Document vyk9LELZnwErMXMmnkvky3Zk8

* < MONSANTO COMPANY Organio Chemicals Division Standard Manufacturing Process Por AROCLORS Department 246 deposition exhibit ffft Ye 7 7' WrT Wfln wWl^^n W WW^^n Supersedes: Process description for the manufacture of Aroclors, Dated: December 17, 1962. it. &. CA, Prepared by: h. fl. 6ole, ' Engineer Approved by: wuca Approved by: ncD^ai wu w rETnTTr^.S^srvlBor % ^-p^j JLlbdAttMs Jft /iV D~. B. Hor/DrgT Prdti. Mgr, Issue P.ET Heisler," flen. Prod.apt. Copy of CONFIDENTIAL INFORMATION ThiB Process is the property of Monsanto Company, and the recipient is responsible for its safekeeping. It contains confidential information of Monsanto Company which must not be reproduced, revealed to unauthorized persons or sent outside the company without proper authorization. Either retain in a secure file or return to the Office Services Department. COMPANY TRAN 0091,2 CONFIDENTIAL HARTOLDMONOQ26588 MONSANTO COMPANY Monsanto, Illinoi SAFETY REVIEW COMMITTEE Messrs: P. E. Heisler - WGK H. C Carder - WGK Process Holders Title: U, Bucknelln - Org. Res, H. LrCRobbaod - Org, Res. Tentative Amendment No. "A" Tentative Amendment No. "A" to the Standard Manufacturing Process for Aroclor (Dept. 246, WGK) dated 7/20/64. Objective: Alter present plant distillation system and operations for a plant test. Plant test will indicate equipment needs and ability to produce improved quality (stable) Aroclor. Present Practice: Two Aroclor Di stillation Systems are run in parallel. The two systems are continuous ly fed crude Aroclor from the #2 Blow Tank. The distillation is a straight take-over operation. When a run of one type (1242, 1248, etc.) is completed (80, 000-500, 000#) a final boil down is conducted in No. 2 still and the bottoms are dropped. The boil down material is combined with the previously distilled material and pro cessed to finished product. The bottoms are drawn off and sold as Montar or discarded Following the boil down and bottom*s drop the stills are ready for the next product run. Proposed Procedure: Run the two stills in series. Continuously feed the No. 1 still with crude Aroclor and use this system to pre-heat the entire feed and to distill off a low-boiler fraction (up to 10% of feed). Continously feed the No. 2 still from No. 1 still pot. Collect the intermediate fraction in No. 2 receiver and process as in normal operation. At the end of the run (4-5 days) boil down and drop bottoms. Do not combine the boil down (high-boiler s) with the intermediate fraction. The low boiler s from No. 1 receiver and the high boilers from the boil-down will be isolated in a storage tank, if possible. COMPANY CONFIDENTIAL TRAN 009193 HARTOLDMON0026589 Tentative Amendment "A' - Z- March 10, 1965 If they pass non-electrical Aroclor apecifications, they can be used as such. If the total amount has to be discarded because no storage is available, or because t hey are out of specification, the cost would be $3, 000 based on total product costs. Specific operating conditions for the stills will have to be determine d in the field by cut and try methods. Justification; Foreign competition appears to be capable of producing Aroclor which is more stable than that presently made by Monsanto. An improvement of product stability is necessary to protect our market position. laboratory data* indicates that the distillation operation ha s a significant effect on product stability. These data indicate that product stability can be improved by: 1. Removing an unstable low-boil fraction Z. Preventing entrainment 3. Preventing contamination by high-boilers or bbil down This test will evaluate our ability to control the plant distillation in the three areas mentioned above,, with existing equipment. Failure of the test will indicate that more drastic revisions to the existing equipment will be needed to approximate laboratory conditions. Comments:' The production rate will be limi-ted by maximum vapor and heat loads that can be sustained in the entrainment and condenser systems on N, Z still. In the past 55, 000#/day have been attained in these systems. The upper limit is not presently known. Duration: The test duration will be 4-5 days. If desired operation conditions cannot be obtained during this interval the test will be cancelled or revised. Prepared by*. COMPANY CONFIDENTIAL *WGK PR&D Reports J-62, 2/15/65 and J-78, 3/ 8/65 Qyi:'jJJJz. D. R. Middleton . J. Luecken TRAN 009194 HARTOLDMON0026590 Tentative Amendment "A" Approval*: -3- March 10, 1965 D. . Harris vrnd A. Hullendore COMPANY confidential TRAN 009195 HARTOLDMON0026591 I ** MONSANTO COMPANY Monsanto, Illinois July 12, 1965 Messrs; P. E. Heisler - WGK H. C. Carder - WGK Process Holders R. W. Bucknell - Org, Res. H, L. Hubbard - Org. Res. Tentative Amendment No. "B" TITLE; Tentative Amendment No. "B" to the Standard Manufacturing Process for Aroclor (Dept. 246, WGK) dated 7/20/64. OBJECTIVE: . Run two plant tests using revaporized CI2 and dilute (25 mole %) Cl*, as feed stock for Aroclor 1242 production, PRESENT PRACTICE: i The Dept. 246 Chlorinators are batch charged with biphenyl (Bi0). The BiO is then chlorinated by continuously feeding "Snift" gas to the ehlorinator mass until the desired specific gravity is reached. The "Snift" Gas is a mixture of Cl2 (from DeNora 6c Hooker Cells) H2, N2, 02, CO* and trace amounts Of organic impurities. The Cl2 concentration is in the range of 75 - 95 mole % and varies with operations in the Cl* depart ments . PROPOSED PRACTICE (Two Plant Tests, 1242 Aroclor) 1. A plant, chlorination test will be run using re vaporized Cl* from Dept, 232 as the Cl* feed stock, Due to limited capacity of the revaporizing facilities in Dept. 232, we will probably be able to run only two chlorinators at a time, making a total of 5 - 6 chlor- inator batches and processing through the remainder of the system as normal. Necessary samples and measurements will be taken to determine effect of concentrated and impurity free Cl* on Aro clor stability. This material will be treated as normal production as it passes the routine plant controls. .2 A plant chlorination test will be run using revaporized Cl2 diluted to 25 mole % with dry air as Cl* feed stock. This test will be limited to 2 chlorinators due to dry air capacity, making a total of 5-6 chlorinator batches and processing through the remainder of the system as normal. Necessary samples and mea surements will, be taken to determine effect of dilute and impurity free Cl* on Aro clor stability. This material will be segregated from normal electri cal grade 1242 Aroclor. It will be used Sox non-clectrical 1242 if it passes specification. COMPANY ' CONFIDENTIAL TRAN 009196 HARTOLDMON0026592 Tentative Amendment No. "B11, JUSTIFICATION: Foreign competition appears to be capable of producing Aroclor which is more stable than that presently made by Monsanto, An improvement of product stability is necessary to protect our present US. market position and for possible expansion of foreign sales. These tests will provide information as to the effect of contaminants in chlorine, and the possibility of local over chlorination due to concentration effects. COMMENTS: - For the revaporized Cl* test the production rate will be limited to about 32, OOOdf/day for a duration of 1 - 1 1/2 days, For the dilute Cl* test the rate will be limited to about 11,0001/day for a duration of 3 days, SAFETY: No increase in safety hazards is for seen in these two test runs. Prepared by: APPROVALS: D, R. Middleton D. E. Harris 7-/6-6S- SAFETY REVIEW COMMITTE COMPANY CONFIDENTIAL TRAN 009197 HARTOLDMON0026593 MONSANTO COMPANY Monsanto, Illinois September 1, 1965 Me sere: P. E. Heisler - WGK H. C. Carder - WGK Process Holder R. W, Bucknell - Org. Res. H. L. Hubbard - Org, Res. Tentative Amendment No. __ C TITLE: Tentative Amendment No. C to the Standard Manufacturing Process (Dept. 246, WGK) dated 7/20/64. OBJECTIVE: Run plant te6t using chlorinator without catalyst basket, PRESENT PRACTICE: The Dept. 2 46 batch chlorinator* (31 diam, x 16' high) are batch charged with biphenyl, which is chlorinated with snift gas. At the present, each chlorinator has a catalyst bed. The catalyst bed is 2'3" in diam, and 81 high and consists of 1 1/2" pipe nipples, Z" long, PROPOSED PROCESS (1242 and 1260 Aroclor) Remove the catalyst bed from one chlorinator and run three to five 1242 and three to five 1260 batches in that chlorinator following standard operat ing procedures, except without the catalyst bed. The test material will be kept separate from other production and will be used only if it is equivalent to normal production aroclor, according to routine analyses, Du ring the test batches the chlorinator off-gas will be sampled and analyzed for chlorine,, to check chlorine utilization of the chlorinators without the bed. The purpose of the catalyst bed is to provide iron, which is chlorinated to ferric chloride, the reaction catalyst, It is standard operating procedure to charge 0.05% by weight ferric chloride to each batch, Ferric chloride will, of course, be added to the test bate he s. JUSTIFICATION: During operation the catalyst becomes plugged with tars and ferric chloride and it is probable that only a small portion of the iron of the bed is available for utilization. Also, the plugged bed hinders chlorinator circulation and probably leads to hot spots in the chlorinator. There is a problem of cross contamination from batch to batch with the bed^which results in an excessive amount of overchlorinated products , COMPANY "an 009198 CONFIDENTIAL HARTOLDMON0026594 Tentative Amendment C 2 JUSTIFICATION? (Cont'd.) During 1 956 there were levere problem6 with arodor stability, One of the problems wa s a lack of a consistent analytical method for checking stability. Previous to that time the catalyst bed was relied upon to supply ferric chloride and ferric chloride, per se, was not added. One of the results of the stability problem was the addition of ferric chloride to each chlorinator batch, to allure that sufficient catalyst was available, Since that time analytical methods have improved and any unstable aroclor produced would be detected immediately. The removal of the catalyst bed, then, improves chlorinator operation by increased circulation, elimination of hot spots, and prevention of contamina tion, The addition of ferric chloride provides sufficient catalyst, Any unstable aroclor produced would be detected immediately by the present routine analyses. SUPPORTING DATA : It is reported in St. Louis Research Report Nos. 1640 and 2072 that a minimum level of 0. 03% FeCls is necessary to produce stable aroclor. No mention is made of the need for iron, and none wa6 used in the lab chlorinators. SAFETY: No increase in safety hazards is anticipated. QUALITY: Work is in progress to improve aroclor quality (stability). It is anticipated that the removal of the basket will not harm quality but, if anything, will improve it due to improved circulation,, elimination of hot spots in the chlorinators, and elimination of cross-contamination from batch to batch. DURATION OF TEST Three to five 1242 and three to five 1260 batches will be made without the catalyst bed. If this material i6 equivalent to normal production material, according to routine analyses, the chlorinator without the catalyst bed will be used for normal operations, and this amendment incorporated as a process revision. If the test material is not equivalent to normal production the bed will be replaced. COMPANY TRAN 009199 HARTOLDMON0026595 Tentative Amendment No, C 3 COMMENTS: This plant test would normally involve some loss of production. The pre sent aroclor stock position is such that it is anticipated that it will be nec essary to run only three of the five chlorinators during September. Also, some repair s to be made dur ing September will require removal of the catalyst bed from the No. 3 chlorinator, September, then, is an ideal time to run this test. Prepared by: W. C. nramp/T APPROVALS: P, E. Heisler ir Date D. E. Harris Date p. - emc SAFETY REVIEW COMMITTEE ?-.y -z -T 3--(?v3*"~~ . company CONFIDENTIAL TRAN 009200 HARTOLDMON0026596 MONSANTO COMPANY Monsanto, Illinois SAFETY REVIEW COMMITTEE y.p October 20, 1965 Messrs: P. E. Heisler - WGK H. C. Carder - WGK Process Holders R. W. Bucknell - Org. Res. H. L. Hubbard - Org. Res. Tentative Amendment No. "D" Title: Tentative Amendment No, "D" to the Standard Manufacturing Process for Aroclor (Dept. 246, WGK) dated 7/20/64. Objective: Evaluate potassium carbonate as a replacement for lime in the Aroclor distillation system. Present Practice: Aroclor is distilled in two parallel Bystems, continuously fed from the No. 2 blow tank. At the start of a run (1242, 1248, etc. ) 200 lbs. of lime (calcium hydroxide) is added to each still pot. At the end of a run (250,000-500,000 lbs.) bottoms are dropped and the cycle is repeated. Proposed Procedure: Segregate the two distillation systems at the start of a 1242 run. To one system, add the normal amount of lime to the still pot and proceed normally throughout the run. To the second system, substi tute 200 pounds of anhydrous potassium carbonate for the lime. Dis till away from the potassium carbonate for a minimum of two days. The product distilled from the potassium carbonate will be analyzed by routine tests before it is combined with normal production , material. ' >ay, '-'it will b ' . COMPANY CONFIDENTIAL 009201 HARTOLDMON0026597 Tentative Amendment "D" 2 October 20, 19G5 Justification: The presence of a base during distillation serves two known purposes: It neutralizes free acid, and It reacts with the FeCla present. It Is also thought that the base can react with some unstable Aroclors, converting them to a more stable form. Recent WGK PRfcD laboratory data Indicates that distillation from KgCOs Increases the stability of the high boiling fractions of Aroclor 1242 (low boll and mid fractions are essentially unaffected). If this proves to be the case, it would Indicate that using KgCOa and making a simple low boil cut may be a practical way of making a stable Aroclor. Safety: No increase in safety hazard Is anticipated. No unusual effect was seen in laboratory distillations using KgCO. Comments: -- - No production loss will be involved since WGK Dept. 246 is presently running at only 75% of demonstrated capacity. Prepared by: APPROVALS: D. E. Karris /o/>y/cr Date Date A. Mullendore Date >4 COMPANY CONFIDENTIAL TRAN 009202 HARTOLDMONOQ26598 MONSANTO COMPANY Monsanto* Illinois Msssr s: P. E. Heifiler - WGK H. C. Carder - WGK Protest Holders December 3, 196 5 R. W. Bucknell - Org. Res. H. L. Hubbard -Org , Res . Tentative Amendment No. "E11 TITLE Tentative Amendment No. "E" to the Standard Manufacturing Process for Aroclor (Dept. 246, WGK) dated 7720/64. " OBJECTIVE Produce more stable Aroclor 1242 by chlorinating without a catalyst basket in the chlorinator and processing as normal. Produce more stable Aroclor 1242 by chlorinating without a catalyst basket in the chlorinator and processing it through the still system with pota ssium hydroxide added in place of the normally used lime (calcium hydroxide). Provide sufficient product, produced as above, for testing by customers. PRESENT PRACTICE Biphenyl (Bi0) is chlorinated in the chlorinators which contain catalyst baskets. Previously the basket furnished FeClj catalyst for the reaction, Pre sently (since 1957) sufficient amount of catalyst, needed to produce stable Aroclor, is added to each chlorinator when batch charged. At the beginning of a product (1242, 1240, etc.) run 200 pounds of lime is added to each still. The purpose of the lime is to tie up FeCl> and neutralise HC1 in the crude. PROPOSED PROCEDURE Produce 8-9 batches of 1142 in No. 5 chlorinator with the catalyst ba sket removed. This ha s been done previously a s per Tentative Amend ment No, "C", Process half of this crude material through the remainder of the system as normal, and drum it off from the finished product tank. Process the other half through No. 1 still system, but substitute potassium hydroxide (0.06% of crude charge) for the lime in the still. Drum this . material off from the finished product tank, thus producing approximately , 1, 000 gallons of each type of test material to be used as samples for evaluation by electrical grade customers. Any^exc*sa t estimatoria 1 will COMPANY TRAN 009203 CONFIDENTIAL HARTOLDMON0026599 V , PROPOSED PROCEDURE (Cont'd. ) be sold at non-electrical grade 1242 providing it panel all (pacification*. JXJSTIFICA TION From previous plant testa, the Aroclor produced in a chlorinator without the catalyst basket was equivalent or better than normal material. By removing the baskets, hold-up and cross - contamination are reduced. Results of PR &c D Laboratory studies indicate more stable Aroclor (i.e. 0. 