! PIre alarm & extinguishers.Sprinklers Installed In all_ Hose connections for casual gas heating. Waste oans. Used water collection. Lighting. ; HONS 046431 XII - 68 Equipment List 0T-0640 - 0751 XII. EQUIPMENT LIST, contd. Open Tanks 0T-0640 Drum, 110 gal. ICC5, pABI #217-1941. With float valve on city water line. Conhai ct 3 OFM pump P-0378. To pump from drum through rotomete|p to add absorption system. Black Iron $18.50 as trans from pept. 360. 0T-0751 Seal cans for baromet|pic legs of the ejectors. MSC-O76O, -01292, -0:1685 On the ground floor. Steel vessel 4'0" I.D . x 6'0" high, for city water, to conform to state law. I MOMS 046438 XII. EQUIPMENT LIST, contd. Pumps XII - 69 Equipment List P-0346-0575 Note; .The pumps are changed around from one duty to another, in the cou:yse of ordinary maintenance work, but the details given bAlow will serve to show what type of pump is used for any given duty. Oversized pumps may be used in some cases to diminish the number of types required in the depart]ment. P-0346 P-0378 Swaby Submerged Pump made up 11/18/29. Size #1$, Cast Iron. On CT-0848 In TCB store tank, CT-0848. Chas. Lewis pump Serial 4597, Type BA-481, cast iron vertically split shell cent. pump. Cl bed plate connected with flex, ooupling, direct to 1/4 HP 3600 RPM motor. OB M-0466, 3 gal. PM - 35' head, 3450 RPM. Order B693 on 1/15/31. Price $68.00 incl.motor, M-01772. Boosts city water to HC1 absorber. P-0427 P-0565 Horizontal oast iron pump 1$ HP Monsanto Design. Direct connected, cold rolled steel shaft. Includes base, coupling and c guard. Blaokmer pump. Serial 197033, type PA-50L bronze rotary pump, bronze lining, bronze steam Jacketed heads, monel shaft. Cl base, 1.65' sp. gr., temp. 350 to 500*P. - 50 gal. Order B-8170 on 4/23/36. Chg. out $155.45 on 6/30/36. Distillate traryrfer pump. P-0571 Oberdorfer gear pump for filter press. Motor M-OI650. P-0573 Vertical submerged centrifugal pump purchased from The Engineering Equipment Co. Serial 33007, Size L-QB with l" inlet and 3" outlet. Compare P-0604, which is a Taber pump on #4 scrubber CT-0759. P-0574 Ditto. P-0575 Taber submerged pump Serial 33009. Order B7517 on 4/16/36. Req. 9161 Chg. out $177.80 on 6/30. Direct to vertical M-0848 ijn CT-0756 on #1 scrubber. Same as P-0573 and 0574. MONS 046439 XII. 1 iCUIPMBNT LIST, eontd. Pumpa, oontd. XII - 70 Equipment List P-0578 - 0580 P-0578 Taber horizontal oe;litrlfugal pump. Serial 33040. Type L-2, 2$" inlet 2" 01iqtlet connections. Semi-steel with monel shaft and wate r Jacketed stuffing boxes. Bed plate ready to receive mo^or. 20' static head, rate 80 g.p.m. 1.5 sp. gr. at 500*: Uses M-084g. On #2 chlorlnator. CT-0744. / .Order B8237 on 4/24,736, Req. 69401. Chg. out $152.92 on 6 30 There are four pumps P-0578, 0579, 0629 and 0907, one for each main chlorii.nator. Liquor in from chlo:iplnator bottom outlet and out back to the chlorlnator. The charge can be pumped, if necessary, from one chlorlnator to another, or to the air-blowing vessels CT-0750 and CT-2086. No. 1 chlorlnator cain be emptied by gravity to the gas-fired ohlorlnator CT-0808 and there is also a pump line for the same service (dlsus 4d). The charge from No. 1 chlorlnator can be pumped diree tly to No. 1 vacuum still S-043. There is a line by fhlch partly ohlorinated diphenyl can be pumped from a chiorlnator to any scrubbing tank, CT-0759, -0760, -07$:1 or 01014. There is a sampling cook on each pump delivery, with a small box to hold tpie used Bample material, and to deliver it back to the pump intake. P-0579 P-O58O Taber horizontal cejhtrlfugal pump. Serial 33041. Same as 0578-80. For mi(idle chlorlnator CT-0744, uses M-0B50. On #3 chlorlnator or 0833. Taber horizontal ce|^ltrlfugal pump. Serial 33042. Same as 0578-79. Prom ow tank CT-0750. Uses M-O85I. HONS 046440 XII. 1IQDIPMBNT LIST, contd. XII - 71 Equipment List P-0582 - 0593 Pumps. contd. P-0582 Taber vert, submerged centr1 Pfigal pOmp.'. " Serial . 35048. , Pig. 1940, Size C-3, 2i" Inlet, 2" outlet zconnections, bronze except shaft which Is monel metal, 11'6" length of col pipe. Spare pump for underground tanka. Order B7514 4/16/36, Req. 69158. Chg. out $409.20. Direct to 1 -0852. Same as P-0583 and 0584. Used In Aroclor 1260 store tank. Submerged pump In CT-I0768 TCB Btore. P-0583 Taber vert. subm. oerit. pump. Serial 33049. In CT-0769, direct to M-0853. Same as P-0582-0584. Aroclor storage. P-0584 Taber vert. aub. cent pump. Serial 33050. In CT-O768, 1254 store tank, dlrq et to M-0854. Same as P-0582 and 0583. P-0585 Taber vert. aub. cent pump. Serial 33069, Dwg. A387, Type C-3, fig. 1940, 2" Inlet and outlet. Cl body, renewable, bronze bear:'lngs, bronze lmpellor mounted on nickel steel shaft, Length 11'6", sump cover plate, cap. 50 gal. p.m., 6$ static head, sp. gr. 1.18 at temp. 165 *-170 *F. D^:'lven by M-O856 In CT-0748, Diphenl store tank. Order B1' +518 on 4/16/36, Req. 69162. Chg. out $257.62. P-0592 Taber vert. sub. oen$ pump. Serial 33113, type C-3, Pig. 1940, 2" Inlet $nd outlet. All Iron construction on nickel steel shaft length 11'6". Cap. 50 g.p.m., 601 statlo head, sp gr. 1.368 at 70* to 90*P. In CT-0749P driven by Mi-f0873. Order B7516 on 4/16/36. Req. 69160, ohg. out $255.41. * general service ana diphenyl tank P-0593 Taber vert. sub. cen' ;. pump. Serial 33111. Type L-2, fig. 1940, Si" inlet and 2" outlet, casing, yoke, lmpellor made of stei1 shaft nlokel steel, column supporting Intermediate bearing, wrought iron. Length 7'9". HONS 046441 XII. ItQUIPMENT LIST, oontd. XII - 72 Equipment List P-0593 - 0629 Pumps, oontd. P-0595 contd. Cap. 75 OPM, static hisciAi 15', sp. gr. 1.8 at temp. 700*P. Driven by M-0871. On Number 1 still. Order B7515 on 4/16/56), Req. 69159. Ohg. out $382.91. In still S-045. Same jas P-0574. Sung) plate. Drawing A-495. P-0594 Spare motor same as P-p595. Serial 35112. Driven by M-0872. P-0595 Oberdorfer gear pump, Serial 2835. #7AXZ unloader pump, all bronze gear type, 10-15 OPM at 20# pressure. Used to circulate Aroclor on No. 1 still cooling system. Order B13188 on 7/2/56 Req. 71152. Cost $78.80. P-0604 P-0615 Vert. sub. cent. pump Taber. Serial 33207, Size L-QB, l|" Inlet and 1" outlet. All Iron const., open lmpellor on nickel steel shaft. Same as P-0573-4 and 5. In CT-0754. Order B13195 on 7/2/36, Req. 71148 on 7/1/36. On #3 scrubber, CT-0761. .Blackmer Pump Serial 4201747 Size 502, 50 gallon pef:r min. right hand rotary gear pump. B: ze with bronze liner and monel shaft. Steam J ticketed heads. Order B20818 on 10/16i,/36. Req. 73912 on 10/16/36 Ohg. out $148.27 on 1 ]|/30 Direct to 3 HP 1800 M. 01449. On filter press P-0159 P-0617 Blaokmer pump. Serial 201902. Size 100L, all Iron, Jacketed right hand pUmp, base plate for motor, and flex. coupling, direct oonm4cted (M-0914). Order B21241 on 10/22/36, Req. 74034 Chg. out $145.20. Spare pump. P-0629 Taber horlz. cent, pivute. Serial 33708. Type L-2, 2$" Inlet and 2" outlet, Size 103. Order B2833 on 2/9/37. Req. 76766 on 2/5/37. Chg. out $152.52. Direot to M-0975. On No. 1 chlorlnator. MONS 046442 XII. EQUIPMENT LIST, contd. Pumps, contd. XII- 73 Equipment List P-0674 - 0984 P-0674 On #1A scrubber, CT-0}013, driven by motor M-0848 on No. 1 chlorlnator. P-0731 Taber sub. cent, pump Serial 84722, Size L-QB, l" Inlet and 1" outlet, Order B3854 on 3/4/38, Req. 86891 on 3/3/38. Chg. out <174.25. In CT-01013. P-0907 Taber horlz. cent, puiyp Serial 56622. Size 103, type L-2, 2i" Inlet and 2" outlet connections, semi-steel through out with mone} shaft and water Jaoketed stuffing boxes, with bed plate ready to receive motor, 20' static head, rate 80 0PM, 1.! sp. gr. at 500*P. Order B12801 on 6/5/44 , Req. 10230 on 6/5/40. Chg. out $155.28, driyi'en by M-OI656 to circulate liquor for chlorlnator CT-01:<83, #4 chlorlnator. P-0909 Taber sub. pump. Ser^ial 36676. Size L-OB with If Inlet and 1" outlet, $11 Iron const., open Impeller on nickel steel shaft Order B13110 on 6/10/40. Req. 10366 on 6/10/40. Chi out $193.75. On CT-0968 sorubber llq. tank. Also on CT1-0760. P-0929 Taber sub. pump. Ser:$al 36853. Size C-3, fig. 1940, vertical 2j" inlet aniji 2" outlet. Bronze except shaft to be monel met.il , lg. of col. pipe 11'6". Order B18442 on 8/23/40. Ri q. 12559 on 8/23/40. Chg. out $404.59* On stg. tanlf CT-01310. Driven by M-01706. P-0932 Roper oast Iron pump RIBI #169. Size 1" rotary, geared, complete with base, g<liars, pinion, big stand and adapter plate for motor mountlng. P-0984 Roper pump. All Iron series "0" rotary pump for $0PM. 1.6 sp. gr. 50' head }ump, spiral gears pkgd. stuffing box with non-graphltlc white asbestos pkg. built In by-pass and complete with basy , drive gears. Order B4ll8 on 2/17/4: , Req. 18322 on 2/17/41. POr filter In CR. On Sparkler f: Iter P-0172. Replaced by P-0571. MQNS 046443 XIX. EQUIPMENT LIST, oontd. XII - 74 Equipment List P-0997 - 01258 Pumps, oontd. P-0997 Taber vert. sub. pump l Serial 37682. Type CL4, 2j" Inlet and 2" discharge for 75 0PM against 251 head. Pump of dynamo steel with wrought Iron pipe column and nickel steel shaft, water copied, stuffing box. Order B6379 on 3/13/41. Req. 19214 on 3/13/41. Chg. out $446.53, In S-062. Driven by M-OI856. Shaft has two Intermediate C.I. bearings. P-01037 Blaokmer pump. SerlaJ. 