15 ppm Cl by thermal chemical chlorides) can be made by addition of KOH to the still pot and stripping off the first 1.2% of the low boilers. Plant equipment will not permit this type of fractionation, but an improve ment over normal production is expected. SAFETY No increase in safety hazzards is anticipated. No unusual effects were seen in the laboratory distillation using KOH. Normal precautions in handling KOH will be followed. APPROVALS: Prepared by*. D. R. Middleton D. R. Middleton E. Heisler Vs/jf Date Ur_ tr, 2 <T. D. E. Har: Til ft^ R. W, Bucknell Date lllyiS Date' UA fl'fX < ' ry-f` PAift. fZ/l/tS___ ft ft*-- O COMPANY TRAN 009204 yf CONFIDENTIAL HARTOLDMON0026600 Monsanto, Illinois .May 10, 1965 AMENDMENT DISPOSITION .Tentative Amendment No."A" to the Standard Manufacturing Process for Aroclor(Dept.246, WOK) dated 7/20/64, Tentative Amendment No, "A" Is dated 5/10/6$. TO: Messrs: P. E. Heisler - WOK H. C. Carder - WOK D. E. Harris - WOK J. J. Luecken - WOK R. W, Bucknell - Org, Res, H. L. Hubbard - Org. Res. J. A. Mullendore - Gen. Off. Process Holders - c/o P. J. Prader - WOK This memo is to serve as a disposition of the subject tentative process amendment. The purpose of the amendment was to alter the present plant distillation system and operations for the duration of a plant test, The purpose of the plant test was to indicate equipment needs and ability to produce Improved quality (stable) Aroclor, No improvement in stability was realized and the need for fractionation was demonstrated,* The distillation system was returned to normal operation as specified in the Standard Manufacturing Process. The subject amendment should be recorded in the Standard Manufacturing Process, but not incorporated as a process revision. 00. ft, D. R. Middleton Technical Services Dept. vmd WOK TSD Report - Aroclor: Improve Electrical Grade Quality, 91370:5198, Report No.l, dated 4/14/65. COMPANY CONFIDENTIAL TRAN 00,205 HARTOLDMON0026601 DISTRIBUTION SHEET 1. Technical Information Center St. Louis Research 2. Technical Information Center St. Louis Research 3. Security Pile (Records Center, St. Louis General Offices) Director of Manufacturing/Technical Production Manager Organic Engineering ......... - ---------- 5. Production Oeneral Superintendent/Production Supervisor - W.G,K. 6. Plant Technical Services 7. Extra C. 8. Extra 9. Extra Q-f. 10. Extra 9Copy COMPANY CONFIDENTIAL TRAN 009206 HARTOLDMON0026602 I. II. III. IV. TABLE of CONTENTS SYNOPSIS OP PROCESS ........................................................ FLOW SHEETS........................................................................... A. COMPLETE PROCESS FLOW SHEET B. CHLORINATION REACTION STEP C. AERATION AND DISTILLATION C. BLENDING, FILTRATION AND STORAGE PROCESS IN DETAIL ............................................................. A. NOMENCLATURE AND BATCH DATA B. CHLORINATION REACTION STEP C. AERATION AND DISTILLATION D. BLENDING,FILTRATION' AND STORAGE E. BY-PRODUCT HYDROGEN CHLORIDE COMMENTS ON PROCESS ......................................................... A. CHLORINATION STEP B. AERATION tc DISTILLATION C. BLENDING & FILTRATION D. OENERAL APPENDIX A - EQUIPMENT LIST ...................................... APPENDIX B - FINISHED GOODS AND RAW ................... MATERIAL SPECIFICATIONS APPENDIX C - PHYSICAL AND CHEMICAL DATA . . , APPENDIX D - UTILITIES............................................... .... APPENDIX E - PERSONNEL................... '......................... APPENDIX F - PACKAGING AND SHIPPING ................... APPENDIX G - MATERIAL BALANCE ........ APPENDIX H - ATMOSPHERIC DISCHARGE AND . WASTE DISPOSAL ., APPENDIX I - PROCESS CONTROL PROCEDURES . . . APPENDIX J - SAFETY AND TOXICITY DATA . . . . APPENDIX K - BACKGROUND ................................................ APPENDIX L - TIME CYCLES ............................................... APPENDIX M - QUALITY CONSIDERATIONS ................... APPENDIX N - MISCELLANEOUS .......................................... COMPANY CONFIDENTIAL Page . 1-2 2 4 3-6 7 ..7-6 8 . 9 -12 . . . 12-21 ... 22 . . . . 22-29 . . . . 20-2^ . . . .22-26 . . . .27-23 . . . .29-^1 . . . .A2 . . . A2 ...M ... .51 . ... 52 . . . 52-59 . . . . 6.0-62 TRAN 009207 HARTOLDMON0026603 Dept. 246 <- Process Description AROCLOR 1. SECTION I SYNOPSIS OF PROCESS Aroclor Is a trade name used to designate chlorination products of biphenyl, biphenyl high boilers, or mixtures of the two. Liquid Aroclors are produced by chlorinating biphenyl to 21, P2, M2, M8, 54, 60, and 62% chlorine content. Chlorination above 6y% yields a solid product at normal temperatures. Liquid Aroclors are ldentlfiet by four digit numbers: The last two digit numbers represent the chlorine content (percentage by weight), and the firrt two numbers represent the Aroclor condition (crude or distilled). Crude Aroclor: start with the prefix 11 whereas distilled Aroclors start with the prefix 12. For example, Aroclor 1242 is a distilled chlorinated biphenyl containing M2% chlorine. The first process step in the manufacture of Aroclors is a chlorina tion reaction. Biphenyl ( 0-0) and chlorine (Cle) gas in the presence of a Ferric Chloride (FeCla) catalyst are reacted to form a chlorinated aromatic compound, Hydrogen chloride (HC1) gas is liberated during this reaction and piped to the muriatic acid department. The exact chemistry of biphenyl chlorination is unknown. Many isomers are formed. A schematic representation of biphenyl chlorination is as follows: BIPHENYL M.W. 154 CHLORINE M.W. - 71 n HC1 +p6,200 n Btu. AROCLOR . HYDROGEN M.W.*(257.1- CHLORIDE 595-6) M.W. * 56.5 COMPANY CONFIDENTIAL THAN 009208 HARTOLDMON0026604 Dept. 246 - Process Description 2. AROCLOR SECTION I SYNOPSIS OF PROCESS The eecond process step ie the aeration and diatillation of the crude Aroclor. Dry air ia blown through the crude Aroclor for a period of two hour a or more. Aeration removes most of the free hydrogen chloride. Diatillation of-crude Aroclors is done-under vacuum auto matically controlled with the controller pre-set between 30 - 50 mm Hg. abs. to obtain the best performance. Distillation of crude Aroclor aeparatea residue lime, ferric chloride, and tars from the finished product. The third process step includes blending, filtration, and storage of Aroclors, Approximately 0. 1 -1 0.2% by weight of Attapulgus earth is .added to the distilled Aroclors The mixture is agitated and filtered to the finished product tank. The purpose of the Attapulgus earth is to absorb moisture and chloride ion to improve the electrical properties of the Aroclor. During the filtration of distilled Aroclor. 2-16 or. samples of the finished product are taken to the laboratory for control analyses. If the control analyses pass specifications, the batch is transferred to a storage tank. This process description will describe the production of Aroclors 1242, 1246, 1254, 1260, 1254 Xylene mix, and 1262. , COMPANY CONFIDENTIAL TRAN 00,209 HARTOLDMON0026605 Dept. 246 Procen Description AROCLOR SECTION II FLOW SHEETS This section contains the following flow sheets. 2. Complete process flow sheet. 2. Chlorination Reaction Step 3. Aeration and Distillation 4. Blending, Filtration and Storage. COMPANY CONFIDENTIAL TRAN 009210 HARTOLDMON0026606 HARTOLDMON0026607 AERATION A DISTILLATION i I % :h COMPANY CONFIDENTIAL TRAN 009212 HARTOLDMON0026608 l COMPANY CONFIDENTIAL than 009213 HARTOLDMON0026609 Dept, 246 - Process Description AROCLOR SECTION III PROCESS IN DETAIL A. Nomenclature and Batch Data Aroclor i* a trade name used to designate chlorination products of bipbemyi^ biphenyl high belle rs, or a mixture of the two. The physical properties vary from light free flowing liquids to crystalline and non* crystalline solids, depending upon the degree of chlorination and the composition of the raw materials. Chlorinated biphenyl yields a liquid product of increasing viscosity up to and including 63% chlorine. Chlo' rination above 63% yields a solid product at normal temperatures, A numerical system of nomenclature, consisting of four digits, has been developed for identifying the various Arociors; The'first digit denotes the aromatic raw material used in the chlorination step. The figure 1--- indicates 100% technical grade biphenyl. The second digit denotes whether or not the product is distilled. The figure -1-- indicates undistilled product, and the figure -2- - indicates a distilled product. The last two digits of the nomenclature system denote the approximate percent age by weight of chlorine contained in the finished product. For example, Aroclor 1242 is a distilled chlorinated biphenyl containing 42% chlorine, Manufacture of all liquid Aroclors is essentially the same. Batch data are listed below: Type Aroclor 1242 1248 1254 1260 1262 Biphenyl Charge 4000# 4000# 4000# 4000# 4000# Chlorination Time 10 - 12 hr. 10-12 hr. 14-17 hr. 16-20 hr. 16-22 hr. Specific Gravity of Crude 1.349-58 1.408-18 1.498-508 1.558-69 1.580-90 at 65*C at 65 *C at 65*C at 90*C at 90`C Weight of Crude Batch . 6670# 7580# 6450# 9600# 10,600# Weight of Distilled Batch 6330# 72001 8040# 9100# 9850# Tons of 100% by-product HC1 per Batch 1.24 1.43 2.27 2.47 2.70 Theoretical Molecular Weight 257.7 292.6 326.6 369.5 395.6 COMPANY CONFIDENTIAL TRAN 009214 HARTOLDMON0026610 Dept, 246 - Proce Description AROCLOR 5. SECTION III PROCESS IN DETAIL B, Chlorination Reaction Step Chlorination of biphenyl ii the only proeen step whe re a chemical reaction take* place, All other Arcelor process operations a re mechanical. The starting raw materials for Aroclor production are biphenyl and chlorine gas. , Biphenyl is received in 8, 000 and 10, 000 gallon tank cars from Anniston, Alabama, The biphenyl in the tank cars is a solid mass because the crystallising point of biphenyl is .68. 7 *C. Steam must be applied to the -----tank car coil to melt the biphenyl. It-is noeeeeary to msit-a vent hole------through the solid mass of biphenyl by insertion of a hairpin steam coil through the tank car dome before applying steam to the tank car coils. The vent hole avoids a pressure build-up in the bottom of the tank car and possible damage to the car. When the biphenyl is completely melted, it is sampled (or crystallising point and moisture content and unloaded through the tank car standpipe by air pressure to the 25, 000 gallon storage tank. Dry air is used to unload the biphenyl cars to keep the biphenyl free from moisture. The flash point of biphenyl is 112 *C. Chlorine gas is received in a 4 inch pipeline from the chlorine depart ment. In order to facilitate operation of the chlorine liquefaction system, "sniff gas with a purity of 75-95% (the remainder being air) is transferred from the chlorine department. The normal pressure of the chlorine gas in Department 246 is 20-25 psig. Biphenyl (4000#) is charged into each chlorinator. from the measuring tank. The biphenyl charge in the measuring tank can be regulated by valves at different overflow levels. The fotir overflow levels on the measuring tank permit biphenyl charges of 1800, 2800, 3600, and 4000 pounds. The measuring tank is equipped with an agitator and circulating pump. Two pounds of ferric chloride (0. 05% of charge) are charged into the measuring tank for each batch. The charge from the measuring tank is pumped through the circulating line to the chlorinators. Chlorination is carried out in five chlorinators . Each chlorinator is three feet in diameter by sixteen feet high, and constructed of steel. Each chlorinator has a catalyst bed which is 2' 3" in diameter by 8 feet high. The catalyst bed consists of 1 1/2 inch diameter by 2 inches long pieces of pipe which are similar in nature to raschig ringe. The biphenyl charge is heated to 120*C. or higher before chlorination is started. After charging the chlorinator, circulation of the charge is started before the chlorine feed is begun to maintain an even distribution of the ferric chloride catalyst. . COMPANY 1UM oo92i5 CONFIDENTIAL HARTOLDMON0026611 Dept. 246 Proees* Description AROCLOR 6. SECTION 111 PROCESS IN DETAIL B. Chlorine gas from the chlorine department passes through a Brink mist eliminator and evaporator before entering the chlorinator. The . mist eliminator remove* most of the impurities, and the vaporator insures that all of the chlorine is gaseous. The purified chlorine gas is admitted to the bottom of the chlorinator , through a distributor plate (Sparger) and passes through the catalyst bed. A chlorinator temperature less than 170*C. should be maintained during the chlorination reaction o avoid sublimation and subsequent condensation of biphenyl in the off-.gas system. Each^chlorinator is ____ equipped with a Brink mist eliminator. The purpose of the off-gas mist eliminators is to trap entrained particles of Aroclor and biphenyl. The chlorination temperature in the chlorinator s is controlled by auto raatie chlorine gas flew regulation to hold the temperature within 4* 5 *C. The chlorination tempe rature must be at least 120*C, at the beginning of the batch and no more than 170*C. to finish off a batch. The normal batch temperature is 150*C. The louvers of the air-cooled heat exchanger located in the external circulating line of the chlorinator are positioned ( such that the batch temperature will remain between 120*C. and 170*C. The exact batch temperature will depend on the chlorine flow rate which will fluctuate to maintain a batch temperature of 150*C. The louver adjustment is manually controlled by a hand valve located in the control room. The temperature of the batch is recorded at four different points; (1) in the center of the chlorinator, (2) just above the chlorine sparger in the chlorinator, (3) at the discharge of the chlorinator pump, and ^ (4) at the discharge of the air-cooled heat exchanger. Point 1 is alarmed for high temperatures, and point 4 is alarmed for low temperatures. As ^ a safety device, a high temperature sensing element is positioned at point 2 to shut off the chlorine gas flow if the reaction temperature exceeds 190*C. COMPANY CONFIDENTIAL The batches are continuously circulated at an average flow rate of 200-220 GPM from the bottom of the chlorinator, up through the air-cfeeled heat exchanger, and back into the top of the chlorinator over the catalyst bed. Chlorine feed up to e maximum of 1500 pounds per hour is fed into each chlorinator through a flow recorder-Integrator which is alarmed. The aero return integrator measures the total amount of chlorine gas flow per batch at any given time and will shut off the gas flow when the desired pre-set pounds of chlorine has entered the reactor. The average chlorine feed rate is 1000 pounds per hour. Progress of the chlorination reaction is checked periodically as needed t after a pre-set amount of chlorine gas as measured by the recorder-inte grator passes into the chlorinator. The degree of chlorination is measured by determining the specific gravity of a sample taken from the circulating line. More frequent gravity checks are made when approaching the end of chlorination. TRAN 009216 HARTOLDMON0026612 Dept. 246 - Process Description AROCLOR Y. SECTION III PROCESS IN DETAIL C. Aeration and Distillation When chlorination 1b complete, the crude Aroclor is pumped Into number two blow tank (Capacity 2000 gallons). The crude Aroclor is aerated In-the #2-blew tank for two hours or more with dry air. Aeration of crude Aroclor removes most of the free hydrogen chloride. Crude aerated Aroclor Is transferred from the #2 blow tank to the #1 blow tank. The #1 blow tank Is used as a crude Aroclor feed tank to - the stills. Crude aerated Aroclor Is transferred from the #1 blow tank to vacuum stills through an automatic control valve which maintains a constant level In the stills. Under normal conditions the automatic feed to the stills Is. shut off after distilling about 75,000 pounds of Aroclor. (This Is equivalent to filling 7 still receivers). . The still is then boiled down until a temperature 0 difference between the still coil inlet and outlet approaches 40 c. At this point distillation is discontinued and all but a small heel of the residue is drawn off to drums and discarded or sold as Montar. The still is immediately recharged with crude Aroclor and 200 pounds of lime is added directly to the still pot. Hydrated lime is received in 50 pound bags. The lime neutralizes any residual HC1 in the still liquor and prevents sublimation of ferric chloride during the distillation period. Distillation of Aroclors is done under vacuum automatically controlled. The best performance is obtained at a steady vacuum which can be pre-set by a controller between >0-50 mm Hg. Abs. Natural gas is used to heat the coil of the Aroclor still furnaces. The pressure of the gas burner (eclipse, st. 108.5* 2", #508, 60000C BTU/nr.) is adjusted as needed for production requirements^ The normal gas pressure is 2-> psig. . ' D. Blending, Filtration, and Storage When the still receiver is filled, the distilled Aroclor is pumped tc the blend tank (2000 gallon capacity). After two fillings of the receiver tank have been pumped to the blend tank, approximately *10 pounds of attapulgus earth is added t the distilled 1242 Aroclor. All other Aroclors are earth-treated with 20 pounds of Attapulgus earth. Regular Attapulgus earth is received in 50 pound bags. The mixture is agitated and filtered to the finished product tank (2000 gallon capacity) through a >6 inch stainless steel Sparkler Filter. The Attapulgus earth is roasted at 250C. for a minimum of four hourt . in a Qrieve-Hendry drying oven before addition to the blend tank. The purpose of earth heat treatment is to remove any moisture in the earth and activate it. The Attapulgus earth absorbs water and ; ionic impurities. This improves the electrical-quality properties oi the Aroclor. COMPANY CONFIDENTIAL TRAN 009217 HARTOLDMON0026613 Dept. 246 - Process Description 0. AROCLOR SECTION III PROCESS IN DETAIL D. Blending, Filtration, end Storage (Cont'd.) is cleaned after about 5*7 batches or as needed. During the filtration, 2*lb os, samples are taken to the laboratory for control analyses, If the control analyses pass specifications, the batch is trans ferred from the product tank to a storage tank. After several batches have accumulated in the storage tank, the contents of the tank are mixed, ' and composite samples are taken for lot analyses, Three underground (15, 000 gallon) tanks and five Above-surface (each ~ 20, OOO gallons) are available for storage of the finished products. The blend tanks, finished product tanks, and Aroclor 1242 and 1254 ` storage tanks are blanketed with nitrogen. The pressure of the nitrogen gas is 10 psig. Nitrogen blanketing maintains the electrical properties of the Aroclors. The Aroclors from the storage tanks are drummed, "pumped to tank cars, ' pumped to tank trucks', or transferred to Department>A<-24 6 or B-246' mixing ' tanks for the production of Fyranole, interteens, or Pydraul A-200. Batches of Aroclor 1254-mix are mixed in the #1 blend tank. This opera tion consists of a mijc of 10% xylene, and 90% Aroclor 1254, Xylene is received in 55 gallon drums , The flash point of xylene is 85 *F. Mixing, sampling and drumming of 1254-mix is accomplished directly from the blend tanks. After the blending operation, the blend tank must be cleaned. The bottom outlet of the tank is opened and the tank is cleaned out with live steam and then blown with air. . E. By-product Hydrogen Chloride The by-product hydrogen from the chlorinators is collected in a common pipeline header and flows to the central HCl absorption unit to manufacture Muriatic Acid in Department P-218. If Department F-218 is unable to handle the off-gas, it may be sewered at Department 24b by pa a ting through a Haveg S-K drowning jet. The removal of HCl from the off-gas concentrates the original quantity of hydrogen and air to a point well with in the explosive limit. Therefore, it is essential to either dilute thip gas going up the vent stack or increase its velocity past the flame propogation rate (15 ft. /sec.). This is accomplished by introducing a sufficient quantity of steam into the vent stack. COMPANY TRAN 009218 HARTOLDMON0026614 Dept, 246 Process De scription AROCLOR SECTION IV COMMENTS ON PROCESS CHLORINATION STEP A , Raw Material Yields 9. Biphenyl and chlorine are reacted to form a chlorinated biphenyl called Aroclor. The yields on biphenyl and chlorine vary with the type of Aroclors produced. Each particular type of Aroclor has its own standard yield factors. Yields are not reported for the individual type on Aroclor each month. An average yield is reported monthly and compared with standard and theoretical yields which are calculated according to the quantities of the various Aroclofs produced during the month. Standard and theoretical conversion factors used in computing Chlorine and biphenyl yields are listed below. STANDARD CONVERSION FACTORS AROCLOR 1242 1248 1254 1260 1262 1232 1254 Xylene CHLORINE #/# Product .9032 1,0323 1.6130 1.2903 1.3333 0.6882 1.0452 BIPHENYL tf /H Product 0.6180 0.5580 0.4978 0.4368 . 0.4163 0.7216 . 0.4480 THEORETICAL CONVERSION FACTORS AROCLOR 1132 - 1232 1142 - 1242 1148 - 1248 1154 - 1254 1160 - 1260 1162 - 1262 1254 - 10% Xylene CHLORINE #/ Product 0.6400 0.840Q 0. 9600 1.0800 1.2000 1.2400 0.9720 BIPHENYL #/0 Product 0.6891 0.5919 0.5357 . . . 0.4754 0.4147 0.3976 0.4279 COMPANY CONFIDENTIAL TRAN 00921' HARTOLDMON0026615 Dept, 246 - Process Description 10. AROCLOR SECTION IV COMMENTS ON PROCESS CHLORINATION STEP_____ B. Capacity The monthly production capacity of Department 246 is 1,700, 000 pounds (2, 400, 000 pounds is expected by August 1, 1964) of Aroclors on a 7 day ,, per week ba sis. The capacity of the chlorinators is a function of the following variables. ' Lc Baleh Cooling Rate Chlorination of biphenyl i an exothermic reaction which produce s 510 BTUS per pound of chlorine gas unde rgoing a reaction with biphenyl. Biphenyl can be chlorinated as fast as the exothermic heat can be removed from the batch and maintain a batch temperature of 150*C. 2. Chlorine Flow Rate - the reaction time decreases as the Chlorine flow rate increases. The chlorine flow Tate is approximately 1000 pounds per hour per chlorinator. A maximum chlorine flow rate of ' 1500 pounds per hour per chlorinator can be attained if desired. The concentration of chlorine in the "anift" gas is another factor control ling the rate of chlorination. 3, Catalyst - The chlorination rate increases when ferric chloride catalyst i6 added to the charge. The be6t re6ult6 are obtained when the biphenyl charge contains .05% ferric chloride catalyst, C. Quality . Some of the factors which affect Aroclor quality are as follows: 1. Temperature - According to research experimental results, the chlorinator temperature must be greater than 120*C. at the beginning of the chlorination reaction to produce stable Aroclors. 2. Catalyst - Good contact is necessary to produce stable Aroclors. It is suspected that agitation and circulation of the reactants improve the effectiveness of the catalyst. The catalyst is also responsible for the chlorine positioning on the biphenyl molecule. Ferric chloride catalyst may be responsible for producing the desired end product. Results of research work concerning catalyst and Isomeric distribution are given in Appendix N. TRAN 009220 HARTOLDMON0026616 Dept, 246 - ProceB Description 11. AROCLOR SECTION IV COMMENTS ON PROCESS CHLORINATION STEP C. Quality (CoatM, ) 3. Raw Material Purity - The purity of raw materials can affect the quality of Aroclors both directly and indirectly. In a direct manner, impurities which are ionic lessen the resistivity of Aroclors, Dis- - tillation of crude Aroclor separates most of the ionic impurities; however, minute impurities can be carried over to the receiver tanks. Attapulgus earth can remove the remaining impurities in most instances. If any ionic impurities remain after the earth treatment, the resistivity of the Aroclors will be low because such impurities will conduct electricity even in minute concentrations. In an indirect sense, impurities such as sulfates in the chlorine gas, will poison the ferric chloride catalyst and thus unstable Aroclors will be produced. The chemistry and mechanism of the catalyst poisoning are not known for certain. AERATION AND DISTILLATION Steam is not applied to the coils of the blow tanks when aerating Aroclor 1142 and 1148. This prevents the loss of Aroclor vapors. Eighty.psig steam is applied to the coils when aerating other Aroclors. High moisture may be removed effectively by blowing the crude Aroclor with dry air. Vacuum trouble on the stills is usually caused by flashing of product, air leaks, plugged vacuum lines, or improper functioning of the vacuum jets. Flashing can usually be stopped by operating the still at a slower rate or increasing the flow of cooling water to the vapor condenser. Vacuum trouble can be traced systematically from the jets and usually ieolated. High color and entrainment will result from overheating (around 25*C. ; above normal distillation temperature) Aroclor , faulty operation of the distillation step, or boiling down the still too far, (Tars will carry over). The "tail - end" still fraction (tars) is a possible source of unstable Aroclors. company confidential TRAN 009221 HARTOLDMON0026617 Dept, 246 - Proeeii Description 12. AROCLOR SECTION IV COMMENTS ON PROCESS BLENDING AND FILTRATION Attapulgus Earth it added in the blend tanks to reduce moisture and inorganic chlorides as well as improve electrical properties. If batches do not meet specification (See Appendix B), redistillation may be necessary. The Attapulgus Earth is roasted for 4 hours at 250*C, before addition to the blend tanks, COMPANY CONFIDENTIAL TRAN 009222 HARTOLDMON0026618 Dept. 246 Proeen Description 13. AROCLOR APPENDIX A EQUIPMENT LIST This section contains an equipment list with each piece of equipment listed by Item Numbers in a consecutive numerical sequence. Miscellaneous items of Dept, 246 such as Instruments have not been assigned Item Num bers. Equipment without Item Numbers is not included in this equipment list. All equipment of Dept, 246 will have Itejm Numbers assigned some time in the future. This equipment list should be expanded as additional Item Numbers are assigned. Item No, Equipment Name Equipment Number Description 2 01 Biphenyl Transfer 19-0582 Pump 66-3930 Taber vertical submerged cent, pump, sire C"3, 2 1/2" inlet, 2" outlet. Connection bronre except shaft which is monel. Motor is 3 HP, 1800 RPM. 102 Biphenyl Storage 21 -2210 Tank Tank purchased from Rogers and Wrigler. Capacity is 25, 000 gallons. 10" 6" DIA x 40' 6" long. 3/8" plate shell. Design pressure is 50 p6i. 103 Biphenyl Head 21-0767 Tank 16-7225 Tank made by Graver. Dwg. C-799. Steel tank 4' 6" ID x 51 611 str. side, dished heads, shell 3/8", top head 3/8", and bottom head 3/4" with 1/2" jacket over it and ending 9" up on tank side . Welded throu ghout. Test of tank is 60# and jacket is 105# hydro, pressure. Mixer i6 Mixco Model N33G75, gear driven propeller. Motor is 440/3/60 TEFC, 1725 RPM. 104 Biphenyl Feed 66-7224 Durco Horiz. Cent) pump. 2" inlet, 2" outlet. Cap. 100 GPM Motor is 7 1/2 HP, 1760 RPM 205 Chlorinator #1 21-3261 Tank made by Nooter. Dwg. E-880. 