246058. 5W03202 bronze, size 51L with base and relief Iralve. Still receiver to blender. Order B16097 on 7/21,Al Req. 22429 on 7/21/41. Chg. out $177.56. On gr. fl. NE of P-0172. P-01054 Pump made by Well Sbrlal 13132. 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-01056 Taber horlz. cent, piujnp. Serial 38318. Type L-2, size 103, 2i" Inlet 2" ou'tsLet oomplete with base. Order B19730 on 9/3/41, retq^ . 24125 on 9/2/41. Chg. out $157.44 on 4/31/44. On #4 chlorlnator CT-01283. P-Ollll Blaokmer Pump Serial (249113. #5 OL all Iron steam Jacketed pump with C] base plate and gear drive ready to receive our 3 HP l80< RPM motor size 511. Order B16349 on 7/23/41, Req. 22597 Chg.out $105.05. Driven by M-O2877. For dlscha:iking rail tanks. P-01258 Blaokmer pump. Serial 269500, Size 1202-50. Pig. 3203 oomplete with relief valve. No base. #2 still receiver to blending tanks. Order B29303 on 1/28/43. Req. 40312 on 12/30/42. Chg. out $134.63. Bronze. MQNS 046444 T XII EQUIPMENT LIST, contd. XII - 75 Equipment List P-01277 - 02251 Pumps, oontd. P-01277 Taber vert. sub. cent pump. Serial 40890. Type CL-4, 2$" Inlet, 2" outlet size 584. Pump to be dynamo steel with wrought 1 ton pipe, column cap. of pump 75 OPM at 25' head for lquld 1.8 sp. gr. Order B8875 on 7/12/V5, Req. 45713 on 4/16/45. Chg. out $454.00 on 2/27/45. At S-062 Spare. Sams as P-0997. #2 still pump (spare P-01509 2" Taber pump. 60 0?lM. 150 ft. TDH. Shaft. Flexible coutj iling. M-05014. S. 0. 1.5 500*F. Steel with monel P-01540 0. E. Filter pump - I. W. comer of lean-to. Taber pump 504 stainless steel. 2" suction, lj" discharge. Located Indoors. Pumps from ld Pyranol blender CT-01521 to filter presses. P-01757 On Sweetland filter F-0259. Now used on F-0258. 504 stainless steel 2", J.00 gpm. Motor M-05718. P-02052 2" Taber. Semi-steel, monel shaft, water Jacketed stuffing box. 1.5 Si 0.,500*F. P-02077 P-02078 Blaokmer pump, from 7TCB store to blenders. Bronze lined, with monel shaft. N.W. of Bldg. CR. Taber 3" x 2$" 150 g>m. 80 ft. head. Horizontal impeller. P-02179 Taber Pump from new >lender CT-02621 to filters. Motor M-04025. P-02251 Viking pump on Arodpr mixers. M-0514. Pyranol plant. MONS 046A45 XII. EQIPMENT LIST, oontd. XII - 76 Equipment List Pumps, oontd. Note; London Engineering Deb>t. Final Report on the start-up of the Newport Aroclor pp..iant states that Hamworthy pumps were not found satisfactory In use. Oood Jacketing Is needed. There was trouble front corrosion of core plugs in some pumps, leading to leakage of steam Into the goods. Steel end covers were used later. The same reports dlsckiss the difficulties encountered with the still pump, which was looated In a small secondary vessel, below the vaoptiurn still. HUNS 046446 XII. EQUIPMENT LIST, contd. XII - 77 Equipment List R-026 - 027 Retortg R-026 Aroolor 1269 Retortas (embled and erected by Monsanto. Pots from Mooter. Jaoket from Oraver. 516.00 for 4. Req. B699O6. Burners from Surface Qombustlon. Req. 69374. Burners - gas fired. Jacket, steel, flrebrl,ck lined, holding 3'0" 0D x 3'8" lg. over dished bottom still pot with cover. Equipped with 2 gas burners anq stack, still pot 1/2" fire box steel,removable so reidue 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. Oeneral arrangement of solid Aroclor plant. Oas heater for discharge line. Platform for retorts. Mr. Soffranko In 1947 commented that the retorts would be better with thicker bc> ttoms than shown In drawing B-646, and that spare retort1 should be held. MQNS 046447 XII. EQUIPMENT LIST, eontd. XII - 78 Equipment List S-043 stnia 8-043 No. 1 Vacuum still pi P'ohased from Graver. Plant A Drawing C-809. Size p1 dla. x 516" long on straight side, 1/2" shell, dls^ved head 5/8" supporting brackets 60# Hydro press test Order B-7705 on 4/17/pi6, Req. 69225, Chg. out $336.00 on 2nd floor, 12 level. S-043, No. 1 still, at the Krummrlch plant, Is of the shallower type, like the Anniston stills, and like them It has a vertical vappur pipe (with Hagan separator Inside the still), leading tp the top of a vertical condenser, CT-0770, whereas No. 2 still is of the deeper type, and has a cyclone, CT-0l4|l3 In place of the vertlaal vapour 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. Hr.Furzey, December LI, 1951 reported that the cyclone gave better coloured pistillate than did the Hagan separator. Anniston, January 1950, reported satisfactory performance of their kagan separators Newport have the Internal Hagan separator. In a report dated Marc!ih 31, 1952. Mr. Dalton of the Krunmrlch plant mentlpns a modification to the Hagan separator at the Kruminr:ioh plant. The Aroclor colour was better after the phange, but It was not certain that the alteration really! caused the Improvement. There Is no attempt at fractionation, and the condensing systems were planned bo give the lowest pressure drop attainable, consistent with removal of coloured entrainment particles. The deepef* pattern of still S-062 was ohosen to give more disengage;ment space for vapour, but It does not appear to hive glhiren any better coloured distillate, and It has the dlsadvpntage of requiring a longer shaft etc. for the submerge^ pump. The condenser on No. 1 still delivers to reoelver ICT-0771 MONS 046448 XIX. BCUIfMENT LIST, contd. XII * 79 Equipment List S-043 StlllB, oontd. S-043 oontd. No. 2 still has heat ekohanger CT-01491, head tank CT-01398 with gravity flow (of cooling water only) to oondenser CT-01378. CT-01398 hap an internal ooll (not used) and there Is no temperature control Instrument . The distillate goes to reoelver 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 stlII was provided with a subsidiary vessel, located at a : wer level than the main vessel, and containing the sul lerged pump. With this arrangement, It was hoped to dimlnlblh the liability of cavitation of the pump, and to permit the use of a much shorter shaft for the pump lmpellor. The arrangement, howevbi:r, was unsatisfactory, largely because the pump gland was exposed to hot liquid Aroclor (See the London Engines ring Dept. Final Report on the start-up of the Newport plant). Numerous different gliand packings were tried, the gland was given a lantern rl|fig, fed with liquid Aroolor etc. etc., but finally a 1ohg vertical steam Jacketed pipe was fitted on top of the oondary vessel, to oarry the . stuffing box above the| level of the oharge in the main still. This looatlon ^lso put the driving motor Into oooler surroundings, ahid 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 manlld on the still cover, on b wide pipe down the centre of which the pump shaft runs, The delivery pipe from the pump runs Independently up through the same manlld On the cover of the stjl 11 (welded through). Differential expansion may distort Ithe alignment of the parts, and may MONS 046449 XII. EQUIPMENT LIST, oontd. XII - 80 Equipment List Stills, oontd. $-043 oontd. displace the Impeller axially within