3* ID x 16' long with pig. head. Shell 3/8" and head 7/16" thick, 3/16" jacket over lower half of tank. . 106 - Chlorinator #2 21-3245 Same as Item No. 105. COMPANY CONFIDENTIAL TRAN 00,223 HARTOLDMONOQ26619 Dept, 246 - Process Description AROCLOR APPENDIX A EQUIPMENT LIST (Cont'd.) Item No. 107 108 Equipment Name Equipment Number Chlorinator 21-5251 #3 Chlorinator 21-1283 #4 Description Tank made by Leader Iron Works. Otherwise, same as Item No. 105. Same as Item No. 107. 109 Chlorinator 21-1432 Same as Item No. 107 110 #1 Mist 15-0581 Eliminator 111 H2 Mist 15-0582 Eliminator 112 #3 Mist 15-0583 Eliminator 113 #4 Mist 15-0584 Eliminator 114 tf5 Mist 15-0586 Eliminator 115 Chlorine Mist 21-4042 Eliminator 116 Chlorine . 38-5487 Vaporizer ' 120 Knockout 121 Chlorinator 19-4305 #1 Pump 66-8109 . Tank made of carbon steel. Element made or carbon steel. Design pressure is 50 psig. and design temperature is 300CF. Same as Item No. 110. Same as Item No. 110. Same as Item No. 110. Same as Item No. 110. Tank made by Alpha. Carbon steel construction. Coded tank. Element 316 stainless steel. 15" Dia, glass fiber inverted type. Design pressure is 50 psig and design temperature is 300F. Chlorine vaporizer made by Armstrong Company. 8 5/8" OD x 111 long. Carbon steel construction. Chlorine side designed for 250 psig. at 400F. Steam side designed for 100 psig at 400F. Steel vertical 60 gal. tank. Durco Mark II horiz. cent. pump. Inlet Is 3" and outlet is 2", ductile iron, with Durametalllc seal and Manzel lubricator. Rate is 200 OPM at 25' static head Sp. Or, of 1.5* Motor is 10 HP, 1800 RPM. COMPANY CONFIDENTIAL TRAN 009224 HARTOLDMON0026620 Dept. 246 - Process Description 15. AROCLOR APPENDIX A EQUIPMENT LIST (Cont'd.) Item Equipment No. Name Equipment Number Description 122 Chlorinator 19-4506 *02 Pump 66-8110 Same as Item No. 121. 125 Chlorinator 19-4507 #5 Pump 66-8111 124 Chlorinator 19-4508 #4 Pump 66-8112 Same as Item No. 121. Same as Item No. 121. 125 Chlorinator 69-5892 Same as Item No.121. #5 Pump 66-6509 ... 126 Blow Tank 21-2086 #2 Tank made by Graver. Dwg. E-865. 7' Die x 7' str. sides, dished heads 1/2", Shell 5/8", 5 turn coil of 2" pipe sup. ported on brackets welded. 127 Blow Tank 66-2956 #2 Pump 69-0577 Taber horiz. cent. pump. Type L-2. 2y" x 2". Semi-steel with monel shaft and water jacketed stuffing box. At 20' static head, rate is 80 0PM, 1.5 Sp. Or. at 5O0F. Motor is 5 HP, 1800 RPM. 128 Air Dryer 14-0104 Anders lykens Corp. Air dehydrator. Two code welded tanks filled with 55 llz activated alumina. Dwg. *06456. 129 Blow Tank 19-0629 #1 Pump 66-9080 . Same as Item No. 127, 150 Still *01 20-0045 .1 Vacuum still purchased from Graver. Dwg. C-809. Size 6' Dia. x 5'6" lg. on str. side, shell, dished head 5/8". 60*0 hydro, pressure test. 151 Furnace #1 27-0045 Steel heater furnace. Steel shell 5/1* x 5'9" Dia. x 4* 10i" lg. lined with insulating fire brick. One coil 2" xHj pipe, 12 turns formed into a 2' Dia coil with spare blocks and legs. Dwg. E-886. 152 Still *01 Pump 19-0594 66-4891 COMPANY CONFIDENTIAL Taber vert. sub. cent. pump, type L-2. Casing, yoke, and Impeller made of steel. 2" inlet and 2" outlet. Length 7' 9". Capacity is 75 0PM., static heat 15', Sp. Or. 1.8 at 700F. Motor is 5 HP., 1750 RPM. TRAN 009225 HARTOLDMON0026621 10. Dept. 246 - Process Description AROCLOR APPENDIX A Item No. Equipment Name EQUIPMENT LIST (Cont'd. ) Equipment Numbe r Description 133 Still #2 20-0062 Vacuum still purchased from Noote r. Dwg, 6944. 6J ID x 11' 10" str. shell, internal pipes, standard dished heads. Glass wool insulation 3" with 1/2" finished coat. 134 ' 135 Furnace #2 Still #2 Pump 20-0066 66-1759 69-1277 Same as Item No, 131. Taber vertical sub. cent. pump. Type CL-4, 2 1/2 X 2", size 384. Pump is dynamo steel. Capacity is 75 CPM at 25' static head, Sp. Gr. 1.8. Motor is 7 1/2 HP, 1750 RPM. 136 Condenser #1 38-0770 Heat exchanger, made by Nooter. Dwg. B-651. 12" DIA 5' long having nineteen 2" O. D. 11 ga. monel tube6, monel tube sheets, monel reducer, and carbon steel jacket and back up ring6 on flanges 137 Condenser #2 38-1378 Same as Item No. 136. 138 Receiver Tank #1 21-0771 Vacuum receiver tank made by Nooter. Dwg. C-795. Size is 5' 6" D1A x 5' 6" str. side, 3/8" shell, 1/2" bottom and removable head. 2" IP, size xHy monel coil with 2" inlet and 1" outlet. 3 turns, 5* D1A along side and 3 turns spiral on bottom. 60# hydro, pressure test on tank and 300# on coil. 139 Receiver Tank #2 21-1377 Tank made by Nooter. Dwg. C-795. Same as Item No. 138. 140 Receiver Pump #1 66-9067 Blackmer pump. Type PA-50L, bronze 69-0565 rotary pump, monel shaft, C.l, base. Capacity is 50 GPM, 1.65 Sp. Gr, , 350 to 500 *F. Motor is 2 HP, 1740 RPM. 141 Receiver Pump #2 66-5670 Same as Item No. 140, 69-1258 COMPANY CONFIDENTIAL TRAN 009226 HARTOLDMON0026622 Dept, 246 - Process Description 17. AROCLOR APPENDIX A EQUIPMENT LIST (Cont'd.) Item Equipment No. Name Equipment Number Description ,142 Blend Tank 21-0779 #1 Tank made by Graver. Dwg. E-862. Welded steel tank, 7* Dia. x 71 high, dished heads ", shell 3/8". All sur faces spraymd with .005" zinc then .003 tin. 2" xHy pipe coil and supports. Cage bronze stirrer and bronze shaft. Test of tank is 60# and coil is 300# hydro, pressure. 143 Blend Tank 21-1399 #2 66-0217 144 Blend Tank 19-1757 Pump 66-3718 Same as Item No. 142. Taber Horiz, Centrifugal pump. 304 s.s. 2" x l" capacity 60 GPM, 100' head. Motor is 10.0 HP, 1800 RPM. 1^5 36" Sparkler 15-0238 Filter Filter made by Sparkler Mfg. Co., 33-D12 horizontal plate filter. Type 304 s.s. Jacket tested for pressure of 30 psi. 146 Finished Product Tank #1 147 Finished Product Tank #2. 148 Storage Tank #3 21-0780 21-1400 21-0768 Filtrate receiver tank. Dwg. E-862. Same as Item No. l42, . Tank made by Nooter. Otherwise, same as Item No. 142. .* Tank made by Graver. Dwg, C-609. Horizontal steel, 101 Dia. x 2o' long on str. side, dished heads, shell i", head 9/16". Test of tank is 60# and coil is 300# hydro, pressure. All coils, supports, inside surface sprayed with .005'' zinc and .003" tin. 149 Storage Transfer Pump #3 19-0585 66-0853 Taber Vert. Sub. pump. Dwg. A-387. Type G~3, 2" x 2", C.I. body, length 11*6". Cap. 50 GPM, 60 static head, Sp. Or. 1.18 at 170F. Motor is 3 HP, 1800 RPM. 150 Storage Tank #4 21-0769 Same as Item No. 148, 151 Storage Transfer Pump #4 19-0584 66-1501 Taber Vert. Sub. Pump. Type L-2. 2|" x 2". Length 11'6". Cap 50 GPM at 40' static head. Motor is 3 HP, 1800 RPM COMPANY CONFIDENTIAL TRAN 009227 HARTOLDMON0026623 Dept. 246 - Process Description AROCLOR 18. APPENDIX A EQUIPMENT LIST (Contd. ) Item Equipment No. Name Equipment Number Description 152 Storage Tank 21-1510 Tank made by Leader Iron Works. Dwg. C-609. 10' OD x 26' Long on str. she Same as Item No. 148 for other characteristics. 155 Storage Transfer Pump #5 19-OQ29 66-0856 Same as Item No. 151, except length 1; 4'7". 154 Storage Tank #8 21-5526 Alpha tank 12'6" Dia. x 22' high. 20,000 gallon storage capacity. Aluminum constructed Dwg. TS-D-501X. 155 Storage Transfer Pump #8 19-5172 66-2651 Durco pump, model WH2 Alloy constr. 2' x l", 8" Impeller. Cap. 160 QPM at 55' head. Motor Is 7i HP, 1740 RPM. 156 Storage Tank fj 21-2404 Slpha tanlc. 15' O.D. x 20' high. Vertical tank, constructed of 5/8" mi: steel. Capacity Is 20,000 gallons. 157 Storage Transfer Pump in 19-2077 66-1691 Pump made by Blackmer. Monel shaft, 2i" x 2i". Cap. 90 QPM, 15' head. Motor is 5 HP, 1750 RPM. 158 Scales 24-0246 24-0187 Made by Toledo Scale Co. 800# capacity dial type scale. 167 Blow Tank 21-0750 #1 Tank.made by graver. Dwg. E-B65. 7' Dla. x 7' str. side, dished heads i", shell 5/8". 5 turn coil of 2" xHY pipe 169 Surge Tank 22-0751 Cyclone collector made by Graver. Dwg. B-695. 48" Dia. x 27" on str. side, 5' 6" long and tangential inlet near top of side. 5/18" steel throughout of walded construction. 170 City Water 69-1085 Pump #1 66-5565 Taber Horlz, pump, Model CB5, 5" x 2-' 9" impeller. Cap. 180 GPM, 50' head. Motor is 7i HP, 1800 RPM. 171 City Water 69-2078 Pump #2 66-1796 Same as Item No. 170 COD Exhaust Blower 11-0265 Made by American Blower Co. Type 450E. Capacity is 6408 SCFM at 1510 RPM. Dwc E-10699. Motor is 15 HP. COMPANY CONFIDENTIAL TRAN 009228 HARTOLDMON0026624 Dept. 246 - Prooess Description 19. AROCLOR APPENDIX A EQUIPMENT LIST (Cont'd.) Item Equipment No. Name Equipment Number Description .185 186 Coke Scrubber 01 Coke Scrubber 02 21-0756 21-1396 Scrubber liquor tank made by Graver. Dwg. C-800. ^6" Dla. x 5'6Y' on Str. Side. Coil 3 turns of li" xHY pipe. Same as Item No. 185, 200 Cyclone Separator 21-1413 Separator made by Heintz Steel. 3' id 6' high tangential separator with integral vapor pipe complete. 201- Air-cooled Heat Exchanger 05 38-5528 Air-cooled heat exchanger made by Dialer. Cooling capacity is l,200,0OC Btu/hr. Steel construction except for aluminum fins. Fan motor is 2 HP, 1150 RPM. 203 Steam Vacuum 55-5523 Jet 01 264 Steam Vacuum 35-1686 Jet 02 #2 i Worthington 3-stage vacuum Jet. Same as Item No. 203. 205 Steam Vacuum 35-3533 Jet #3 206 Off-gas Drowning Jet 35-4756 3-stage porcelain Kubatl vacuum ejectc with 10" ID porcelain condenser. Jet has a capacity of 10#/hr. air at standard conditions. Jet designed for 150# steam and 2 mm Hg absolute. Made by Schutte-Koertig. 8" Haveg fum< scrubber. Complete with standard nozzle. 207 Drying oven 14-0138 210 211 212 213 Air-cooled Heat Ex changer 01 Air-cooled Heat Ex changer 02 Air-cooled Heat Ex changer #3 Air-cooled Heat Ex changer 0k 38-5564 66-8113 38-5566 66-8115 tl:?& Qrieve Hendry drying oven, 44o V,, 3 phase, 60 cycle, manual reset temp. controller range 0-4Q0C. 3: Same as Item No. 201. Same as Item No. 201. <m Same as Item No. 201. Same as Item No. 201. o TRAN 009229 HARTOLDMON0026625 Dept. 246 - process Description 20. AROOLPR APPENDIX A EQUIPMENT LIST (Qont'd.) Item No. None Equipment Name Chlorine Pressure Recorder Equipment Number 29-1547 Description Made by Taylor Instrument Co. Pressure Recorder with 2 pens. Cat. No. X176JF235. Range 0-100 v None #5 Chlorinator Flow Recorder 29-2019 Made by Taylor Instrument Co. Plow Recorder - Controller. Cat. No. 137RF135. . 12" chart, 0 to 10 Sq. root chart. None Water Meter 29-2486 Made by Worthington Corporatlo 3" model IH turbine type water meter. None #1 Still Tempera ture Recorder 29-3885 Made by Leeds & Northrup Co. Temperature Recorder. Range 0 - 400C. None #1 Still Absolute 29-1170 Pressure Controller Made by Taylor Instrument Co. Absolute pressure Reoorder - Controller. None None 200# Steam Flow Recorder 29-0835 #2 Still Absolute 29-3353 Pressure Controller Made by Bailey Meter Company. Flow .Recorder. Made by Taylor Instrument Co. Absolute Pressure Recorder Controller. None None #2 Still 29-024** Temperature Recorder #2 Still Level Controller 29-1463 t. Made by Leeds & Northrup Co. ' 6 point Temperature Recorder. Made by Taylor Instrument Co. Liquid Level Recorder - Controller. None None Chlorinator 29-0288 Temperature Recorder #1 Blow Tank 29-291$ Temperature Recorder Made by Leeds & Northrup Co. 12 point Temperature Recorder. Made by Taylor Instrument Co. Temperature Recorder Controlle Adjusts 200# steam to #1 Blow Tank Cat. #86 RM43185-12. COMPANY CONFIDENTIAL . TRAN 009230 HARTOLDMONOQ26626 Dept. 2^6 - Process Description 21. AROCLOR APPENDIX A Item No. Equipment Name None 80# Steam Flow Recorder None 200# Steam Flow Recorder EQUIPMENT LIST (Cont'd.) Equipment Number ,r Description 29-5A52 Made by Foxboro Company. Type TJ7, recording flow meter with integrator and indicator. Meter body 3l6 S.S. Integrator for 80#, *fOOF. Steam. 29-5^52 Made by Foxboro Company. Type T57 Recording Flow meter with integrator and indicator. Meter body 316 S.S. Integrato for 200#, 510F. Steam. COMPANY CONFIDENTIAL TRAN 009231 HARTOLDMON0026627 i I Dept. 246 - Process Description AROCLOR 22. APPENDIX B , SPECIFICATIONS The folliwing is a list of the raw materials used for the manufacture of Aroclors. Specification sheets are Included w..ere they exist. Material Code Raw Material 82601 ............................................................. Biphenyl 35500 ............................................................. Ferric Chloride 38800............................................................. Lime 19400................................................................ Attapulgus Earth 81059 ............................................................. Chlorine 43099 ............................................................. Nitrogen The following is a list of the finished products manufactured in department 246. Specification sneets are included where they exist. Product Code Product MCS 295 Aroclor 1254-10^ Xylene Aroclor 1232 81101 (Electrical & Non-Electrical) Aroclor 1242 81102 (Electrical & Non-Electrical) Aroclor 1248 81103 (Electrical & Non-Electrical) Aroclor 1254 81105 (Electrical & Non-Electrical) Aroclor 1260 81107 Aroclor 1262 81101-81102 (Mix) 1242 - 1248 Mix ' 82868 Montars 1,2,3 and 4. ~ COMPANY I CONFIDENTIAL TRAN 009232 HARTOLDMON0026628 OftOANIC CMtMCAL* MVIAION SPECIFICATION WATCRIAL DIPHENYL (BIPHENYL) CHIMICAL FORMULA MINO DtFTA. 246 AUFFLUR ANNISTON PLANT MOt -t. 154.20 . tv+gymou ipici op oo AMPL POO AMALVtlt 2 x 16 oz. V.M.Bottles UNRESTRICTED INFORMATION Routine Tests Property Appearance and color Crystallizing Point GENERAL INFORMATION Distillation Range: First Drop to Dry Point Specification Light Yellow "Cryat. Solid 68.7*C, min. 2.5C, max. Must include 255*0 within Range Issued 6/9/61 W.O.Krummrlch Plant By If Method Number ---------------- 10,252 - 10,298 10,299 I Thii specification Is the property of Monsanto Chemical Company and Is for Internal use only. COMPANY CONFIDENTIAL __________________________________________ fTI NM <v. IA/MI TRAN 009233 HARTOLDMONOQ26629 ' MONSANTO CHEMICAL COMPANY OHOAMC CHIMC&Lt DIVISION W. Q. Krummrlch Plant FINISHED PRODUCT SPECIFICATION PHOOUCT COOH 810SQ USB Internal BALES CODE PRODUCT fYVeJe kmae) TTP Chlorine (Snift .QasJ.__ PHODUCT (Gbmtiml TYPE 0P*T. OR JOS 252 CHEMICAL POHMULA Mixture ML WT. M*L AMPLE POH ANALTMt 100 c ,c, Oas Burette Issued DEC 23 W Wbv. _Q%K.rummrlch Plant RAW iv;ate;;,.\L Dale App.0vi:dPA9.?.?..l^?_ For Dept UNCLASSIFIED INFORMATION Oeneral Tests (made only on request) Property Typical Analyses Chlorine (Clg) Oxygen (0g) Carbon Dioxide (C02) 86$ By Volume 5$ " 1.5$ " 11 Carbon Monoxide (CO) Hydrogen .(H2) 0.1$ " 1.0$ " 11 II Inert Oases (By difference) 8.4$ " n Moisture (H20) @ Std. Conditions Direct pipeline transfers to using Depts. 9 255, 2?6, 257, 246 This specification Is for internal use at WQK Plant only. Method'Number fD IN IUV. U/Mt COMPANY CONFIDENTIAL TRAN 009234 HARTOLDMON0026630 HORSANTO CHEMICAL COMPART. wrrvr-ssswoTO.nt RAW MATERIAL SPECIFICATION MIWIU COOK 38BOO_ uwa MMb 222. 246 vrrw(BR MATHHAL POMWl* Ca (OH)i Mb rr. IVfUIIDII IMU BP UWLI POM AMALVIII ._ Iesucd 6/20/6^ . V. 0. arummrich Plant By M. D. Dealv UNCLASSIFIED INFORMATION general Teafee (made only on request) .' Property . Specification Method Number Appearance Fine white or slightly gray powder, free from lumps or gritty material 10,188 Assay (ca(OH)t) . Carbonates as (CtOO) Magnesium ' Sulfates (as 80s ) . 92.00^, mln . ' ?*00$, max. 0.50, max. 0.J0, max. . . 10,191 . 10,19? 10,192 10,189 m lx imv. /*> ZZL I TRAN 009235 HARTOLDMON0026631 W. G. Krummrlch Plant MONSANTO CHEMICAL COMPANY WtMC C MIMIC M.* WVIIWH RAW MATERIAL SPECIFICATION MATBRIAk COOS 33500 WIN* MAT*. UAPLII* MATCBIAL _____Ferric Chloride Anhydride CHf MIC At POftMULA T. 162.21 IVMMIPM ac* *r 2/26/57 Fe Cl lAMPkl FOR ANALYIII 3 X 8 02. w. M. Bottle UNRESTRICTED INFORMATION General Tests (made only on request) Property Specification Appearance Black pov>dcr or granules Assay 97*0^, min. Sulfates 0.0556, max. Ferrous Salts Trace, max. Solubility; 10:10 of Water Complete to slightly turbid, max. 30:10 of Formula JO ale ohol Complete to slightly turbid, max. Issued 11/15/62 W. CL. Krurpmrich Plant J.F.Q. Method No l6-A 22-570 120-570 S-570-1 112-D & M M M(y. Il/Ml COMPANY CONFIDENTIAL TRAN 009236 HARTOLDMON0026632 pontine Tests Property . . . Volatile Matter {at 950*c). Hfe^'^et! " . .; . : .Through,VSS ?t5 . .. ' . Specification 6> ;8^, . . . . * ' 9^e min. ' . Method Number f ' - --V ,, This material is not aooOpted without the supplier's analysis of the above properties.,. " ' . ; - . o JM M liy, MSMI company CONFIDENTIAL TRAN 009237 1 u HARTOLDMON0026633 MOKSAKTO CHEMICAL COMPAHY PRODUCT COOK 81115 ORKAMIC CMERSC ACS DIVISION W. 0. Krummrich Plan USE ' Internal FINISHED PRODUCT SAC SS CODE SPECIFICATION JDKPT. OR JO* 1 ?U6 J.P.O. PRODUCT (Trad. Hamt) TTPK Aroclor 1232 (MCS - 236) PROOUCT (CAanlul TTPK 32^ Chlorinated Biphenyl CHI Ml CAL fOHMULA issued APR 7 1964 W. Q^Uc^ww^eh yiarTC MOL Wt. IWTIRKOII tries or New ' * A*fLI PW ANALTAII 2 X 16 02. w. M. BottleJL Routine Tests Appearance Sp. Cr. @25/15.5*0 Acid Number Color, APHA HgO General Tests Chlorine Specification Clear Liquid 1.266 - 1.276 0.014 mg. KOH/grm. max. 100, max. 55 ppm., max. 51.5 - 52.5* Method No. 10,114 10,087 10,084 10,620 This specification Is for internal use only. n IN M IRKV* IK/SSI Company CONFIDENTIAL TRAN 009238 HARTOLDMON0026634 HONSARTO CHEMICAL COMPAHY ANNISTON AND KRUMMRICH FINISHED PRODUCT SPECIFICATION PRODUCT PRAODRUOCCTT(-CpRMaM3142 PMOUCTCOM USE SALES ACU COOK Alston 1256 - WOK Issued 1/24/62 ___ _ - W.O.Kruamrich Plant by E,0. Martin 104 0-130-04ft/p1*1/l6r0'?/0Q CRUDE COMMERCIAL tvpi CHS MIC AC PONMUCA ' MIXTURE MOC VT. --- ____ -- AMPCI PON ANACTili ... UNRESTRICTED INFORMATION Routine Tests ^jrf^M^Battle WOK Property Specification Method Number Appearance and Color Brown to black oily liquid Anniston ---- WOK 10,084 Specific Gravity 25/l5.5C 1.384 - I.394 14-49-54 10,114 Acid Number (mg. KOH/g.) 0.7# max. 14-46-54 11,552 RESTRICTED INFORMATION Acid Number of the crude, which is stored in non-lacquered metal containers shall be 0.2mg. KOH/g. max. HI IN M <NV. U/M) COMPANy CONFIDENTIAL TRAN 009239 HARTOLDMON0026635 MONSANTO CHEMICAL COMPANY 'bhwdek 8261! ANN. rw6K 1 27L ANN. KRUMMRICH and ANNISTON FINISHED PRODUCT SPECIFICATION USE r.o 3 e s SALES COOE 1040-240-04/11/16-05/09 PROOUet Nam*/ TTPI AROCLOR 3242 ELECTRICAL GRADE (PYRANOL 1499) mme)PROOUCT (Cham)**, TtPK CHEMICAL FORMULA Mixture f Issued 4/15/62 W.0.Krummrlch Plant By 0< O* Trt **AL MOL WT. --- ^17/61 AMPLE POP ANALYSIS 5x5 pt. Amber Bottles UNRESTRICTED INFORMATION Routine Tests Property Specification Method Number WOK ANNISTON Color (APHA) Condition Sp. Or. @ 25/15.5C Acidity (mg. KOH/g.) Moisture (HgO) Refractive Index @ 25C Inorganic (Free) Chlorides Pour Point Dielectric Constant (3000 cycles @ 100C) Resistivity (500 VDC 9 100C 0.1" GAP) AS OHM-CM x 109 Hydrolysis Stability Test (As Chlorides) Monsanto Stability Test (As Chlorides) Distillation Range (ASTM D-20, Corrected) 100 Distilled by wt. 90^ Distilled by wt. 50, max. Clear 1.581-1.592 0.010, max. 55 ppm., max. 1.6240-1.6260 0.05 ppm., max. -14 C or Lower 4.70-4.90 500, min. 1.0 ppm., max. 0.4 ppm., max. 525C, min. 560C, max. 10,084 10,084 10,114 10,087 10,620 10,125 T-2092 10,115 11,608 11,607 14-44-54 0-1 14-49-54 14-42-54 14-55-54 3 4-54-54 014 14-47-54 ' 14-56-54 14-55-57 T-2087 11,505 10,117 010 14-61-57 14-51-54 GENERAL TESTS (Made only on request) Sulfates Dielectric Strength S 25C Flash Point (F) Fire Point Viscosity 9 100*F (SUS) Corrosion Test (6 hrs S 210C with bright aluminum foil) Change in wt. of AL {%) None 12,169 55 KV, min. 11,605 558-592 None 10,125 10,125 82-92 10,086 10,126 COMPANY 0.0 CONFIDENTIAL ee 045 14-28-54 14-28-54 14-4-52 14-55-57 (Over) TRAN 009240 CZ1 *N M (REV. M/M) HARTOLDMON0026636 A.C. A.C. A.C. A.C. Color (APHA) Condition Acidity (mg. KOH/g.) Inorganic(Free)Chloridea GENERAL INFORMATION . Specific Heat 3 25C Coefficient of Expansion (25-65C) Fixed Chlorine SPECIAL CUSTOMER REQUIREMENT General Electric Hydrolysis Stability Test (As Chlorides) Thermal Chemical Chlorides 60, max, Clear 0.010, max. 0.05 ppm., max. O.JO 0.00068 cc/C 42.5-45.5jC 0.5 ppm., max. , O.75 ppm., max. 10,084 10,084 10,087 T-2092 1ij.44.54 0-1 14-42-54 014 T-2087 12,722 010 COMPANY CONFIDENTIAL TRAN 009241 HARTOLDMON0026637 MONSANTO CHEMICAL COMPANY MtAMC CHCMCAL* DIVISION Krummrich and Anniston FINISHED PRODUCT SPECIFICATION fAOOUCT (Tm* Htmt) Aroclor 1248 MlOPWCt (OwaM Hmme) fHOOUCT CODK 81102 - 82641 USB Sales otfT. on jos WOK 246-Ann.27 Issued__ JUL 1 5 1964 W. 0. fruffiTeF^FT&KT~ By ^ O __ itiu cods 1040-260-04/ll/l6-03/09 TTf 1 _____ Mon-Elec tribal 0 rade______ Tn (MvietL p&mmjL& moLjrr.___________ wmmidu tftei or 8-4-61 Mixture Aim fON ANALVMI 3 _x_l6_az. W.M,-Bottles UNRESTRICTED INFORMATION Routine Tests Appearance Condition Color, APHA Sp. Or. 965/15.5*C Acidity (mg. KOH/g.) Moisture (HgO) (ppm.) Viscosity 9130*F (SUS) General Tests Flash Point (*f) Specification Colorless to light yellow-green liquid Clear 100 max. 1.405 - 1.415 0.010, max. 50, max. ' 73-80 370, min. WOK Anniston Method'Uo. 10084 0-1 10084 10084 10114 10087 10620 10086 0-1 046 052 050 047 049 10123 14-28-54 COMPANY CONFIDENTIAL TRAN 009242 HARTOLDMON0026638 ' BOWAItTO CHEMICAL COMTAHY MWMt mmmms ffiWMC? CH 81102 | 1 27 Ann. Kffl SPECIFICATION Sales ' 1040-260-04/ll/l6-05/09 immvet . . tffB Aroolor 1248 Electrical Grade (Prranol 1498) (nM TTP* SMMeAli It.ued 1/10/611 Corrected 2-16-64 * Mixture wramiNi *se of 2-12-60 MW>t.g m AMAkvau ------ 5 x 5 Pt. Amber Bottles UNRESTRICTED INFORMATION Routine Tests 'Specification Method No*s WQK Annlsto Color, APHA Condition Sp. Or. 65/15.5*0 Acidity (mg. KOH/gm,) Moisture Refractive Index #25*0 Inorganics (Free) Chlorides Pour Point Dielectric Constant (1000 cycles #100*0) Resistivity (500 VDC l00*Cr.0,lM OAF) as OHM-CM x 10^ Hydrolysis Stability Test (as Chlorides ) Monsanto stability Test (as Chlorides) instillation Range ' (ASTM D-20, corrected) 10* Distilled by Wt. 90$ Distilled by Wt. 50, max. Clear 1.405 - 1.415 0.010, max. 55 ppm., max. 1.6285 - 1.6505 0.05 ppm., max. 0*C, max. 4.5 - 4.7 500, min. 1.0 ppm., max. 0.5 ppm., nx. 345*0, Bln. 385*0, max, '.General Tests (made only on request) 10,084 14-44-5 * 10,084 0-1 10,114 14-49-5 10,087 14-42-5 10,620 14-55-5 10,125 14-54-5' T-2092 014 " 10,115 14-27-51 11,608 14-56-51 11,607 14-55-51 T-2087 010 11,505 14-61-57 10,117 14-31-54 Sulfates Dieleotrio Strength 925*0 Fire Point 4 Viscosity #54.4*C (SUS) Corrosion Test (6 hr. 210*C with bright aluminum foil) Change in wt. of A1 (%) ( Mono 35 KV, Bln. None to boiling point 75-80 12,169 - - 11,605 043 10.125 14-28-54 10,086 14-4-52 10.126 14-55-57 COMPANY CONFIDENTIAL (over) TRAN 0092*3 T * I m M tt/MI HARTOLDMON0026639 A. C. Color, APHA A. 0. Condition A. C. Acidity (mg. KOH/g.) A. C. Inorganic (Free) Chloridea 60, max. Clear 0.010, max. 0.05 ppm., max. 0ENERAL INFORMATION t Specific Heat 25*C Fixed Chlorine 0.27 47.5 - 48.5% 10,084 14-44-54 10,084 0-1 10,087 14-42-54 10,118 010 COMPANY CONFIDENTIAL TRAN 009244 HARTOLDMON0026640 MONSANTO CHEMICAL COMPANY MltMC CMKCtU WYIIWN Krummrich and Anniston PRODUCT CODE 81103 - 82613 USE Sales DEPT. ON JOS W0K-246-Ann.27 Issued JUL 1 5 1964 W. 0 . Krummrich Plarit By_ -`ft Ti V < FINISHED PRODUCT ALU CODE SPECIFICATION 10M 0-280-04/11/16-03/09 PMOOUCT (TrMb HmJ ' TYPE ' Aroclor 1254 paoduct Non-Electrical Grade ' TYPE CHEMICAL POMMULA Mixture ML *T. WPIMINI IPIM OP *i-4-6l SAMPLE POM ANALYSIS 3,, a_ 16.oz4_j>L_JL_J3am^____ _ UNRESTRICTED INFORMATION Routine Tests Color, APHA Sp. Or. 65/15.5*0 Acidity (mg. KOH/g.) Moisture (H20) (ppm.) Oeneral Tests Flash Point Viscosity 210*F (SUS) Specification 100, max. 1.495 - 1.505 0.010, max. 50, max. None 44-48 , WOK Anniston Method' No. 10084 10114 10087 10620 046 052 050 . 047 10123 10086 14-28-54 049 COMPANY CONFIDENTIAL TRAN 009245 HARTOLDMON0026641 . aOKSAJTTO CHEMICAL COMPAfT rmm*. Issued 4/13/62 Sales M. 0. Krummrich Plant By E. 0. Martin SPECIFICATION 1040-280-04/11/16-03/09 weowt ft** . rr* AROCLOR 1254 1JZCTRICAL GRADE (PfRAMOL l4?6) ' ?WI (MHKU n*IML* , Mixture MDLVf, -- evnnpu jg* #r 10/10/61 TORESTRICTKD INFORMATION Routine Tssts . Property .. l re* ? x 5 pt, Anber Bottles 8pi3i?ISaHn Color, APHA . Condition Bp* Or. 0 65/13.5.*C AojLdlty (ag. XOH/ga.) Molitur (H*0) Refraetiv Index 25C Inorganio (Free) Chlorides Pour Point Dieleotrio Constant (1000 oyoles 100*C) Resistivity ' (500 VDC 100 C 0.1 OAP) ms OHM-CM x IQ9 Hydrolysis Stability Test (As Chlorides) Monsanto Stability Test (As Chlorides) . Distillation Range (ASTM D-20, Correoted) fyOfl Distilled by Vt. 50^ Distilled by*Wt. 90* Distilled by Vt. 50,' Max. Clsar I.495-I.505 0;010, aax. 35 W,' ar. I.6370-I.6390 0.05 ppa., aax. 7-12*C ` 4.15-4.35 500, min. 1.0 ppm., stax. 0.5 ppa,-, aax. QmmAL TESTS (Mads only on request) OTifate* ' Dlslsstrio Strength 25*0 PXbsh point Fire Point % Yleoeslty 210F (SUS) Corrosion Tsst ( hr* 210C with bright aluminum foil) Cl^nge in et. of A1 {%) Mon 55 KV, min, Hons lent 44-48 0.0 (Oyer) PiiMi COMPANY CONFIDENTIAL Method Humber VOX ANNISTON 10,084 10,084 10.114 10,087 10,620 10,125 T-2092 10.115 11,60B 14-44-54 0-1 14-49-54 14-42-54 14-53-54 14-34-54 014 14-27-54 14-36-54 11,607 14-35-57 T-2087 11,503 10,117 010 14-61-57 14-31-54 02.169 U^j605 10,123 10,123 10,086 10,126 043 * l4-2&~5\ ir-2ar5^ 14-4-52 14-55-57 TRAN 009246 HARTOLDMON0026642 *. * A.C. Color, APHA A.C. Condition A.C. Acidity (mg. KOH/g.) A.C. Inorganic(Pr)chlorld* ICTSIKAL SPBCIPICATIOK Cornell - publiler . Resistivity ' (500 VDC 100*C 0.1" CAP as OHM-CM X lo") OPISRAL IKP0RHATI0H Speolflo Heat 25*C Coefficient of Expansion (25-65'C) Fixed Chlorine 60, max. 10,084 Clear ' . 10,084 O.OlOi'Isax.'io,087 0.05 ppm*, max. 10,118 2500, min. 11,607 .*? "* 0.00066 oe/*C 54.5-55.5^ o-i 14-48-54 010 14-55-54 COMPANY CONFIDENTIAL TRAN 009247 ! HARTOLDMON0026643 M0KSANT0 CHEMICAL COMPANY ORRAMIC CHEW CALI DIVISION ANNISTON AND KRUMMRICH FINISHED PRODUCT SPECIFICATION PROOUd AROn.nR 1 ]6n PRODUCT (OMlul IMI| PRODUCT CODE DEPT. OR JO SALES IALU COD* ftp* CRUDE COMMERCTAT, TTPE CHEMICAL FORMULA . MIXTURE 1 Issued 1/24/62 .0.Krummrich Plant ^y__ KOI T. - - EUPERAEOE*PEC* OP 3/28/58 _____ ___ IAMPLE rOH ANALYSIS . Anniston: 2 x J.6 __ UNRESTRICTED INFORMATION Routine Tests Property Appearance and Color Specific Gravity 90Vl5.5eC Acid Number (mg. KOH/g.) Specification Brown to black viscous sticky mass 1.558 - 1.569 0.7, max. Method Number Anniston WOK 10,084 14.49-54 14-46-54 10,114 11,532 RESTRICTED INFORMATION ** Acid Number of the e^nde, which is stored in non"lacquered metal containers shall be 0.2 mg. KOH/g., max. o in mv. ii/hi COMPANY CONFIDENTIAL TRAN 009248 HARTOLDMON0026644 KONSANTO CHEMICAL COMPANY ORAA MIC CHEMICALS DIVISION Krummrich and Anniston FINISHED PRODUCT SPECIFICATION PROD-.CT (DM* Hmm> Aroclor 1260 PRODUCT (CMbIhI nmmt) PRODUCT CODE DEPT. OR JOS 8llQ5_._-J.26l 4 WOK 246 Ann.27 uta Salejg sales code 1040-290-04/ll/l6-OV09 TYPE Non-Electric Grade___________ TYPE CHEMICAL FORMULA Mixture MOL *T. OF 5rir..^L AMPLE FOR ANALYSIS 3- x .iSuo^Ji^.M^-Balt2aiL UNRESTRICTED INFORMATION Routine Teste Condition Color, APHA Sp. Or. 90/15.5*0 Acidity (mg. KOH/g.) Moisture (Hg0) (ppm.) Viscosity 210*F (SUS) General Tests Flash Point Fire Point Specification Clear 150, max. 1.555 - 1.566 0.014, max. 50, max. 72-78 None None WOK Annistc Metnoa No. 10084 . 10084 10114 10087 10620 10086 0-1 046 052 . 