Its casing. Another trouble which appeare4 was that air leaking In through the gland oould travel do>i en the central pipe around the shaft and oause cavltatl^i>n In the pump. The remedy for this Is to have holes In tiki pipe,oommunleating with the main vapour space In the vi$ssel. The stuffing box is w4i ter cooledj the bearings Inside the still may give triiluble, this clearance must be Just right. Carbon bushing have shown some promise. It has to be remembered that the charge oontalns a fair amount of solid (lime) etc. hloh might lodge to some extent In Jthe still instead of lowing to the secondary vessel. The Internal bearings are lubricated by Aroclor bled off the pump delivery lin4 but they may become choked by the solid matter In the clbarge. See also the descrlpt^ on of the Anniston still and pump on pages 20Section VI,.above, and oomments on the distillation prooess. pages 4-, Seotlon VII. From the bottom of thq oondenser at the Krummrloh plant, the distillate passes through a Jacketed line to a Jacketed sight glass With sampling fitting, and so to one of the receivers 0T-0771 or CT-01377. There Is a ring of gas burners a;round each condenser exit, to deal with the heavier Aroc lors, but the burners are not much used. Condenser CT-0770 can be cooled by Aroclor circulated by pump P-0595 through th|ie condenser shell space then through heat exchanger, CT-0831 (cooled with well water) and through a sight glass to head tank CT-0766, and so back to the pump. This syiStem Is alternative to the ooollng by- distilled water us<id on this condenser, but It has gone out of use since the Krummrlch plant gave up the production of the hlgliier Aroclors. HONS 046450 XII. EQUIPMENT LIST, contd. XII - 81 Equipment List Stills, contd. 8-043 contd. There Is a steam and ter coll In the head tank to keep the Aroolor at around! 110-120*C. There Is a Taylor Tullscope temperature ontroller 1-0510 controlling a tvalve on the steam lnll t to the coll. This Aroolor cooling is more convenient foil higher Aroolors, but the water system Is preferred f'or the lower Aroolors. The system normally wok*]ks at about atmospheric pressure though the vent (on the top of heat exchanger CT-0831 Is usually kept dosed, apd there Is a pop valve at the same point). The sketoh on page XII - 82 will serve to show the arrangement and to Indicate oprtaln minor features not described above. Each still has a bottok outlet which will completely entity the still, also an outkiet at about the same level of the top of the bottom dlsh[ whloh will leave about 80 U.S. gallons of bottoms in the still. Both deliver to open topped cans on small w|heeled "dollies" under a hood ventilated by suotlon fan B-0148. Rising stem gate valves are used on thep e outlets and gas flames are freely used to heat them for tame 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 skle wall, about 7*6" bfr:low the cover, but this well was not In use May 1955. Eaoh| still body has a BS & B relief disc of AlPb, 8" diameter, Vacuum supported, calibrated to rupture at 25 pslg. Thei receivers do not have relief discs. MOMS 046451 XII. EQUIPMENT LIST, contd. XII - 82a Equipment List S-043 3-043, oontd. Drawings, B 483 A 493 Water-cooled condenser on No. 1 still] /CT-0831 -01397 -01491 Sump plate Tor submerged pump I ( S-043 B 644 Head tank for cooling medium CT-01398 B 651 B 662 Tubular condenser Vapour exit pipe (0I::007137708 S-042 C 795 C-807 Receiver ----------- .................................................. CT-0771 Ooke tower --------- ------------------------------------------ CT-0753 C 809 No. 1 Still -- ............................ -........... -- S-042 C 815 Piping of vacuum still - FC-045,CT-0770,-01377 C 864 like B 483, on n6. 2 still ..................... S-062 C 6942 Piping diagram, No. 2 still ................... S-062 C 6943 Piping diagram,Jlo. 2 still ------------------------- S-062 D 6944 No. 2 still --..................................-........... - S-062 E 6952 D 6956 General layoutNfe. 2 still ------------------------- S-062 j General layout, tlo. 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-01378 MONS 046453 XII. EQUIPMENT LIST, contd. XII - 82b Equipment List S-062 -0459 Btllls, contd. S-062 #2 Vacuum still purclhased from Nooter. Serial #52. Dwg. D-6944, 6' ID x 11 10" str. shell. Internal pipes, etc. Std. dished heads, Olaas wool insulation 3" with 1/2" finish coat. Order B10730 on 5/12/4U. , Req. 20421 on 4/28/41. Chg. out $950.00. Sx$Bi]pended between 20'6" and 12' platform in CR. S-0459 Is another number for C-0808, gas fired chlorinator. HONS 046454 XII. EQUIPMENT LIST, contd. XII - 6!i Equipment List SC-091* - 02a6 scales SC-094 Howe Portable Scale #822, Serial 1563205, all Iron platform 30$ " x 50$" Cap. 1500 lb. Order B9986 on 5/20/3*6, Req. 69955, Pyranol Plant. SC-098 Howe scale. Serial 1364566. #1420 Skeleton type, Dali bearing, dormant seale, cap. 2500# with double beams. Platform 46 x 58. All metal lncl. steel shaft. Order B14351 on 7/20/36. peq. 71536 on 7/17/36. Price $213.85. SC-0100 Scale purchased from The Exact Height Scale Company. Serial 39992. Styld 1226, cap. 200# on ratio of 10 to 1. Dial with indicapor travel 12$" under wgt, and 2$" over wgt. Fitted with bag holder for 100 to 200# bags. All on swinging rack. Order B17906 on 9/9/pi>6. Req. 72843. Chg. out $289.41. In lean-to near V-0 and V-045. SC-0246 1000 lbs. capacity, Pyranol Plant. MONS 046455 XII. BCUIPMKNT LIST, oontd. XII- 84 Equipment List T-014 Transformer T-014 Transformer made by pfestlnghouse. Serial 530335. 200 KVA, type SK, n< used 440 volt primary 110/220 volt seoondary. On the ljeater of the Leotrodryer PC-046. Cost $10.00. Outsldtj SK comer Bldg. CR. Also used formerly for strip heaters In the still receivers, etc. MUNS 046456 XII. EQUIPMENT LIST, contd. XII * 85 Equipment List TW-0166 - 0312 Towers TW-0166 Fused Silica Tower purchased from Amercel Co. Inc. 1 "U" bend trap, 1$ absorbers seotlone B/P 0111 8" ID x 6'6" C to center. Order B8l6l, Req. 69399. Same as TW-OI65. Regarded ks obsolete design. TW-0182 Scrubbing HC1 tower| made by Haveg. Drawing C-4705. "41" std. 2'6" dla 10'2" deep, 5/8" thick walls x 3/4" thick bottom, machlhtied dished head, and connecting material, 2" thick Haveg dril/ed plate with neoessary supports 4-3", 1-8" and 1-10" std. Haveg nipple type outlets with figs. Order B20284 on 10>, /|>/37 Req. 83234 on 10/5/37. Chg. out $668.56 on| 12/31/37. On 38' level steel Struct, south side of CR. TW-0206 Scrubbing Tower put based from Nooter. Drawing B-5815 support, drawing C-l|>8l4 tower. 17-18" ID x 8' wAlded steel oonst..tower, weldep steel scrubber support for tower. Order B7346 on 3/2'7/40 Req. 8063 on 3/27/40. Chg. out $277.00 onl 4/30/40. Above CT-O756, scrublber by pump tank. TW-0221 HC1 absorption towi 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. Oas line of Haveg. Cap, to produoe 205* Baume HC1 at 4620# per h:icjur. Order B4625 on 2/33/''41. Req. 18520 on 2/21/41. Chg. out $5321.13 dh 8/21/41. On steel struct. S of CR. Schwartlng and oth<(i]rs "Process Description -- For Aroolors", November 12, 1953, state that the Fansteel off-gas absorbers are oonstnkcted of Hav?g 60, and have Tantalum heat exchange surfe|ices. TW-0312 Absorption tower. Fansteel AL-300. Haveg 60 parts, Tantalum tubes, (si tantalum parts salvaged from an older unit. ) MONS 046457 XII. DRAWING LIST XII - 86 Drawing List Note i Some of the earlier drawings t^ere made at the JFQ plant, and the later ones at the Krummrlch 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 JFQ plant, [whereas those marked "B" are from the Krummrlch plant. In column 3, on the following [pages, the letter "L" indicates that prints of drawings were sent to Mr. Cooper, London, by mlr mall, April 24, 1947. "8" Indicates that prlntt| of drawings were sent to Mr. Cooper, London, by isurface mall, 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 dilawlngs were found July 28, 1950, and that prints were sent to Mr. Buis, London. MONS 046458 XII. EQUIPMENT U3T, eontd. XII - 86 a Equipment List V-044 - 046 Conveyors V-044 