050 047 049 10125 10125 14-28-5 14-28-5 m IN M IREV. IS/SSI COMPANY CONFIDENTIAL HARTOLDMON0026645 MONSANTO CHEMICAL COMPANY mw S^Ann. MtliC C MM CAL* WIIMW ilios - way Anniston and Krumrarich Plants UM FINISHED PHODUCT Sales SPECIFICATION (ALU ettOt 1040-290-04/11/16/-05/09 r (TvmOs Hem) AROCLOR 1260 TTPt ELECTRICAL GRADE NMtUCT fOtmmimi &me) (FYRANOL 1482) tWMCtL PONMULA Mixture Issued 2/7/62 W.Q.Xrummrich Plant By f, mu. m. -- 5/26/58 (AMPLC POM ANALVitl 5 x 5 pt. Amber Bottles UNRESTRICTED INFORMATION Routine Tests Property Specification Color (APHA) Condition Specific Gravity 8 90/l5.5*C Acidity (mg KOH/g.) Moisture (HgO) (ppm,) Viscosity 9 210*F (SUS) Refractive Index 9 25C inorganic (Free) Chlorides Pour Point (*c) Distillation Range (ASTM D-20,.Corrected) 10$ Distilled by wt, 50$ Distilled by wt, 90$ Distilled by wt. Corrosion Test (6 hrs. 9 210*C with bright aluminum foil) Change in weight of A1 ($) A,C. Color (APHA) A.C. Condition ' A.C. Acidity (ag.KOH/g.) A.C. Inorganio (Free) Chlorides 150, max. Clear 1.555-1.566 0.014, max. 55 max. 72-78 1.6455-1.6470 No detectable amt. 25-54 585-598*0 590-404*0 400-420*C 0.0 , 150, max. Clear 0.014, max. No detectable amt. (Over) Method No. WOK --Anniston 10,084 10,084 10,114 10,087 10,620 10,086 10,125 10,118 10,115 10,117 14-44-54 14-49-54 14-42-54 14-55-54 14- 4-52 14-54-54 14-48-57 14-47-54 14-51-54 10,126 14-55-57 10,084 10,084 10,087 10,118 14-44-54 14-42-54 14-48-57 n IN M (HIV. U/WI COMPANY CONFIDENTIAL TRAN 009250 HARTOLDMON0026646 UNRESTRICTED INFORMATION (oont'd) Property Specification Oener&l Tests (made only on request) Flash Point * None Fire Point 4 None Fixed Chlorine (%) Dielectric Strength f 50*G Resistivity 59.5-60.5 JO K.V., min. 500, min. (500 VDC 100*Co0.1" gap as ohra-cm. x 10) Dielectric Constant J.6-J.8 1000, eye les, 100*C Method Number MOK Anniston 10,12J 10,123 10,088 11,605 11.607 14*28-54 14*28-54 14-1J-54 14-J5-57 11.608 14-J6-45 RESTRICTED INFORMATION Monsanto Stability Test (As Chlorides in ppm.) 0.7; max. ll,50J 14*61-57 GENERAL INFORMATION Evaporation Loss after 6 hrs. 100*0 (*) 0.2, max. 10,116 14-J2-54 Stability test - after JO days at 100*0 in glass sealed in air No liberation of chlorine or chlorides COMPANY ' CONFIDENTIAL TRAN 009251 HARTOLDMON0026647 morjarto chemical compart OMAMC chimcau cxviiiom SPECIFICATION eeuT (r*mh> Mm**) AROCT/m 116? fkoouct roMiMi **> MPPycr eooi Iooft. m ^oa ,lf?o?:d8B * ___ Lsi2;6aPletori SALES ALU COOK Issued 1/24/62 W.Q.Krummrlch Plant by E.0. Martin 1040-170-0T4TF/K1 l/l-03/Q5______ __CRUDE COTMTFMKERCTAT. CMMCAI. FORMULA . MIXTURE ML T. - SUFKMKOM IF1CI OF 3/28/58 SAMFLl FOK AMALYBII 1 pt, can. Anniston; 2 x 1.6. os... W...M, .Bottles WQK UNRESTRICTED INFORMATION Routine Tests Property Appearance Color Specific Gravity @90/l55C Acid No. (mg. KOH/g.) Specification Viscous liquid Brown to black 1.577 - 1.587 0.7* max. Method Number Anniston WOK ---- 10,084 ---- 10,084 14-49-54 10,114 14-46-54 11*552 RESTRICTED INFORMATION Aoid No. of the erode which is stored in non-lacquered containers shall be 0.2 mg. KOH/g., max. m in m **. / COMPANY CONFIDENTIAL TRAN 009252 HARTOLDMON0026648 . MONSANTO CHEMICAL COMPANY M* ITKJffi Issued 1/24/62 . frMAMC CHCttCAU WVlitOK ANNISTON AND KRUMMRICH IM FINISHED PRODUCT SALES W.G.Krummrich Plant by E.O. Martin SPECIFICATION PMOOOCT (Tresth Itmao) AROCLOR DISTILLED PRODUCT (Onmlool Homo) 1040-300-04/11/16-0-5-00 TP 1262 TYP1 ... CHBM1CAL POMMOLA MOl. WT. - - - 3/28/58 MIXTURE AMPLK PON ANALYAW _2_x_l6-_gz^--M-j_________________________________________ __________________________________________ UNRESTRICTED INFORMATION Routine Tests j Property .1 ( Appearance Specification Viscous liquid Method Number 10,084 ! Color APHA 150, max. i Specific Gravity 9 90/15. 5*C 1.572 - 1.583 Acid No. (mg. KOH/g.) 0.014, max. j Viscosity @ 210F j 86 - 100 SUS GENERAL INFORMATION 10,084 10,114 10,087 10,086 Pour Point (ASTM) Distilling Range Total Chlorine Specific Gravity t coeff (85 - 130*C) 35 - 38C 390 - 425C 61.5 - 62.5* 0.001/C i CD ** M (MIV* /! COMPANY ' CONFIDENTIAL TRAN 009253 HARTOLDMON0026649 MONSANTO CHEMICAL COMPANY ORGANIC CHIMCAU DIVUIOM Krummrlch and Anniston FINISHED PRODUCT SPECIFICATION PftDOUCT COOK 82868 utc IALKI CODE See PRODUCT (Tt* Nmme) Montars 1 and PRODUCT (Chmti--I fimn*) _ PpAychl.orlnated Polyphenvls CHEMICAL FORMULA [DIPT. OR JOt IWOK 246 Ann,_j Sa les Below TYRE T TP Issued .Ml, W. 0wlTru By t 5 1964 Mixture fcOI. WT. _________ _______________________ ______________________________ IVI>lltllO(l tFIM Of" |a*MPLK POM ANALVftt 6-15-61' 2 X 16 ozx, s UNRESTRICTED INFORMATION Routine Tests Appearance General Information Specification Black Solid Anniston WOK WeTElod No. 14-17-52 11521 Physical Properties (Typical Values) Montar 1 Montar 2 Softening Point (ASTM E-28-51T) Acidity 5^-160`C Slightly Basic 70-170*C Slightly Basic Chlorine Content 56-112* 44-48* CaO Fe Benzene Insoluble Plash point 5-15% 0.5-1.0* 500-620*? 5-16* 0.5-1.0* 12.5* RESTRICTED INFORMATION Montars 1 and 2 are the still residues from distillation of Aroclors 1242 and 1248 respectively. Composition of these Montars Is not controlled, being entirely dependent on conditions required to make acceptable distilled product. Sales Code Nos. Montar 1 6405 - 001 - 04 - 05/09 Montar 2 6405 - 002 - 04 - 05/09 COMPANY CONFIDENTIAL TR*N 5* 94 <AEV. Il/ll) HARTOLDMONOQ26650 MONSANTO CHEMICAL COMPANY Oil AMC C HIM CALS DIVISION Krummrich and Anniston FINISHED PRODUCT SPECIFICATION PRODUCT COOI dipt, or jo* issued ju^51964 82868 WOK 246 Ann.27 W. o. Krujnmrich Plant USI By DtS L-L Sales SAL IS CDOI See Below PRODUCT (Trta. tat; Montars 5 and 4 PRODUCT (Ofuml--I Htm) Polychlorinated Polyphenyls TTPI WPS CMIMICAL FORMULA tmt nr.___________ lUMAMOft (Pica OP 6-15-61 Mixture AMPLI POM AMALVKB 2 x 16 oz. W. M. Bottles UNRESTRICTED INFORMATION Routine Tests Specification Anniston WOK Metho? No. Appearance Black Solid 14-17-52 11521 Oeneral Information Physical Properties (Typical Values) Montar 5 Montar 4 Softening Point (Method ASTM E28-51T) 86-l68C 92-206*C Acidity Slightly Basic Slightly Basic Chlorine Content 50-52* 54-56* CaO 5-10* 5-10* Fe 0.5-0.6* 0.5-1.0* RESTRICTED INFORMATION Montars 5 and 4 are the still residues from distillation of Aroclors 1254 and 1260 respectively. Composition of these Montars is not controlled, being entirely dependent on conditions required to make acceptable dis tilled product. Sales Code Nos. Montar 5 6405 - 005 - 04 - 05/09 Montar 4 6405 - 004 - 04 - 05/09 m IN M IRIV. M/((> COMPANY CONFIDENTIAL TRAN 009255 HARTOLDMON0026651 Dept-. 2^6 - Process Description AROCLOR APPENDIX 0 PHYSICAL AND CHEMICAL DATA 2>. COMPANY CONFIDENTIAL TIUM 009256 HARTOLDMON0026652 Dept. 246 - Process Description AROCLOR APPENDIX C PHYSICAL CONSTANTS 24 COMPANY CONFIDENTIAL GENERAL PHYSICAL PROPERTIES OF AROCLORS F orm............................................................ . Color............................................................ Aroclor 1242 Practically colorless mobile oil 100 Max. (APHA) Aroclor 1248 Aroclor 1254 Yellow tinted Light yellow mobile oil viscous oil 100 Max. (APHA) 150 Max. (ARIA) Aroclor 1260 Light yellow soft sticky resin 150 Max. (APHA) Aroclor 1262 Light yellow sticky clear resin 150 Max. (APHA) Acidity-Maximum (Mgm. KOH per Gnu ) 0. 015 0.015% 0.015 0.015 0.02 Average Coefficient of Expansion................................... cc/cc'C. 0. 00068 (25*-64*C) 0.00070 (25*-65*C) 0.00066 (25*-65*C) 0. 00067 (20*-100*0 0.00064 (25*-65*C) Typical Density Specific Gravity 25*/25*C (77*/77f)l. 380 Pounds per Gal. -25#C (77*F) 11. 50 1.445 12. 04 1.538 12.82 1.620 13. 50 1.646 13. 72 Distillation Range-ASTM D-20(Mod) C ............................................... 325*-360* 340*-375* 365*-390* 385*-420* 400*-430* Evaporation Los s -%-ASTM D-6Mod. 163*C....................................... 5 hrs. 3:0 to 3. 6 100 *C.......................................... 6 hrs. 0. 0 to 0. 4 3.0 to 4. 0 0.0 to 0. 3 1.1 to 1. 3 0. 0 to 0. 2 0.5 to 0.8 0. 0 to 0.1 0. 5 to 0. 6 0. 0 to 0.1 Flash Point-Cleveland Open Cup. *C 176*-180* ' *F 348*-356* 193*-196* 379*-384* None None None Fire Point-Cleve. Open Cup... .*C None* *F None None None None Four Point-ASTM D-97............ *C -19* -7* 10* 31* 37* *F 2* 19- 4* 50* 88* 99* Softening Point-ASTM E-28 *C -- -- -- -- -- *F -- - - -- - " -- HARTOLDMON0026653 *t r n 0 0 9 2 5 7 Dept. 246 - Process Description AROCLOR APPENDIX C PHYSICAL CONSTANTS (Cont'd.) 25. GENERAL PHYSICAL PROPERTIES OR AROCLORS (Cont'd.) Form Aroclor 1242 Practically colorless mobile oil Aroclor 1248 Aroclor 1254 Y ellow tinted Light yellow mobile oil viscous oil Aroclor 1260* Aroclor 1262 Light yellow Light yellow soft sticky sticky clear resin resin Fefractive Index-D-line 20*C 1.627-1.629 1.630-1631 1. 639-1- 641 1. 647-1. 649 1.6501-1.6517 Viscoaity-Saybolt Universal 210 *F (98. 9*C) 34-35 36-37 Sec. (ASTM)-D-88) 130'F (54.4* C) 49-56 69-78 100*F (37. 8*C) 80-93 185-240 44-48 260-340 * 1800-2500 72-78 3200-4500 --- 90-103 600-103 (160* F or 71*C) o o fu is m HARTOLDMON0026654 Dept. 246 - process Description AROCLOR APPENDIX C PHYSICAL CONSTANTS (cont'd.) PHYSICAL AND CHEMICAL DATA Diphenyl Specific Gravity: 0.992 at 75C/4C. The Swann chemical company bulletin of 1920 gave thermal data on diphenyl. Viscosity of plphenyl (from Anniston piles) P. 7CCT 170 lBo 190 200 220 250 500 >50 400 4 50 482 centipoiB'es l.^y 1. >09 1.208 1.114 1.024 0.901 0.752 0.574 0.459 0.274 0.212 0.282 Specific Heat (from Anniston Files) F. B.T.U./lb 200 200 400 500 600 700 800 900 1000 0.416 0.470 0.547 0.616 O.658 0.679 0.686 0.690 O.696 COMPANY CONFIDENTIAL TMan 009259 HARTOLDMON0026655 Dept. 246 - process Description AROCLOR 27. APPENDIX C PHYSICAL AND CHEMICAL DATA (Cont'd.) Diphenyl (cont'd.) Another record gives the following values for liquid diphenyl X. Sp. Heat cals./gram 100 0.260 150 0.280 200 0.412 250 0.460 }00 0.518 350 0.575 400 0.610 4 50 0.625 Vapour cp - 0.460 0.625 4puC. (d. a. Roper, Design Data for units 4 & 5) penalty of Liquid Diphenyl (from Anniston files) . C 75 100 150 200 250 200 . 350 400 450 Grams ./cc 0.9885 0.9695 0.9294 0.8885 0.8470 0.8010 O.75IO 0.6918 0.6180 of vaporization . 65.4 g. cal./g. at 258.5C. COMPANY CONFIDENTIAL TRAN 009260 HARTOLDMON0026656 Dept. 246 - process Description AROCLOR appendix c PHYSICAL AND CHEMICAL DATA (Cont'd.) 28. Specific Gravity of Aroclors at Various 'temperatures For 1242 ,- 1248 1254 or GE l4?6 1260 or QE 1482 Temp. 60 65 70 ll 85 90 95 100 60 65 70 ll 85 90 95 100 60 65 70 85 90 95 100 60 65 70 ll 85 90 95 100 SP Or. 1.547 1.544 1.558 1.555 1.552 1.529 1.524 1.519 1.515 1.415 1.410 1.405 1.400 1.597 1.594 1.590 1.585 1.581 1.505 1.500 1.495 1.490 1.485 1.480 1.475 1.470 1.465 1.584 1.580 1.575 1.570 1.565 1.560 1.555 1.550 1.545 Lbs. per gallon (us) 11.25 11.20 11.16 11.15 11.10 11.07 11.05 11.00 10.96 11.78 11.75 11.71 11.68 11.65 11.62 11.58 11.55 11.51 12.55 12.50 12.46 12.42 12.58 12.54 12.50 12.26 12.21 15.21 15.17 15.15 15.09 15.05 15.01 12.96 12.92 12.88 . COMPANY TRAN 009261 confidential HARTOLDMON0026657 pept. 246 - process Description AROCLOR APPENDIX C PHYSICAL AND CHEMICAL DATA (COnt'd.) 29. por 1262 Temp. c. 60 65 70 80 85 90 95 100 Specific Gravity of Aroclors ....at nous~~Temperaturea fcont! d) SP. Or. Lbs. per Gallon 1.604 1.600 1.597 1.59.3 1.588 1.582 1.577 1.572 1.588 15.40 15.56 15.52 15.28 15.24 15.19 15.15 15.11 15.07 Heat Capac.Lty of Aroclors at various Temperatures (cal/gm c.) `-^temperature Arper?'''-^* 0 50 100 125 150 175 200 250 300 1242 1248 1254 1260 Aroclor 1242 1248 1254 1260 .280 .270 .255 .220 .500 .280 .265 .255 .520 .295 .275 .250 .350 .505 .285 .260 .335 .315 .295 .265 .340 .320 .500 .270 .350 .350. .310 .280 . 365 .340 525 .290 .380 .355 .540 .505 Latent Heat of vaporization of Aroclors Temp. Range Latent Heat of vaporization 500-310C. 300?-330?C. 500-550C. 30C-370C. 6l ca1/gm 54 Cal/gm 50 cal/gm 48 cal/gm COMPANY ^ CONFIDENTIAL TRAN 009262 HARTOLDMON0026658 'f JL?gf> n)** n* JO* Treffrrfrrw... urniwm .... jc PHYSICAL CONSTANTS DATA -AEQJMK.HAa-tlfcfihnicalL Swgr 2 ytofttitt sv~--~- b** 1947 . 7/5/57 NAME formula C'j oH-Cl Mo[*culi_Weight____ ' .. Total CU 47.5 - 4C. 5 Ye SOURCE a p AT f Snecs. ! /1 l /5ft Aooearancc Boilms Point M M m Besli!-ens tf r ' . tl't . 1 i! I 1 V 'full it. 4". < ?.' : ; '' BoilitH. Point 1_ Beilin# Point i mm' Cryslalliains: Point _ . Nellinf Point Solution Point Specific Gravity f ...... ............ 65/15.5. 1.410-1. 420 Specific Gravity v Pounds per Gel. 25 C Coefficient of Expansion 12. D Refractive Index * nJ Infia Rod Spectrum (He/erentt) Ultra Violet Spectrum fHef&mee) ___________ /} ` Viscosity Viscosity o * ............ * Surface Tension Solubility in War Solubility in *' pt _ ,, Solubility in _ _c Sp. Gr. Temp. CoefM50-TO^CT "(T3OTS7*C ........ Specs. 4/11,55 ----------------------------------------- t .. .. a^ Specs. 4/11/55 t Flash Point F miwr C. 0. C. Fire Point C Heat of Combustion ...... He of Forettfien ThermalJtjbjIJty (ML/*t/fin,l______ ______________ __ Uepf.Htii.orfiaiai__________ ______________________ UtfilHiMO*,' $ptt>!i( Heat . Critical TemoerMute Critical Pressere Dissociation Const** 382 None .. Aroclor Bulletin OH * 1 15 " ( 1 454) ----------------------------------- ------------------------------------ ....................... ......................... ................................... ... < -------------------------------------- ----------------------------- . '* V \ 9 msS> s u 5 5 r ' . _-- t1 orsAamnl nUnUa76> l.l. Toxicity (Give RtfertneeJ Schwarts. U. S. RuAJiMlt 1. Sgry.icc Bull. 22!^ -4636 11 JaAislriitl_P.Qijg.nj Ls..Ha^jLrjdtei & SQlvnmji NOTE: The is lota ehauU mi hi relent td on me rtli if Mill r>. COMPANY CONFIDENTIAL HARTOLDMON0026659 fPT c-ff'T'- .... PHYSICAL CONSTANTS DATA p,SS* lUlITTHei ' AROCLOR *. ~ 1160 ITfiihnican tinueiun&i. rsaiiuia j ~sm~^ o^,,,s tBWFnrro *T .... ..... bJLVK' 1^47 Hev. Hv A. M. ~ il-.'nburff m N AMI For mule ._ Molecule/ tiM Cl'?H-t kCLc "~ >; - 7/5/57 Total CL 59. 5-60. 5% source tOATe Snprs 17 -? 1 -S4 AaOtlUnce Berime Point at 7(0 wo Pmnt M fim fed lift? Point M un Beilin* Point a mm CroUllitine Point JELilqwalQ__.PlarJl.,5tickv mai 5 Soecs 12-21-54 t f '* Uoflinf Point 'Solution Point SoKilie brevity * ffUTTTT 1.558-1. 572 Soecs. 12-2 1-54 Specific Cf*yitv u tand* per Gel. 25 <*C 13.5 ......... - Coetlicient of Exoenjion 0 Reftoclive Indu I Mu Red Spectrum (Ktfrrtm/ ' * ' ............. ............................. .... UItu Violet Spectrum (Rtfmtnt*/_____ ____ _____ -------------------- ------------ ---------------- - Viscosity Viscosity e SMace Tension SolMbtiitv (n Ms Solubility m ' . --------- :----------------------t----------------- f -- Solubility m . .. Sp Gr. Temp. Coeff. (75- 130WC) .0. 0010/WC Specs 12-21-54 FTsh Point #F (Ue$Mj Fire Point C . Hest ol Coabustjor) He# of FwmMion fhetmel ability (eM/w/awiO , LMfot Htft pi f(Bion LMenl Heat of V. $PfCilie Heit Cttticil Tesneerituff Cntieil Pressure ' DissoelrtiM CotilMtf ---- -------------------------- -------------- --- -- . . Nnnff____ None _ . ---------- . .e .......... . ------------------------------ -- . . . ' CS>............. ........ 5 m o S 5 TeiicHy f&w AiftrtnctJ HOT I: Thtu rfoio *KouU m*i if rtittstd w L` - TRAN 009265 --" _1 S chMLajlx;__li,_S^PiihL-He.Jilt. "InAisieial Poison^MiA rds and Solvents" by M. 11. ^Auc^Cflififiy .*^($#1 odiitio*at ikriu if mc*i >7 COMPANY CONFIDENTIAL HARTOLDMON0026660 ipf . Qt* PHYSICAL CONSTANTS -DATA tlftWCTU'Al. FOKMUL A ABQCLOBJ 154 (Idmejl). - i i t 7, S%o rwBFtitD rr-"'. JL -A-^M--LLLLejorniiig- MAME itoiU____________ Soleeulit Weight kauma___________ _-- tsU.ifit Point AWm______ foM *L. sm____ Beitint Point M . foiling Point A mm________________ jPfygUllumjt Point_________ ;___________ Mhm foul----------------------------------- WliiSO.fyfBL. \miliiSniviiu. _ _. fii, liLJj___ Specific GnwtY y_____ _____ ____ __ Powids pCflTSl. H~ '>i~ c Coetticient o( Exppinon__ Reflective lnde /___ JLL Inlli Rod Spccttuii <hrjr>rr,rt Ultra Violet Spectrum iRtfwmttj_____ t _ __ ViS-esity_ . ____ j___________________ ____________________________ Suftolinstfift_______________ ________ . SoimitilrmUor ^JMlilsnD.--------------------------------loiybilliy In____________ _____________ S&SdMtXznW* Qos.iLli5 -JLC1 *T< l'STT 7/5/3 7 Total Cls 53. 5 - 54~5^~ Cl L _____ _Spaes.. JL2.? 21-54. .iiaw.njgjikgjc oily iiqv>i<iL.SjaicjLIl2j:ibi.i'." ISSF.-lJUL .12J_. 0. 000957gc~ ir Fluh Point ftF (Method)_____ Fire PoInf^C.___ '________ HJ!U(j.uiUen_________ HeJ. oJ Focmfion______ .___ Thermit_ aJbilitjf (caT.At'min.L Ufflt EtSISfl____ __ UtflUia,0( i. Specific Heat 1' Crilicil TetnoerUptl QiilMfmmi______ _____ Oiitocution CmMM None .Nont_ -4- ..4 ll 8m O o JS 5 TRAN 009266 ToiieHy (Give Refmnee) Schwartz, U. S. Pub. Health Servtce. Bull. *2 2u _.>_i; 'Industrial Poisons, Vol, P,-463-364 1U , NO T 6 1 Tktu date elwtJd Ml it rtltmetd nilH/.*.?^inS2}evJBloSPtl Mi Sa/JSP&ft.,. t/ ni re iu HARTOLDMON0026661 Cu... PHYSICAL CONSTANTS DATA TtjftTXWirtf """* 'lm--. A ROC LOR 1162 fTechnlcal) * rm'prctrsr^-^rz------------- NAME FwwuliC | ?H-C1. Iteltculu Weight. Aooemnce_____ _________________________ Boiitm Point MJttji___________ M% frit* AtBoifmi PaiM & _ea Boiling Point < m _ Ciystilliini Point___________ lidtint .funi______ Solution Point . Specific Gnvitv r_____9Q/i5^5. Specilic Guvily 4_________________ Pounds pei Gil. * ys C Coefficient of Explosion _ Reflective Index Infii Red Soectfum (Rtfttme)__ Ullii VieTd Speetrem/Re/f/enc*;____________ &<>*'.------------- --------- --------------- yilEGBfr/--....... ...... ... --------- Sitffge Imiiefl_________________________ SoliOilitv in W4jr SsM'lifcJi!_____________________________ Solubilily in _ __ ___ ____________ Sn.Gr. .Tx'mp' 0lL i85.-.12QECX. Ain 1347' ___ 175/47 Total Cl? 61,5 -62. 5^~ hxmtnlo. MiLCit _siicju^^ 6 _RA T_ _ 11-3 5 JL^5UL-_L-&U,, nxjzzzz TZ3,,Jlasx.Id.L* 5.5. . _. o.ooio7ffc_H"4 -- Hash Point F (Hhed) E^^ZZZI______ Hf*ilf.e#y|liefl............... ............... Heit el Foimftion_____________ CiiepiHiitM.Fia(ciwi(..A_A_>i_(kL_.________________ LAfOi H*L9f ,yac.____ teiiQfJftU_______________ CjiiiHLISP^iSjfit_____ ,_____ CiiticLaiitM____ _______ Dissociition CmdLM Hone. [Mon----- # fl TRAN 009267 ** o Toxicity (Him Rtftirntt/ SehriurlT. U. 5. Puh. Hull t. ''Industrial Poisons .ttaz ark 5 aatLASafll vAimfayJ\L 1L__ NOTE: fAtst dote etwuli mi ii Jacobs Vol. rtltttd ulif / miimu 1|P -46 3 - 464, Cktnicoi Company. X9 C/lt ~7 Mainonaf < Affix if Mm *ufT. HARTOLDMON0026662 pin PHYSICAL CONSTANTS DATA TUffrlW ARfrCLOR i 2-42 Huctuhal roMWi C ' 7 "' / ?o TftBPItrB Wf A. M. K : > bu m ITfT*------- c r v. 51 / NAME F oimuI a __ _____________ fhttcoplecciiu*laact efrri|ht....__.__._._..... {foiling P^int & 760jim__ Ra r. g v__________ Oojlinj jg :t_ ___ _________ 6e|iiiSi!HiM=I___fiB_____________ .. . Boiling Peifrt.il___ m Crvshlti/ing Point____ . ______________ UeJliui Point. _ .___________ __ ______*. . . loHiiofl.Peinj____ __________ |pfylic Giayilyj _ 2b _C,_______ _____ Specific liiavity 21/ i *>. S C, Pounds pet Sal. 2^C . __________ Cnellici.efU of Eapinsion 25-1>5 C. ReliKlivc Index lh C., . ft l______ Inlia Red Specttum (Rtjtitner/____________ ____ Ujtji Violet Spectrum 'ftr/*r*nrcy_______________ ylcpsity .. 21.0_.fl*. V'scesily i _. fPA.f , ____ _______ Surface Tension.. .Py: SoJtfnlj.ty in Nrfer SeluPiitPjn.. \A AJ jbL .@._2Sj ioJiffeiHty in Py r dir e____ (5 iO 'C. _Ci2_H- CJjl >25? .'avi________________ ..C&Jiirjggs Mcl^e Q:., ?, ?25 - 1*0 C. . ..15^55-C-___ I___ 1'Z __Nr>l_:.c r yst a 11 e_ J^ISfi__________ _______ t ,J8J_ - I , '3..' _____ Z ,,XL_QPQf; b. .wcyxc/lCL_____ .JJ.-.T5. .SUS_________ .14-94.5i?S.,,..:_____ .4 5.1_________________ lr, .. IJbj o . souwee a pate _ IAiluliU..Rn.f OP 1 . .. 1 Sprc-.l.r^'-i. _ 2. .1 -t - \ \ ;..M.QP.-*.. *i_. . Ir .CiiiZ.Si.iZ Flash Point r o. c , Qie Poijt__C__________ c . o.c , Heal of Combustion___.......... ..... ..... Heat of Formation TffOWl SL*ility RaL/kl/.'miSjL. .. LAant Hast e| Fjsier.._____ __ ut_ni Hk&d vjD._r_al/n}j_ SpieiljtHe.il. I 7S C. Crjtical Twnoeialure CrflKlLPlttMA Soer I: c Heat (5 iOQ'C. Po r Pc; r T ' p r na Cn.dvc*.ivit calZ. 51- D e eerie Cergia-* 100 - C . bO.SXjLr, 180 C. None Ai__. O' 29 1*0 -H C. f.r louder KOiri ^lJLJL ajcu'.st.fii. .. . T e be p auL.--------------- M--B^JQPjcjLJi_______ TRAN 009268 ToilCltr ft* it Rtftttntt) Contact Medea Dec* ______________________________ --------------------f------------ 1----------------------- - NOTE: I t(K rfala iksttJd Ml N rtltattj cunUi / Ife/ueRI Ckrmitml CompaMf. Ut* mddiltottml itii 1/ mmi.j'* COMPANY CONFIDENTIAL HARTOLDMON0026663 , r/ ~ tltM ete PHYSICAL CONSTANTS DATA Prr _AAQCL0B_L2AL r TOTOBTT NAME FermuU Molecular Weigh! ' Aouflifince - Boiling Puirit i 760 mm Range Boiling point *_ 1_jwi " Beilins Point A .sa. Boilin* Point at tw Crystalline Point . jaHlint Point Solution Point fi Specific Gravity 25/25'C, Specific Gravity t 65/15. 5WC. Pounds per Gal. f 25 C Coeflicient ol Expansion 25-65C. Rtliactive Index 25uCn & f Intia Red Spectrum fReferent*j Ultra Violet Spectrum (R*/er*net> Viscosrtv.e 130F. Viscosity f . Surtiqe T ansi on Dvnes/em 20WC. jjoiuhifitv in Wiet Solubility in 3A Alcohol @ 25WC. Soltijilitv ift ^vridLn# 29 C. TTfg 4-25-57 CS2 H6 Cl4----- 1 _ 292 (A.Y8L > ,, Yellow Timed Mot Oil 345-385C. __I6S=_21DC. * Non-crystallizing 1.445 1.405-1.415 12. 04 __Q^ PQJP7jP.jcjc / cc l ^C. 1.6285-1.6305 73-80 SUS 44.2 insoluble 15 g. /100 ec 1 i i. 4e. /100 cc souacc a date Monsanto Bull. OP-115/19 ! II If II Sp e c if,lc a t ] on s. 8 9,54 --M-.B. OP- 1--15 -- Specification 9/ 9,54 ML B. OP-115 .. J._ CoU. ei_ 7. 166. (1952 M.fl. OP-115 If Plash Pointc. o. c. File Point C r o e. Hea| ol Cprofrustlon Hep o( Formalion Therms! Stabifity (ealT/'Xg.-`tninI} . LApnl Rej| of Fusion Laent Heat ol Vao. cal/ffm. Specifif H?at @ Critical Temooigure ' Critical PtMstrt . Dissociation Constant SrecLflc Heat @ TOQ^C ' l96wr None _ . ..... ^4 CL 211 . _ 0.356 .* ^ ` . Poor Point Thermal Conductivity, cal/ cm/C/sec. m Dielectric Constant. 100C. e hZ cv. . o 5 9 ,^ 0C. or lower 23. 6 @ 28ur. 4.5-4.7 * * ` a TOXICity I'Giut RefeetneeJ CoAacf Medical Dept. M M . Calculated M. n. flP: LLi______________ IB II To be Dublished M.B. OP-ns TRAN 009269 M.B. OP-11 6 HOTS! These gala not if rebate* ealiigf /gcnfiu CKemieal Company, Vte odditienel ekeeu i/ miiiwj. COMPANY CONFIDENTIAL HARTOLDMON0026664 VffT *1* PHYSICAL CONSTANTS DATA SfSr a. VSI* A PCX.'LOR l?t4 ... ..... rronrte'rr ZTfT~'------ QgTiZ ; AM. El.e-b-rg 4 ?':> 4.* NAME Foimuli__m___________ . Kteie_cu[i2_iei|W__________ XLZ-fcbjCl*. twm'mt________ '_4__ ! Ba'iiniPM i ?&">__ Ri'.gt. n._3 mm t! -EAif---OiL Mor.sai.oJiji. .QP_.li; .'IS. 36*- 40 C 1AQ -3TP0r Swims Ceioi A--no. Soiling Point 4 mm___ CfYstalliring Ponil_______ Nor crys- al. u* >1 l___ ___ Memos fQiqt___________ SNt^ipn PoiiH _ ---- Sutcihc'CuvilYA iVTT^C. | 1 >38 _________________ . --- ` " i r " * * " S%opuemcifisic Cr>iy per Gal, g e 6i>> _________ l.l_ p_____________ J.Z.1Z. Coellicitirt o( Eipision l ' ps^C. jumo&s 421______ __ ,, _ ... -O'------------2i:_c Reli active Indet 4_____ 1.63?0 1.6390 Inllt Red SpjcthW (Rtftrtnttt .SrxjLtl-rxrar. .. . Sj-tlJ_L4. :i i . . UlUi Violet Spedfue /'l'i???^______ iI:; ViJC|ii.l.5..'\_,,.____21Pn_iEft*_*_w__ _____ 4 JI Aa a3,ase:;e>s _f? ____ ______ MB OP Vscgy|y .. kilKLlttiion______ U-IZ^lLsm______ 4 ,,^3_Sl LOO?!* eij|>i lift.!?. MMS._______ l ____ & JnsfllafelE--.1-- ]... Splitiliiy ip. 3A Al;o*-.ol 2~ C IQ g>l?n_cc___j______ Solubility in P\ L4in_@..ll.^C 114. e.7To c~ it ii 1 1? Flash Point __ ^. o. c. ` File PibijI^P_________ ?- o e.__________ ifii!?i CwtitjUt*.. Hfit ef Fwafiw _ ____ ______ 5iheirnt_St*j liity. (cj jAt-.'mnJ_______ LUent Hjpjtji. f taton___________ UtOTlK4Pty.____ zallgm btsiucm1.___ ___ Cfijic?l TjnetfJlUR_____________________ y?r-e ^sus.____ JjO JLAMii_________ OiimiUpft QwAM, 0-33* 4fail2jemL____ _________ rnul CovductlvUv Cal ' 7^m]3^LisKZ I D.ler. r:c Co* o pn c'. >i 5 lOO^CiT 4. If: 4.3: CfelCblA' rd_ xmSjqejji To be p ,,bii-bed . ... ...... ... MR -OP-11* TRAN 009270 Tclltrty ((jive Rtlrrriittl Ccrjjl "1JVlfcili "a.lJJxxi. Jd_E__QE_LLl____ I __ H 0 T E : |At# 4mit theuli net it tiltatti mIiiYi of Montonte CAtauca/ CoMpony. I'lt aitfllieaai tAttll i/ ateti >/<. COMPANY CONFIDENTIAL HARTOLDMON0026665 jPepr Hi UJtN %t * PHYSICAL ftitrfirrr**'1 _______ ABUCLOB l?FQ Sl,st i?) CONSTANTSZJDZOAJTJA2______ jsr se r JcTu*i."?e'ikut a" ** r. .1 -- V ?BESrTi.t B"6 ? ------------------------- A . M j; ! I< f.lUi l`Lf ` J`6'rt---------- * // ct l. i6 fpjmuia............ t<toiu!ai Weigh) NAME ........ _J_____________ _____________ _..ca 2IL .SjFT:-.'j2` . ._lP'i5f..JLP>.Te ... - ! .v ___ .] I.U'iligj! Pointftp mm. .. ji si'~ .. . .. Opim*tojit .* lift__ ___ _ ' ... iiifc ilLCiL'L.ril'UC., ^w^XSii'TEriVCci'.-'ji* VI ............. . Qsulrnt PcinLl . M.._............... ... Boilin Point. .. mm_______ _________ f;/yMaltmn Point. .................. _.. ... MclLu Point .* . ......... ....... ..................... ' Spigiiofi Pomt spofiicCjavijywrr- . ^xm..Q.'-_s:alU^ir4i... f| jt !.y-n 1 :-r feeyfLjccQwiiy..*. .. 5jo, 1. V.. *.i (...:... ... ] .1 Pounds per Gl. .. ' 6C. _ ............. J.?.\l-....... ............... CoeMiCi6nt.ol.t*p.)on. n .j.0dj!'O Reljicltive iInddeexx. 1 . . .* ."r. _n,`i. '. .Q..U1V'L:` ct. ______ _ Inlii Rltedd Spectrum (tkReejjeientn ; .. . _...................... . SpLUlllCd'. i;j i > _\:L<.Oii.LL- . . . Uitil Violet. SjKtium(f/r*nr*r _ Vitcesily <_................ j -nrs Viscosity ................. _ ___ SullKt ItniiOQ .............. .. . .. Solubility jn Water ___ ______ . SoltfH'ty ........... r. ___ Sp'l.ubility.in........... ........ 1.. ... Fl 1jh Point __ ________ __________ No Fire Point_C ____ . .. c_0 ..C _.... ............. Hfit pi QpirtuMion................... .......... . Heit.ol FymAjon .. _____ _ _______ ____ _ Theim* StAjlity(cii.Afc mi/i.1 . .. . .......... (jten't Hept el Fusion............................ .. . Uttnt.Hf* oJ V.JP................................ .............. id ............................ S/*?iJ,'c. Hmja........... _ d ..iL-C-________ .......................... C.ijJicjl Temp.ejeiurt_____ ___________ J* . .. . .. CjutlciLgijeiMJi_______________ __ _______ QamiilLU.QaMM___ _--_ Sf lc il';c Hcp: MMC_. n. :io t Li-xtuLJBaiai. ia T "" ...CAiifiwJ.A.'/.U ... JUTl OP.. 11 '? %! .l2ai:l^u.:JjXu:i:i:iLr>., ltfO SI !u___________ JLO.fi.-. .it= T Toucity rCiK ktfrmtcj t >' i a C oV 4 s: Mc-j , Dt pt. TRAN 009271 _______ :7Zji' MB OP -llo NOTE: rim ^nro tkotli net kt ritto* t4 eutudo t>[ Kemomte CKemteal Company. Vie additional sheet 1 if neeti* m . '' * COMPANY' CONFIDENTIAL HARTOLDMON0026666 a.... i PHYSICAL CONSTANTS TOWraW---"*TM--^liflami2fijLjL.ljfflJroiuol Mix DATA Sy.$79, y su Mixture by Weight YttUPtl WW WT" !\ V Fllf>nh' i* NAME fOMWlJ_____ ______ ___l Moltculu ieifhl___:______ Amemmee___________ ___ SaiJ'ii fsia_l.Zfisa.__ . _m___ ____ Botlina Point 4__ m ... Sotlmt Point < mm _ Cfyililliliftt Point_ Melting Paint _______ ____________ Solution Point ______ ____ toeci>iC-Criv_itY 4.. _ JQ/J. Su. 5.C_ Soecitic Gravity *> ___ Ffwds pei Gil. 95 6C Cocllicicnt ol Expansion _ Reflective Index / li (nilI Red %mUm /He/erentt) Ujiri Violri Sp'ertnw./'fif^*?ft)___________ Vucosiiyj-_____ :.'._10DE.___________ 5Q2*lly i__________ .21Q:l____________ kulsfi Imum____________ __________ Solitilitv in Wier Solubility ifl_____________________ _ Solubility in "BXf a........... 7/3/57 .Syrupy, liquid 90% - Aroclor 1260 10% - Toluol source & pate __ J Specs.. AJ llyJijj_ ULJL -it- .1.. [ML 2 xaV(232 JSui)_ I3.B.5USi_____ Wi3KJ^tL.O/2i. fiasn*Poirt 6P (y*f*4J._Tag Qpen_C-UiL ________ 11 11 MfilLM. Ci!^JnTi25: Heat ol PwmMion ........... ........ ,, U.tt Heit oi.fjBisc.____________ ------------- kM&nlMMjd 1m,-------------------- _ Specific HeM Cilticel TemwKael_ ,,_____________ Giil&iLEmmt. 1 05 .UL0_. WGK Lab 12/ 5/ 4fi sg ss o? Toxicity (Gtvz Rtfmncr) TRAN 009272 HOT E! ftcii data ikould aoi to roloaood (xln/i of Montama Ckomieal Company. Uta additional tkoott 1/ ****"'?> HARTOLDMON0026667 pen W |U(N |(| a PHYSICAL CONSTANTS DATA M1 fffulTW Bfl k, f OBtlCoT' ' Sy.$7 tf"/ TTOrptrTrTf Formula Molecular Wei*ht Anoufenr. NAME ' ' Bollin* Point X 760 mm _ Bwiiifijlftte jl m__ IfllliM Point t Boiline Po/nt A M nm CiYSttlkrini Point Ueltins Point 'Solution Point _ Soecitic Gravitvi 90/15 5C Specific Guvity * 25/25C 'Pounds per Gal. u ?r C . Coefficiam of Expansion 25.65r Reflective Index 26r n i Infra Red Spectrum (Refimtet) Ultll Violet Soectium (Retrente) Viacesitv e S,1QJF\ Viscosity # Surface Tension . Solubility In Via Solubility in . Solubility in . oTrr" Ci'iHojCln ' .195 Liffht veil, sticky Resin 3 90-425C ' , NIL eoumce tdate 0 .Monsamto-Bullet in OP -11 5 " (195 1 1-577-1.587 ~ Specs. 4/11/55 '1.646 MR OP.IIS ra. 72 0. 0006 4 ec7ecV_wC ' 1.648-1.650 . II " "-- 86-100 SUS f ` Specs. 4/11/55 .' * fl Flesh Point F fUetHod) Fin Point C Hut of Condition Heat of Formation Thermit t^lltolsiw^Mii.l Litnt Hut of Fusion Lient Hut of Veo. Soaclfic Heat Critical Tenoeriitfi Cr'rtieil Pressure OiiiMittfan Caudtei Pocr Pbint None Non* . . ' .MR OP-115 II \ * e NFIDENTIAL fl s# of o M 5 . .. * __ TRAN 009273 , TOliCity (Ci\* Reference) ConiJLCt MeiL Degt. MB_QErJJu5______________ ____ 0 1 "" TM" 1 " NOTE I Thee* due tketdd Ml k r$temed emlaido *f ViiumW Ckemitel Cem^eej. I/s ikiriUM/ i*t*n if eettfery. HARTOLDMON0026668 Dept. 246 - Process Description AROCLOR X>. APPENDIX D UTILITIES Tne utility calculatiDns are based on design calculations for a 28.8 million pounds per year production rate. The breakdown of utility usage by Individual equipment is only on estimate. The estimates of utility usage are average values in most Instances as it is difficult to measure the operating time and load for a particular piece of equipment with great accuracy. The total usage of each utility was taken from the cost sheets. Estimates of individual operating time and percentage of the total load were made to calculate the distribution of utilities as given in the following pages of this section. COMPANY CONFIDENTIAL TRAN 009274 HARTOLDMON0026669 Dept. 246 - Process Description AROCLOR APPENDIX D UTILITIES (Cont'd.) I. Power Consumption A. Electricity - Mo V., 3 phase , 60 cycle Peak Item Equipment Motor Load No. Motor HP KW 101 Biphenyl transfer 3.00 pump 103 Biphenyl head tank .75 pump 104 Biphenyl feed pump 7.50 2.6 0.7 6.6 121 #5 Chlorlnator pump 10.00 8.8 122 0 Chlorlnator pump 10.00 8.8 123 0 Chlorlnator pump 10.00 124 0 Chlorlnator pump 10.00 8.8 8.8 125 0 Chlorlnator pump 10.00 127 #2 Blow tank pump 5.00 8.8 4.4 129 #1 Blow tank pump 132 #1 Still pump 135 #2 Still pump i4o 0 Receiver pump 141 #2 Receiver pump 144 Blend tank pump 5.00 5.00 7.50 2.00 2.00 3.00 4.4 4.4 6.6 1.7 1.7 2.6 149 0 Storage transfer 3.00 pump 151 #4 Storage transfer 3.00 pump 153 #5 Storage transfer 3.oo pump 155 0 Storage transfer 3.00 pump 157 #{ Storage transfer 3.00 pump 170 0 City water pump 7.50 2.6 2.6 2.6 2.6 2.6 6.6 171 #2 City water pump 7.50 6.6 l8o Exhaust blower 15.00 13.0 Miscellaneous Totals 135775 0.9 TT5To Monthly Usage KWH 8o 240 1980 3040 3040 3040 3040 3040 200 1580 1580 2340 20 20 200 160 240 200 80 80 2340 0 0 >.o 2U7B5U company confidential TRAN 009275 HARTOLDMON0026670 Dept. 246 - process Description 52. AROCLOR APPENDIX D UTILITIES (Cont'd. ) I. Power Consumption (Cont'd.) B. Electricity - 110 V. , one phase, 60 cycle Peak Load Equipment KW Monthly Usage KWH Lighting 15 5600 Instrumentation 2 1440 Miscellaneous 5 ,2150 " Totals 20 2. Natural Gas Item No. Using Equipment Normal Use SCFH Peak Use SCFH Monthly Usage MSCF 151 #1 Furnace 1200 2400 450 152 #2 Furnace 1200 Totals 2400 2400 4800" 450 860 5. Compressed (plant) Air Item No. Using Equipment Normal Use SCFM Peak Use SCFM Monthly Usage MSCF 127 $2 Blow tank 60 148 #5 Storage tank 60 200 2590 200 90 150 #4 Storage tank 60 200 90 152 #5 Storage tank 60 200 90 154 #8 Storage tank 60 156 #7 Storage tank 60 200 200 . 