V-045 V-046 Screw conveyor made by Essmueller MP'Co .'o. Drawing C-8l6. Size 6", 6'8i" trough length with outlet at each end. Cover of galvanized lA>on. Cl trough ends with zinc and tin sprayed. Req. 69^109. On bottom CT-0764 - North Conveyor. Prom stg. Ijln to bagging scale and back to bobt of elevator, driVi>en by M-0835. Layout - E-877. Flow Sheet - B-640 Screw conveyor made by Essmueller MP Co. Drwg. C-616. Size 6", 6'8-i" 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-0765 south conveyor. Prom storage bln to baggln) scale and baok to boot of elevator, driven by M-0836. Screw conveyor made' by Essmueller MP Co. Drawing C-816. Same as V-044 and 04sj Prom flaker discharge to elevator boot. Driven by chain on M-0827. All these were part of the equipment for Solid Aroclors dismantled In 1952 MQNS 046459 XII. DRAWING LIST XII - 87 Drawing List Drawing Humber A-324 A LS Title Equipment Number Oas-heated chlorination pot(see E-888) CT-O808 E-346 M Muriatic t: |*eatment vessel CT-0861 F-352 H Fractlonat: ,ng column (not Aroclor plant) F-370 A L S General La; rout Layout F-373 F-374 F-375 F-376 P-380 A L S Ducts for ; irocess fumes,solid Aroclors D-012 eta A L S Layout, so .Id Aroclors Layout N Structural steel N Steel and `oundatlon N Electrical layout P-381 N Electrical conduits F-382 N Lighting F-383 F-384 N Service 11 les N Foundation details F-385 N Structural steel, Hurlatlc tower F-386 A L S Piping lay >ut Piping F-389 N Electrical details F-391* A-459 N Gen. arrt. HC1 absorption A L S Bearing fo r blender shaft CT-0779 Sea note on page 86 in this section. MONS 046460 XII. DRAWING LIST, contd. XII - 88 Drawing List {Drawing Number B-483 A-493 A-501 C-502B D-512 D-518 C-605 D-609 B-613 B-640 B-643 B-644 B-645 B-646 B-651 Title Equipment Number L S Water-ooolefl condenBer for vao.still CT-0831 [ CT-01307 t S Sump plate for submerged pump in vac. f CT-01491 still S-043 N Lead-lined tray for HC1 absorber I M Sand filter for muriatic acid L S Storage hopper for solid Aroclor L S Chute for Aroclor flake ,CT-0764n \CT-076y D-012 L S Shear pin cp drive of gas-heated chlorinator M Store tanks CT-0808 CT-0748 CT-0749 CT-0768 CT-0769 CT-01310 L S Relief door gas-fired ohlorinator furnace h a Plow sheet N Separator, not installed CT-0808 Plow sheet L S Cooler on ^ac. still system CT-0766 CT-01398 L S Cyclone on solid Aroclor plant CT-0751 L S Still pots for solid Aroclor L S Heat exchanger on vacuum still R-026 R-027 CT-0770 CT-01378 * * See note on page 86 in this section HONS 0A6A61 XII. DRAWINO LIST, oontd XII - 89 Drawing List Drawing - Number * Title Equipment Number B-653 B-654 A L S Stack for lolld Aroclor plant A L S Support fo r stack CT-0751 CT-0751 B-658 N Ploor grat Lngs B-659 B-660 A L S Chlorine 1 ilet A L S Cyclone - lot Identified CT-0745 CT-0833 B-661 A L S Elevator d rive, solid Aroclors L-031 B-662 A L S Vacuum etl LI vapour pipe S-042 B-663 A N Supports f sr vent line scrubber CT-0762 B-664 A N Vao. still furnace vent pipe 3-042 B-666 A L S Thermoooup Le wells B-675 B-684 B-685 B-686 B-689 c-795 A L S Hood, etc. of flaker A obeol- Strip heat :r clamp for chlorlnator ete A obeol- Heater for Sperry press ete A N Vent stack N Vent staol A L S Vaouum stl LI receiver 0-798 A L S CaCla brea ther D-102 CT-O808 P-0172 PC-045 PC-045 CT-0771 CT-01377 CT-0762 C-799 0-800 A L S Diphenyl h ead tank A L S Scrubber 1 iquor tank ttfe * See note on page/ln this seotlon. CT-0767 CT-0754 CT-0755 CT-0756 HONS 046462 XII. DRAWING LIST , contd. XII - 90 Drawing List Drawing Number Title Equipment Number C-804 0-807 A N Hot water :ollectlon tank A L S Coke scrub >er C-809 A L S 1 vacuum jtm CT-0752 CT-0753 CT-01396 S-043 C-810 A L S Halt tank ["or high boilers etc. CT-0763 C-815 A L S Piping of iracuum still FC-045 CT-0770 CT-01378 C-816 A L S Aroclor co iveyor V-044 C-818 .C-821 A L S Chlorine v ipourlzer N Platform f >r still pots C-822 A L S Chlorlnato ? relief connection CT-0743 R-026, R-027 CT-0744 C-823 A L S Muriatic a >id store tankB CT-0784 CT-O785 CT-O786 CT-0795 C-827 0-829 A L S Weighing t uck, solid Aroclor plant N List of mo lors MSC-0681 C-83O F-838 A L S Oas-heater for discharge of gas-heated CT-0808 ohlorinator N 18" fraeti mating column, not In Aroclor plant 0-847 N Holder for strip heater CT-0771 # See note on page 86 1 . this section. MONS 046463 XII. DRAWING LIST, contd. XII - 91 Drawing List Drawing Number C-848 B-876 E-862 E-863 C-864 E-865 E-867 E-870 K-877 E-88O E-881 E-886 E-888 E-689 E-896 D-978 * Title Equipment Number N Holder fo ? strip heater N Ploor gra :lng CT-0771 L S #1 Blend1 lg tank and #1 Plltra ;e receiver CT-0779 CT-078O L S Buffer ta ik (air blowing tank) A M Heat exch inger for #2 vacuum still (se t drawing B-483) CT-0750 S-062 A L S Setting f >r stills for solid Aroclor R-026, R-027 A L S Setting f r flreheated chlorlnator N Conveyor for Aroclor flake CT-0808 L-031 L S Conveyor for Aroclor flake (layout) V-044 A L S Chlorinat 5r CT-0744 CT-0745 CT-0833 A L S Shell for gas-fired chlorlnator furnace CT-0808 L S Shell for above and brick setting S-043 P-045 L S Drive for gas-fired chlorlnator CT-0808 N HC1 absor ption tower N Ploor gra ting, HC1 tower B L S Diphenyl store tank CT-0347 See the note on page 86 In thjis section. HONS 046464 XII. DRAWING LIST, oontd. Drawing ft Number ft Tl t.T * C-1117 B N Foundation of D-978 D-2076 B L S Turbo aglti tor for blending tank D-2077 B L S Stator for above C-3479 B M Heating fu mace for coll of #2 vaouui (1 still C-3775 B L S Filter for HC1 gas D,425S, B L S Muriatic t ink D-4300 M Pansteel d `awing HC1 absorber B-4J66 B F N Varec. Oau ;e on Pyranol mixer B-4413 B L S T.C.B. Sto >e tanks D-4459 B L a Rubbwr-lln id treatment tank with agitator 0-4616 B L S Scrubber 1 .quor pump tank B-4679 N Obsolete, layout for HC1 absorber B-4689 N Obsolete, 'lplng of HC1 absorber 0-4705 B L S Haveg towel ' (obsolete) for HC1 abs. C-4845 B L S Scrubber 1. quor tank B-05711 M Goodrich n bber-llned tanks C-5743 B L S Scrubber li 1 Pyranol plant 0-5814 B L S Obsolete, IC1 tower XII - 92 Drawing List Bqulpment Number CT-0779 CT-0779 PC-066 F-0106 CT-01260 CT-01321 CT-0861 CT-0968 CT-01013 TW-0182 CT-0104 CT-01575 CT-01162 TW-0206 ft See the note on page 86 In this section. HONS 046465 I XII. DRAWING! LIST , contd. XII - 93 Drawing List Drawing Number B-5815 B-5821 C-5825 C-6144 E-6209 D-6455 B-6838 A-6853 B-6868 C-6863 E-6941 C-6942 C-6943 D-6944 D-6945 D-6946 E-6952 * BN P B LS B MP B LS B' LS B LS N N B LS N B LS B LS B LS MP B LS Title Obsolete, HCl tower support Cyclone Monel gas chamber on flreheated chlorination system Monel cone enser Chlorinate r Pyranol ml xer Assembly c f blending tank Agitator 1 n blending tank Thermocoup le wells Plltrate r ecelver Platform c f still Piping dla gram for #2 vac. still Monel plpl ng diagram for #2 vac.still #2 Vao. St 111 Exhaust Sy stem,mentioned on p.XII-6. Control rc Dm General Is rout #2 Still Equipment Number CT-01259 CT-01279 CT-01280 CT-01282 CT-01258 CT-01263 CT-0744 CT-01283 CT-01321 CT-0779 CT-01399 CT-01399 CT-01400 S-062 S-062 3-062 3-062 S-062 See the note on pa ;e 86 in this section. MQNS 046466 XXI. DRAWING LIST, cont.d. Drawing ft List ft Title D-6956 B L S General la; rout #2 still C-6957 B L S Cyclone on #2 vac. still B-7082 B L S Monel cond inser #2 vac. still B-7121 N Support fo Sperry press A-7136 N Pipe coil 1 inder Sperry press A-8855 M Bearing fo blending tank (See drg, A *59) D-10292 B L S Piping of tlr blowing tank Hand B L S Dryer for ittapulgus Earth sketch (See correi ip. file Mar. 25/47) XII - 9* Drawing List Equipment Number S-062 S-062 S-062 P-0113 P-0113 Annlaton DrawlngB Layout of ehlorlnators) to MCL, June 7, 1946 #2 Aroolor still Detail of thlorlnator") ,,,, ,, (Swan Chemical Co.) ) to ,,, 12' ^7 * * See the note on page 86 of this section. HONS 046467 XIV. HISTORY OF THE PROCESS N MONSANTO. XIV - 1 History of the Process In the years 1927 - 1928, the Swann Chemical Company developed a prooeco for making diphenyl but as the expected demand for It did not continue, other outle^s were sought for the diphenyl, Aroolors were produoed in the laboratory In 1929, and as they showed good electrical proper^les, fire resistance, and general Inertness, the Qeneral Electrlc Company became Interested, and developed the use of Aroclors In transformers and capacltators. A plant was Installed to produce 3000 lbs./day at Anniston. In 1935 Monsanto acquired the Swann Company, so gaining access to their Aroolor patents. As thi demand for AroclorB Increased, additional production equipment was Installed, looated at the Monsanto Illinois factory (th|im plant "B" and now called the Krumnrloh plant). This equlpiilent came on stream In September 1936. The Krummrlch plant site was those partly beoause of the availa- blllty of chlorine there, but when chlorine consumption overtook the production, and chlorine to be purchased, proximity to the rdiphenyl production at Annlst oapaclty, largely designed on had more weight, and additional the plant "B" model, was Installed at Anniston In 1941. By 1946 both plants had doublyId their capacity, to give a t'dtal production oapaclty approaohli 2 million pounds a month. About 1954 chlorine cells were InstAlied at Anniston. The Newport plant was designed mainly on Krummrlch plant information, but to a less extent oii Anniston Information, under Newport Projeot No. 12 of the London (jentral Engineering Department. Chlorination started at Newpo:*t In June 1951, Mr. Clegom from Anniston spending some time at Newport to assist in starting the diphenyl and Aroolor plants tlhere. The first production of Pyrani by MCC was In 1936, when Pyranol i486 was made for the General Electric Company, the blending being done at first in rail tanks. Pyranol 1493 was made In July 1938. The use of tln-tetraphenyl st^:rted In 1944, since when the main production has been of 1467 ( TCB - 1260 mixture plus tln-tetraphenyl). MQNS 046468 XV. OPBRATINQ INSTRUCTIONS. XV - 1 Operating Instructions Operating Instructions were giV('en In the report of lories, Soffranko and Becker, November 1947, pag4 s 84 - and a revised version was put out by the Krummrloh Plant Stapidards Department, August 10, 1954, (copy sent to Newport, Nay 23, 1955). Points oalling for special mention arei -- 1. Care In melting diphenyl Received In care. The first move Is to melt a hole, from the surface, down to the bottom of the tank to prevent developmeiAt of pressure from the heat of the tank ooll or Jaoket. 2. Usual rail track routine f.n handling cars. 3. Exclusion of rain etc. 4. Proper use of tracing on Alps 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. Plre precautions In handliing diphenyl, toluene, and butyl acetate and mixtures containing tpiem. .8 Chlorlnator charges kept as cool as possible, and not olrou- lated In the early stage pf chlorination. 9. Watoh Inlet pressure on c ilorlne line to chlorlnator. .10 Care in emptying chlorlna ;ors not to suck back the scrubber charge. 11. Keep chlorlnator charge out of the chlorine feed line 12. Watch gravity and temperat;ure of scrubber for indication of poor absorption of chlorinie In the chlorlnators. MONS 046469 XV. OPBRATINO INSTRUCTIONS, cohtd 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. Ouard against burning or poking the still colls, .16 The usual care In lighting gas fumaoes. 17- Cara In dealing with hot material tapped from the stills, 18, Cleanliness In handling fiinlshed Aroclors. 19. With higher Aroclors take special oare against blockage of lines. .20 Safety precautions as die bussed under "Hazards", Section XI, above. Pyranols Operating Instructions relating specifically to the Krummrlch plant are given on pages 33- of the rsport "Dept. A-246 Pyranol Process", Lyles, Soffranko and Hiller, Mafch 24, 1947, <4opy. 08 sent to MCL October 15, 1947). Points mentioned are: 1. Checking the moisture confcent of Incoming cars of trlchlorobenzene. Air blowing at kbout 50*C. to remove excess moisture. Sampling of materials at various stages for submission to Qeneral Electric Company. 3. Exclusion of moisture, HCL fume and dirt. 4. As a working rule. In adj|nsting blends of TCB with Aroolor 1260, 1 part of 1260 added to 8b parts of the blend will raise the Sp. Or. about 0.001 and the refractive Index about 0.0001,' MQNS 046470 XV. OPKRATINO INSTRUCTIONS. oon|;d. XV - 3 Operating Instructions Pyranols, eontd. 5. Blands containing tln-tetraphienyl are to be warm (about 80*C.) whan filtered, otherwise some TTP may come out of solution. 6. Waterproof cloth over the dioties of the filtered rail tanks to exclude moisture and dirt wtyle travelling. 7. Avoidance of delay In dealing with samples because of the numerous testing stages required. MQNS 04bA71 ACKNOWLEDGMENT To Mr. J. Soffranko who was In charge of the Krummrloh plant Aroclor Dep;. 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 a!fesembllng Information for the Newport project, alAo the companion report "Dept. A-246, Pyranof. Process" Lyles, S6ffranko and Miller, March 24, 1947. The reports by Schwartlng and others, 1953 and 1954, havfe been used In the present revision of the prooess details. ! Acknowledgment Is due also to other Krummrlch 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. MQNS 046472 Index Page 1 IS {El ACETONE, solubility test on aroclors discussed -VII-11 Aold number, conversion of KOH figure Into NaOH figure -- IX-63 KOH v. NaOH values............ -.......................................IX-40 Aold number, test methods-------- .................................... IX-62-, IX-128 Acknowledgment -------------------------- -------- -------------------------- Section XVI Agricultural uses of Aroclors ...................................................... VII-21 Alr-blowlng of chlorination product ----------------------------------- VI-13- comments on ------------vil-4 Air blowing tanks, etc. .....................-................... XII-17a Air, dry air needed In unloading Air diyer ..................................................VI-35 --.............. -....................... XII-45 Analytical Methods, see "Specifications & Test Methods" and --- ------------- "Control Tests" Anthraquinone derivatives, as tablllsers in Aroclors ----- VII-9 report mentioned VII-34 determination of-----------------------VII-9 APHA --........................................ -------------------------- see "Colour" Appearance ---------------------------- -------------------------- see "Colour" Applications of Products - i-------- VII-18-, VII-30, XI-5 liters'ture survey mentioned -- VII-32 Aroclors, advantages of ---------as animal repellents are complex mixtures ............-................................ VII-19 .................................................XI-5 -............................... -................ II-2 blending of to give Intermediate Aroclor---------- VII-11 butyl aoetate blends see "Butyl Acetate" causes of high chlorine content- --------------------- VII-15changing production from one grade to another - VI-13 --..................-- VI-25 colour troubles ............................................. VII-10- crystallization troutN, les--------------------------VII-11-, VII-2 damaged by heating lr| Iron............ .............................. VII-7 effect of metals on J-------- VI-34, VXI-1, VII-7, HI-1 Isomer ratios v. chlorination conditions ---------- VII-3 need for tin etc. lining In store vessels ---- VI-35 physical and chemical properties ------------------------ III-7 (solid) crystallization point method ----------------- IX-87 4solid, distillation -------------------------------------------- VI-24- solld, manufacture discontinued ------------------------------ V-2 solid, process detallp -------------------------------------------VI-7 solid, specifications! ------ IX-16,--IX-30 specifications for IX-11-, IX-26- MONS O'*6'*73 T Index Page 2 Aroolor, toluene blende ............................................. VII-7 test method ............. -........................... IX-88- unstable Impurities in ............................. II-l, Vll-16 viscosity index Is high ............................................. VII-19 see also finished products Askarels -------------- ---------------------------------------------------------------j_4 bulletin ........................................... VII -30 Attapulgus earth. alternative aaterlals unsatisfactory -- VII-7 dosage of ------------------------ VI-27 dryer ----i---------drying of -4--------- removes T.T.P. -- sample sent to MCL ---------- XII-40- VI-27, VII-7 ............... VII-7 ----------------1X-9 specification ----- .................... IX-3 BATCH RECORDS------------------------------ +--------------- see "Operating Records" Bensene, sample sent to MCL --+--------------------------------------------------- IX-9 Biphenyl----------------- ------------ -------1--------------------------- - see "Diphenyl" Blending, of Aroclors with butyl acetate IX-40 of Aroclors with toluene VI-29- of different Aroolor^, 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 Bolling point range-- -------------- see "Distilling range" Buildings ------ see "Plant layout" Bulletins on application of products ------ see "Applications" Butyl acetate - Aroolor blends test methods ---------------- IX-175- Butyl acetate blends mentloned------------------------------------------------ IX-40 precautions In handling------- .....-- ix-40 colour of blends with Aroolors(test method)IX-178 quality of -.......... -................................ ........ IX-10 specification fof .................................................. IX-29 CAPACITY OP PLANT ...................... ...................................................... X-l- Carbon, no specification -- ...................................................... IX-3 Catalyst ----------------------------------- ------------- see "Iron turnings" Cereolors ----------------------------------- ---------------------------- IX-183 Changing from one Aroolor to aipother ........................ VI-13, VI-25- Chemloal reaetlons with Arocloifis -----------------------------------------VII-21 MQNS 046474 Index Page 3 Chemistry of the Process ----- ------------------------------------- Section II sele also "Comments on the Process" Chemistry of action of chloride scavengers ------------------------ IX-182 Chloride scavengers --------- --------------------------- see "Scavengers" Chlorides in tlntetraphenyl, tefiat method -------------------------- IX-133- Chloride test in boiler water .......................................................IX-107a Oeneral Electric ------------- see "General Electric" Chlorination, batch data----------- ..............................................................VI-5 chart of ft Cl* v lb. Cl* to finish---------------vi-4g chemistry of ----- ------------------------ -- II-2, vil-3 comments on ------ ....................................................... VII-1- continuous, disciMfl,sed............................................... VII -2 no circulation oil oharge at first-------------------- VI-6 process in detail] -............................... .......................VI-4- ' purging of gas li&,et line---------------------------------- VI-6a rate of ------- see "Chlorine flow rates" record charts ......................................... VI-37- unstable byeprodi1UCts mentioned --------- II-1, VII-16 Chlorlnator for solid Aroolors ...........................-...........XII-30- Chlorlnators ------------------------------ ------------------------ XII-7- eto. inlet fitting - --------------- VII-2 Chlorine consumption figures see "Production standards" determination, total o^lorlne.............-- IX-52-, IX-64 - General Electric met]hbid, see-----------"Oeneral Electric" distributors -------- -- ........................ XII-9, VII-2 flow rates ---------------- ...........-........................... VII-1 handling of-------------comment* ...................................... VI-2 ......................................... VII-2 metering eto. ------------[ ...................................... VI-3-, VI-6a- no specification ------ ..............................................................IX-3 quality, ocoments -- ----------------------------------------------------IX-8 use of snlft gas etc. -------------------- VI-2, VII-2 Chlorphenols in Aroolors -------- ...................................... VII-10 mentl ad --................................................IX-8 Cliff-Char ....................................... -------------------------- see "Carbon" Closed Tanks ---------- ----------------Cooks, oholoe of ---------------- ................................................ XII-7---------------------------- --------------- Xii-5 Coke scrubbers ---------- ------------- ----------------------- see "Scrubbers" Colour, see also ------------------- ------------- "Electrophotometer" test methods, Aroolor 1P71 (solid) ------------------------ IX-101 Aroolors 1270 and 1271 f.n toluene solution IX-100,-103a Aroolors ------------------- .................................... IX-57- HONS 046475 Index Page 4 Colour, diphenyl ----------------------- - IX-93 general (APHA)------------- IX-47- (Hazen)----------- IX-153 Pyranols--------- ------------- IX-57- Comments on the Prooess --------- -Sectlon VII Compatibility data(Aroclor) --l------------------------------------------------ III-16 Competitive products -------------------l---------------------------------------------- IX-183 Consumption figures---------------------[-----------------------------see "Cost data" ----------------- "Plow Sheets" -------------- "Yield figures" Control tests, in blending Pyranols ---------------------------- VI-32 Control tests ---------------------- -------------------- Section VIII Conversion factors --------- -- ------------------------------ IX-12b Conveyors ------------------------- ........ .................... - XII-86 a Corrosion test ---------- ----------- see "Oeneral Eleotrlo" Cost data ----------------------------- -- ----------------- see Section x Cost sheets ---------------------------- -------------------------------- X-27- Crystallization In Aroolors, see "Arfclors, crystallization trouble" Crystallizing point test method} Aroclor ------------------------------ IX-87 control test method-- VIII-1- dlphenyl---------------------------- IX-94 glyoldyl phenyl ether----- IX-161 trl-tetra chlorobenzene IX-167 Crystal structure, test method for Aroclor 1271---------------- IX-103a Cyolones, on ehlorinators - VI-9- on stills ----------- XII-78 DENSITY ........................................... see "Specific gravity" Design Reports ---------------------- .................................. VII-31 Dlbutyl diphenyl tin, as a scavSinger-----------------------VII-8, VII-22 Dleleotrlo oonstand and power faiCtor, test method---------IX-144- Dleleotrlo strength, test method IX-135- Diphenyl, comments on quality -- ix-8 Diphenyl handling --------------------- VI-1- Diphenyl measuring tank --------- XII-25 Diphenyl, phys. and chem. prope:tftles........ ........... -.................... Ill-l- sample sent to MCL - IX-9 specification ----------- IX-1 test method (oolour) Distillation -------------------------------- IX-93 -VI-14- comments on --------- VII-4- MONS 046476 Index Page 5 Distillation, of solid Aroolors ............................................. Vi-24 reoord charts -- ............................................. VI-40 semi-continuous - .......................... ................ VI-21- use of moderate vtcuum ------------------------------ - VI-23 Distilled high boilers see High bollerB, distilled Distilling Range, Test Method, rodors etc. -----------------------IX-74- lphenyl---------------------------------- IX-95 ;eneral------------------------------------ IX-41lyoidyl phenyl ether -- IX-162 rlchlorobenzene etc. -- IX-70 rl-tetra ohlorobensene IX-168- Distribution list see title page Drawing list ------- ............. XII-86- see also the drawings listed under many of the Items In t^e equipment list In Section XII Dryer ------------------------------------------- see "Air dryer" Dryer for Attapulgus earth - see Attapulgus earth Du Pont viscosity method (Parllik)]------------------------------------------IX-179 EARTH............... -.................................. Earth treatment of Aroolors see Attapulgus earth --------- see "Treatment" Effeot of metals on Aroolors- ---------- see "Aroolors" Ejectors ------------------------------------- ............... VI-23, XII-64 Eleotrloal grades of materials VII-7 Eleotrloal properties of Aroolors III-8, III-16, VII-32, VII-17 Electrical stability, test meth<d -------------------------------------------- IX-81 Eleotrloal test apparatus, dealing of- ...................... IX-154 Electrloal test methods ---------- VII-32-,IX-155 - eomment4 -r.................... IX-163 Eleotrloal uses for Aroolors -- VII-20, VII-21 Eleotrophotoraeter, operation of| --............... IX-106b- Elevators-------:----------------------------- ------------------- XII-49 Emergency measures ------------------Equipment List-------------------------- ..................... VI-57 --------- Section XII general note -' --...................... XII-1 Evaporation loss data (Aroolors) ........................ Ill-8 FENCHLOR ................................. Filters ----------------------------Filtration of Aroolors, after earth treatment ................... IX-183 ------------ XII-42- -- VI-27-, VI-33 HONS 046477 Index Page 6 Finished Products, oauses of de:fleets---------------------------------------- vil-9- chlorine conitents ---------------------------------------- ii-1 comments on quality-------------------------------------- VII-9listed -- ----------------------------------------- 1-8, j_4 phys. and ohem prop. ------------------------------ III-7- spec, and tea;|t methods---------------------- Section IX see -- ---------------------------------------- Aroolors ------------------ ----------- ------- Montars Plre Hazards ---------------------- ---------------------------------------- Pyranols ---------------------------------------------- XI-6 PIre point, test method ------- ------------------------------------------ IX-82- Flaker ---------------------------------------Flaking of solid Aroolors -*- -------------------------------------------- XII-40 -------------------------------------------- VI-2* Flash point, test method ------- -------------------------------------------- IX-82- Flow meter for chlorine, see- -----------------"Chlorine flow rates" -------------------- "Chlorine metering" Flow Sheets --------------- ------------------------------------- Seotlon IV Fume exhaust system ---------------- ------ see "Blowers" GASKETS -------------------------------------------- ............................................. XII-2- attached by TCB blends for drums ------------------------ ...........................................VII-17 ............................................. VI-34 to resist Aroolors ------ .......................................... VII-19 Oeneral Electrlo Test Methods, domments on ----------- VII-12-, IX-40 ............................. IX-180- (jorroslon test------------------------ IX-85 inorganic chlorides test -IX-77 Rampling-------------------- VI-32-, IX-40 Olyoldyl phenyl ether. chemical nature of ------------------------------- --1-4 chloride oontent of ---------------------- -- VII-8 determine,tlon of In Inerteens -- IX-165- hazards 4*> handling of ------------------ IX-161specifiedtlons.................................................. IX-5 test methiOds---------------------------------------- IX-161- HAZARDS ------------------ Seotlon XI see also -"Emergency measures" Hazen colour determination method -------------------------------------------- IX-153 HC1, .................................. ----------- see "hydrogen chloride" Heat of Evaporation -------------------- ---------------------------II-2 Heat of reaction -- ..................-........................... .........II-2 HONS 04647B Index Page 7 tHigh boilers, distilled, phys. id ohem. prop. --------- Ill-5 handling of ------- ---------------------------- VI-1 no speoifioatlon -------------------------------- IX-1 samples sent to MpL ...................................... IX-9 see also --- ------------------- "Santowax" History of the ProoesB ---- Hold point --------------------------- ---------------- Section XIV' see "Crystallizing point" Hydraulic fluids ---------- ................................................... VII-20 see also under! "Research reports" VII-33 etc. Hydrogen chloride, absorbers - -------------------------------- ----------- XII-85 absorption. Anniston ---------------------------- VII-11- pooling & scrubbing VI-9-.VI-11- equlpment is outdoors,etc. V-2 process in detail ----------- vi-11- see also "Muriatic add" INBRTBBNS ........................... ....................................................... 1-4 Inorganlo ohlorlds 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 Aroolp:irs etc. -------------------------------- IX-84 general methiod............................. -............. IX-91- Iron turnings, preparation of ............................................. VII-1 wastage of in use ....... .................... -............. VII-1 Isomeric ratio, Aroclors ............ .............................. VII-3 trl-tetra chlorbilbenzene---------------------- -- IX-169- JOINTINO AND PACKINGS see "Oaskets" LABOUR REQUIREMENTS ------------------Lay -out of plant ----------------------- u Lectrodryer ------------------------------Lime (hydrated), addition of - speoifioatlon Loss on heating at 100*C., test: method X-2, X-16 ................. V-lsee Air dryer VI-16, VI-22 ...................... IX-3 ................... IX-73 MQNS 046479 index Page 8 MARKET RESEARCH REPORT (MCL) ( ference) -------------------------- VII-31 Melting point test method, Arobi jlor 1271.................................... IX-103 geni 1 --------------------------------------- IX-50- see hilso ------ -"Crystallizing point" Melt tank for Santowax ------------- -.................... VI-2, XII-24 Mill for solid Aroolore ----------- .................................................. - XII-60 Miscellaneous Equipment------ ----- ------------------------------------------ XII-61- Moisture ---------------------------------------- ----------------------------------see "Water" Montars, mentioned ------- ------------- ------------------------------------- phys. properties ------- --------------------------------------------- Ili-17 softening point test i thod------------------------ IX-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-7see also--------- ------------------ "Inventory, monthly" Motors -------------------------------------------- .....................................................XII-50- Muriatic add, carbon treatment of......................................... ---VI-11- batoh records---------------VI-45 Murlatio add, specification see also -------- ....................................................... IX-39 ------------------- "Hydrogen chloride" NOMENCLATURE 1-2- ODOUR, TEST METHOD, AROCLOR 12'TP general ............................................. IX-99 ------------------------------------ IX-56 Off-gas ------------------------------------ - see "Hydrogen chloride" Open Tanks --------------------------- ......................................... XII-68 Operating Data ----------------------- ------------------------------ Section X Operating Instructions, abstracj1t of.........................................-- XV-1- report knentioned------------------------------ VII-31 Operating Records ----------------------- ----------------------------------- VI-36 Outline of Process --------------------- -------------- -- see "Synopsis" PACKING --------------------------------see also "Effects of me| tals" Packings for pump glands -- Parlin viscosity method -- Parr bomb------------------------------ - VI-34- ------- XII-2 to 4 ................. IX-179 see "Chlorine" HONS 046480 Patent Position ------------------------Phenoxy propene oxide ------------------ Index Page 9 see c Iso ---------------------- "Specifications" P.P.O. (phenoxy propene oxide) A'l1"" Previous reports on the process Previous reports, see also "Intr oduotory Notes" at front of book Process, for the different Aroel -------------------------------------------------------1-2 In rietnll -- -- ~ A" ip A"ll" ---------------------------- se also "Bulletins" and "Reports" comments on blending o specifications ------------- ..................... IX-18-, IX-31, IX-36test method for T.C.B. content ---------------------------- IX-106- QUKNCHINO OF STILL BOTTOMS ------- RAW MATERIALS, testing of bulks fefore blending for Pyranole ------- ------------------------------------------------ VI-32 Reoelvers for vaouum stills ------- -------------------VI-15-,VI-21, XII-27 Record Sheets ------------- ----- --- ------------- see "Operating Records" HONS 046401 I Index Page 10 Refractive Index Test Method, A toolore etc. -------------------------- IX-84a e ineral ......................................... IX-15T8 lycldyl phenyl ether --------- IX-163 Resistant paints and drum laoqu irs (Aroclor)------------------------ VI-35 Ring and ball test method --------- SAFETY -.................................. --------------- see "Hazards" Samples sent to MCL, raw materipIs -- finished p:iboduots Sampling procedure, Aroelors ete -----------------------------------IX-9 .................................... IX-183 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-------------------------------- III-5- Scale of Working ----------------------- see "Capacity of Plant" Scavengers for ohlorldes, addition of --.........................................vi-33 alterniatlves -------------------- VII-8, VII-22 ohemlstry of............. ..............................IX-182 oomne(its on--------------------------------------VII-8 effeot of on ohlorlde test --------- VI-33 patent position---------------VII-8, VII-22 removald by earth treatment VI-33,VII-7 Scavengers,, see also------- -"Dlbutyl diphenyl tin" "Olycldyl phenyl ether" ---- "tin tetraphenyl" Sorubber liquor, changes In denpity of------------------------ VI-7, VI-10 Inventory factp;rs .................................................... vi-53 Scrubbers on off-gas --------------- ---------------- XII-22- etc. handling of ................... VI-6, VI-10 Sorubbers on vacuum stills -- ................. XII-19 etc. coimb;nts on ---------------------------------- VII-4- imply,gnatlon of ---------------------- VII-4- Scrubbing of off-gas, comments |>n------------------------------------------------VII-3 Services, requirements of ------- ------------------ X-12a, x-39 Snift gas ------------------------------------ ---------- see "Chlorine" Softening point, method of date:pmination, control test-- VIII-2- Aroclora tuid Montars ------------ IV-59 HONS 046482 Index Page 11 3oftenlng pointsi of Aroolors ( harts) ---------------------------- III-10of Montars (table)----------------------------------- III-17 Solid Aroolors------------------------------ +---------------- see "Aroolors, solid" Solubility data (Aroolors)-------j------- ------------- ----- ------------III-16 Solubility ofgases in Aroolors---------------------------------------------III-16 Speolflcations--------------- -------4--------------------------------- Seotlon IX Specific gravity,test Method, Aroclors ------------------------ IX-71- general method ----------------- IX-96glyoidylphenyl ether-------- IX-164 triohlorobensene ------- IX-69 Specific gravity vs. ohlorine content (Aroolon)ohart -- III-15 vs. lbs. ohlorine and % ohlorine content (Aroolors)ehart -------------- VI-48 vs.teiq>eratur (Aroolors) --------------- III-12Stabillty test-------- -------- ------------------------ see "Oeneral Kleetrio" Stability test method (TCB) test method.............. -...............-IX-120Stabillsatlon of TCB------------------ 1----------------------------------------------IX-10 Stabilisers for Aroolors ---------- l--------------------------------------------- VII-9 Stills ------------------------------------------- |-------------------- see "Vacuum stills" Sulphates, test method in Pyranils etc. ------------------------------ IX-174 Synopsis of Prooess-------------------- 1-------------------------------------------- 1-1- TABIfl OF CONTENTS-------------------------\-------------------------see front of book open--------------------4--------------- -------------------------XII-66 Terphenyls, phys. and ohem. prop. -------------------------------------------- III-6 see also -----------------1- "High boilers" and "Santowax" Test methods, MCL report mentioned----------------------------------------- VII-31 [ ------- ------------------- ----Section IX see also---------------f-------------------------------"Control tests" Thermal data----------------- f---------------------------------------------------- II-2 Tin tetraphenyl, chemistry of action ---------------------------------- VII-14 orystalllses oat from Aroolors--------------- VII-8 determination if in Pyranols ------------------- IX-129 effeot of on chloride test--------- IX-181, -182 mentioned------- 1------------------------------------------------------ 1-4 patent position------------------------------ vii-8, vil-22 removed by Attapulgus earth ------- VII-7, VII-15 sample sent to MCL----------------------------------------- IX-9 specification ------------------------------ --------------- - ix-4- test methods --------------------- IX-132- use of--------------4------------------------------------------------- VI-33 MONS 0A6A83 Index Page 12 Toluene blende, specifications for specification--------- Towers -----------------------------------------Toxicity ---------- ------ ---------- literature review ment^oned references ----------- warning on labels - ............... IX-27...................... IX-2 ............... XII-85 VII-19. XI-1 ------------- VII-29 ....................Ill-2 --------------- VI-54 "Treatment" of distilled Aroolcjrs ----------------------------------------VI-27- comraents on--------------- -- VII-6- see also "Attapulgus earth" Trlchlorobenzene, quality of, cjomsents on ---- -------------------IX-8- alsoussion of-------------------------- IX-8- phys. and chefs, properties------------------------ III-6 sample sent tjo MCL - IX-9 solvent effect VII-l? specification for raw material----------------- IX-6 finished product ---- IX-35 test methods ......................................................... IX-68- Trl-tetrachlorobenzene, cheaper than trlchloro-------------------- IX-40 laomsrl ratio ------------------------------ IX-168- Pspecif! atlon of------------------------------ix-7 test methods ---------------------------------- IX-167- use of VII-8 Turbidity, test method -------------' see also under -------- -IX-159"Colour" UNSTABLB BYB-PRODUCTS OP CHLORIKATION............................. II-1, VII -16 Uses for products ------- --------- see applications of products Utilities -------------------------------- .-- -----------------see "Services" VACUUM STILL HBATINO COILS-------1............................................XII-44- etc. sketch ------------------------------------------ VI-20a Vaouum stills ----------------------------- 1---------------------------------------------- XII-78- dlscusslon of ------- --------------------------------------- VII-5- operatlon of------- 1------------------------------------------------ VI-14- Valves, choice of---------------------------f--------------------------------------------------XII-5 Vapotester ------------------------------ -- XI-6 Vapourlser for ohlorlne--------- ----- VI-2 Vapour pressures ..of Aroolors -* -- Ill-8- curves --Ill-9a- at low temperatures (report mentioned)-----------VII-29 HONS 046404 Vegetation, effect of Aroclors ^n Vleooeltlea of Aroelore --------- ' charts -- Viscosity, conversion graph --------- general test siethod -- Parlin method (IXi Poit) test method------- ---- -- Index Page 13 -- XI-5 . III-8III-10-IX-6lb IX-112- IX-179 IX-6la- WATER, TEST METHOD, IN AROCLORS BTC for traoes Weighing scales Welfare ------------- IX-65-, IX-102, IX-104-------------------------------- IX-65------------------------------- XII-83 ----------------------- Section XI XENENE see "Diphenyl" YIELD FIGURES computation of standard -------- -X-15 X-3X-ll- 046^35 MONS