90 90 Miscellaneous 10 Totals 570 200 TTO" 550 3460 enMPANy confidential TRAN 009276 HARTOLDMON0026671 Dept. 246 - Process Description 33. AROCLOR APPENDIX D Nitrogen UTILITIES (Cont'd.) S' Item No. Using Equipment Normal Use SCFH Peak Use SCFH 142 . 143 1^6 147 1^0 150 152 #1 Blend Tank #2 Blend Tank fl Product Tank #2 Product Tank #3 Storage Tank fk Storage Tank ff5 Storage Tank Totals 3 3 3 3 3 3 3 2T" 4 4 4 4 4 4 4 Purchased Water ' Item No. Using Equipment Normal Use 0PM Peak Use 0 PM 130 #1 Still 3 131 #2 Still 3 203 #1 Vacuum Jet 20 20*1 $2 Vacuum Jet 18 205 #3 Vacuum Jet 15 206 S-K Drowning Jet 25 Miscellaneous 2 Totals 00 5 5 20 20 20 30 10 T10 Monthly Uoagc SCF 21*10 2140 2140 2l4o 2140 2140 2140 I4,yo0 Monthly Usage M. Gal. 150 150 870 770 650 120 100 ?8T0" High pressure Steam TUtiTSTG at Item No. Using Equipment Normal Use Lb./hr. 167 ffl Blow Tank 203 #1 Vacuum Jet 20*1 #2 Vacuum Jet 205 Vacuum Jet Totals Low Pressure Steam at 325P. 210 *150 400 325 1383" Item No. Using Equipment Normal Use Lb./r.r. 102 Blpnenyl Storage 700 Tank 138 #1 Receiver Tank TOO 139 ft Receiver Tank 700 1*12 ifl Blend Tank 200 1**3 ft Blend Tank 200 1*16 #1 Finished Prodict200 Tank Totals 2T0U Peak use Lb./hr. 310 670 615 500 SO?5" Monthly Usage M. Lb. 150 320 290 240 TOUO" Peak Use Lb./hr.. 900 900 900 300 300 300 Monthly Usage M. Lb. 500 500 500 150 150 150 38CRJ TRAN 009277 COMPANY CONFIDENTIAL HARTOLDMON0026672 Dept. 246 - process Description AROCLOR . APPENDIX D UTILITIES (Cont'd. ) ?. Low pressure Steam (Cont'd.) Item No. 14? 148 Using Equipment Normal Use Lb./hr. K2 Finished Product Tank 200 #5 Storage Tank TOO Pea* Use Lb ./hr. 500 900 150 #4 storage Tank 700 900 152 #5 storage Tank TOO 154 $8 Storage Tank TOO 900 900 156 #7 Storage Tank TOO 900 Miscellaneous 1400 Totals THUU" 2800 10,500 ^. Monthly Usage m. ; 150 500 500 500 500 500 1000 "5H0tr COMPANY CONFIDENTIAL TRAN 009278 HARTOLDMON0026673 Dept. 2^6 - Process Description AROCLOR APPENDIX E PERSONNEL Departments 246, a-246, B-246 and C-246 are closely related. Operating personnel may work in all of the departments in a given day. For this reason, the description of operating classifications and assignments for departments 246, a-246, B-246 and c-246 is given as though all four of the departments are Just one department. Operating Classifications ' - Job Premium Operator Standard Operator Repairman Packer Porter Swingman ' Total .Number of Men 7 day/weck Sohedule 1 10 & A Schedule 4 5 42 11 22 t * 10 12* 9* The swingman works two shifts per week (Saturday and Sunday) as a relief foreman, two shifts as a repairman, and one shift operating the premium job. There is an open shift on t.ie standard operator Job that is covered by overtime. The premium operator and standard operator cover three shifts each day. The repairman works the day shift, and with the swingman, there is 7 days per week repairman coverage. Packers work the day and middle shift 5 days per week. The porter works half time in department 246 and half time in department 24}. The premium operator has lead responsibility for his shift. The work force works all three departments Aroclor, Pyranol and Pydraul as one coordinated operation. The assignment of time is 70<{ to Aroclors, \yf> to Pyranol and 15# to Pydraul. Operating Assignments; Premium Operator: Has overall responsibility and operates 5 chlorinators 2 stills and covers the necessary absences of the standard operator. Standard Operator: Operates.2 blend tanks filter, 2 finished product tanks, storage tanks, makes pyranol and pydraul mixes, loads trailer, and tank cars, charges chlorinators and transfers receivers and also belongs to the Fire Brigade. . Repairman; Unloads cars and trailers of Biphenyl, Trichlorobenzene and Tetra-Trlchlorobenzene and finished product, makes weekly safety inspections and department minor repair work. COMPANY TraN 009279 CONFIDENTIAL HARTOLDMON0026674 Dept. 2^6 - Process Description AHOCLOR APPENDIX E PERSONNEL (Cont'd.) Packer: Fills, stencils and labels 5 gallon, JO and 55 gallon drums and clean-up assignments when not drumming. Porter; Cleans office, control room, repair room, wash room and smoking shelter. Swlngman? Works one day per week as premium operator, two days as repalrman and two days as relief foreman, as relief foreman takes overall supervision and day shift on weekends Including arranging for maintenance, night sheets and line-up of work. HARTOLDMONOQ26675 Dept. 246 - Process Description AROCLOR APPENDIX P PACKAGING Sc SHIPPING Aroclor, Pyranol & Pydraul are filled about half in drums and half In tank cars or tank trucks. A substantial amount (about 40#) of Aroclor is used to make Pyranol and Pydraul. Sales are largely directly to the customer. The remainder is in bulk shipments to the J. F. Queeny Plant. All electrical grade tank truck shipments are made in the customers trucks which are stainless steel. Non-electrical Aroclors are shipped in leased trucks and may be iron although other materials of construction are suitable Pydraul is shipped in steel tank trucks. Electrical grade Aroclor and Pyranols are shipped in lined tank cars either 4,000 or 6,000 gallons in capacity. The lining is either tin, zinc or aluminum spray because iron contamination is detrimental to the electrical properties. Electrical grade cars are either owned by Monsanto or on a long term lease. Non-Electrical grade Aroclor is shipped in steel cars. All electrical grade lots and bulk shipments of non-electrical material are sampled from the final container. That is all tank cars and tank trucks are sampled and analyzed after loading. All electrical grade drums are sampled from one of the drums. Tank cars and tank trucks are inspected to be sure they are free of dirt and water or other foreign material before loading. Heels are drained before loading some materials. Car washing when necessary is done by the repair track. Tank cars are sealed with a numbered aluminum seal Lacquer lined drums are used for Aroclor and Pyranol and plain steel drums are used for Pydrauls. A summary of products , weights and containers current use is as follow8 : Product 1232 1242 1248 1234 1254 Xylene 1260 1262 MCS295 Pyranol 1488 Pyranol l48l 5 Oal. m 60 Go 60 60 60 - Weights and Containers ^^onSaTT"-3515aTT"" TT m 600# - 600# Yes -- 600# Yes - 600# Yes - f0# - - 600# Yes - 600# - - 6*15# - -- 675# - 675# TC 0 Yes Yes Yes Yes - 3! \n Zz < 111 Q S n* Oz 0 TRAN 009281 HARTOLDMONOQ26676 'Dept. 2^6 - Process Description AROCLOR APPENDIX F PACKAGING ft SHIPPING (Cont'd.) Product 5 Oal. W--eiSghirtsoaain. d Containers TT TC Pyranol A-13B3B Inerteen PPO Pydraul A-200 Pydraul 280 65 65 59 - 360# 360# - 88 6*5# 625# *1000 Oal. - *000 Ga 1. tc 8000 Oal. Yes -- COMPANY CONFIDENTIAL TRAN 009282 HARTOLDMON0026677 Dept. 2^6 - Process Description AROCLOR APPENDIX 0 MATERIAL BALANCE 39* The material balance on Dept. 2^6 was made with a minimum of field measurements. Most of the estimates on the following page check fairly close with actual raw material usages that can be readily measured. The exact composition of some of the intermediate process streams is uncertain. COMPANY CONFIDENTIAL TRAN 009283 HARTOLDMONOQ26678 * *9-1-4 COMPANY ' CONFIDENTIAL HARTOLDMON0026679 Dept. 246 . Process Des rlptlon AROCLOR APPENDIX 0 *0. SUMMARY OP MATERIAL BALANCE RESULTS Raw Material & Cost ($/lb.) Biphenyl (.0662) Chlorine (.0217) AROCLOR 1242 Usages - Lbs./lOO lbs. product Material Balance Theory Material Balance Usages lbs/100 lbs. 68 63 58 Finished ProcJ. 1 Filter Cake 3.5 Still Bottons .5 Off-das HC1 WJ70 84 91.8 42 Finished Pros. 1.5 Filter Cake .05 Vacuum Jet 2.8 Still Bottoms .95 Air-HCl Mix ture 44.50 Off-Oas HC1 Ferric Chloride (.129) Attapulgus Earth(.0302) Air (.00056) Lime (.0100) 0.03 15 3 0.5 .03 .15 3 0.5 BJphenyl (.0662) AROCLOR 1248 52 56.5 Chlorine (.0217) 96 103.2 .03 .15 3.0 0.5 52 Finish Product 1 Filter Cake 3 Still Bottoms .5 Off-Gas HC1 553 48 Finished Prod. 1.5 Filter Cake .05 Vacuum Jet 2.55 Still Bottom .95 Air-HCl Mix ture 50.15 Off-Oas HCl Tuyrsu These raw materials are the same for production of all Aroclors. COMPANY CONFIDENTIAL TRAN 009285 HARTOLDMON0026680 Dept. 246 - Process Description AROCLOR 4l. APPENDIX 0 SUMMARY OF MATERIAL BALANCE RESULTS (Cont'd ,) Raw Material k Cost ($/Ib.) ' Biphenyl (.0662) Chlorine (.0217) AROCLOR 1354 Usages - Lbs./lOO lbs. product Theory Material Balance 46 H9.8 108 .117-5 Material Balance Usages Lba,/lOQ lbs. 46 Pinlshed Product 0.5 FI Iter Cake 2.8 Still Bottoms 0.5 Off-Oas HC1 W7 54 Finished product 1 Filter Cake O.05 Vacuum Jet 6.8 Still Bottoms P.95 Air-HCl Mixture 5$.7 Off-Gas HC1 TT7T5U Biphenyl (.0662) AROCLOR 1260 4o 43.4 4o 0.9 2.0 Finished Product Filter Cake Still Bottoms Off-Oas HCl Chlorine (.0217) 120 128.8 60 Finished Product 0.5 Fi Iter Cake 0.05 Vacuum jet 4 .8 still Bottoms O.95 Air-HCl Mixture 62.50 Off-Gas HCl T7B78U COMPANY CONFIDENTIAL TRAN 009286 HARTOLDMON0026681 Dept. 2^6 - proceBB Description ,,,, AROCLOR APPENDIX H ATMOSPHERIC DISCHAROE - WASTE DISPOSAL Discharge to Atmosphere Lbs. per C Lbs. of Aroclor Produced Total Lbs./Yr. based on Prod. Rate 28.6Hltgfr 2. HCl fumes from blow tanks O.Ol . .2,000. 2. HCl fumes from other tanks vented to atmosphere 0.01 2,000 5. Chlorine gas from chlorlnator vented to blow tank Un'.cnnvn ,Unknown 4. Aroclor le Biphenyl vapors of tanks vented to atmosphere Unknown Unknown Discharge to Sewers 3. HCl from chlorinators 2. Cle from chlorinators 2.5* 2.0* 500,000* 50,000* Discharge to Waste Disposal 1. Montar 2. Aroclor 0.0176* 0.55* 5,000* 95,000* Estimated COMPANY CONFIDENTIAL TRAN 009287 HARTOLDMON0026682 Dept 246 - process Description 42. AROCLOR APPENDIX I Sampling Point Chlorinators Blend Tanks - Storage Tank Composite Tank Cars & Trailera PROCESS CONTROL Frequency Reason for Sample Normal Range Method Number 2-2 times per batch Specific Gravity .011 2 times each day Color (APHA) . 50-150 Max. Sp.Qr. at 25/15.5 C. .011 Acidity (mg. KOH/g.) .014 Max. Moisture (H*0) (PPM) 25 PPM Max. Refractive Index at 25C. .0020 Inorganic (ffee)Chlorides .05PPM Max. Dielectric Constant .20 Resistivity (500 VDC at 100C. Q 500,Min. 0.1" OAP as ohm-cm X 10^ Hydrolysis Stability 1.0 PPM Test (as Chlorides) Max. Monsanto Stability Test 0.5 PPM (As Chlorides) Max. Sulfates None Dielectric Strength at 25C. 25 KV Min. Viscosity at 100F.(SuS) 10 Thermal Chemical Chlorid- 0.75 PPM es Max. 10,084 10,114 10,087 10,620 10,125 T-2092 11,608 11,607 T-2087 11,502 12,169 11,605 10,086 12,722 Every 1-2 days Same as blend tanks Every Load Same as blend tanks Tests made on electrical grade Aroclora only. Tests made on request only. Special customer test. Maximum range for all Aroclora including electrical and non-electrical grades. COMPANY CONFIDENTIAL TRAN 009288 HARTOLDMON0026683 Dept. 2*16 - Process Description ^ AROCLOR APPENDIX J Safety Equipment SAFETY tc TOXICITY DATA The following is a list of safety equipment (personal and departmental) required in department 2*<6. 1. Fire extinguishers: . A. Dry Chemical [}) - Southwest corner Bldg. CR - Main Floor. - - West wall at top of stairs of Second Floor. B. Carbon Dioxide Snow - Southwest corner of Bldg. CR, ground level. 2. Chlorine Oas Masks (*1) - Southwest corner, second floor - Control room, seoond floor - East side, outside control room - Wall, Southwest comer of sprinkler house, main floor. 3. Scott Air Masks - West of Lean-To 4. Safety Showers (2) - Southeast corner of Bldg. CR, ground level. - Southeast corner of Bldg. CR, 2nd Floor. 5. Davis Vapotester 6. Eye Baths 7. sprinkler system Safety Precautions The folliwing are safety precautions followed in the operation of department 256. . 1. Safety Equipment of Employee Each employee" has the following safety equipment: (1) Hard hat (2) Safety glasses (5) Goggles (4) Rubber and canvas gloves (5) Rubber overshoes. Special equipment may be issued as necessary for performing a particular Job in a safe manner. COMPANY CONFIDENTIAL TRAN 009289 HARTOLDMONOQ26684 Dept. 2^6 - Process Description AROCLOR *5. APPENDIX J SAFETY & TOXICITY DATA (Cont'd.) Safety Precautions (Cont'd.) 2. Sampling of Crude Aroclor *Tlie samples of Aroclor taken during the chlorination reaction are hot (170C.). Precaution must be taken to avoid skin contact of samples and Inhalation of Hydrogen chloride, Chlorine and Aroclor vapors. 5. PI res pi res may result from the Ignition of leaking gas, Xylene, Diphenyl, __ rags, paper, wood, etc. Automatic fire extinguishers and sprinklers have been Installed to combat fires. 4. Explosions " Explosions may be caused from accumulated pockets of natural gas or a rapid burning of Diphenyl In a closed container such as a Chlorlnator. Chlorinators are equipped with a 10" diameter pressure relief line with a rupture disc made to burst at 22 psi In ease Diphenyl within the Chlorlnator Ignites. 5. Toxicity Toxicity does not present a serious problem. However, a complete daily change of clean clothes Is supplied to each person and time Is allotted at the end of each shift to take a bath. Instructions are also Issued to avoid actual skin contact with Biphenyl and Aroclor as much as possible and to wash hands and face before eating. 6. Miscellaneous There are many accidents that can occur that may be classified as health and safety hazards. These accidents may result from such things as broken process lines, acid leaks, steam leaks, etc. The worst inherent hazards are as follows: . 1. Free Chlorine from ruptured line or major leak. 2. HCl Gas from ruptured line or major leak. J>. Dropping bottoms from stills. %. Hot Aroclor & Diphenyl. Safety Record The last lost-time Injury in Dept. 2^6 was January 28, 19^8. The frequency of minor injuries is low, around one per month. Toxicity: This material Is a liquid under normal conditions and has a medium toxicity range for liquid ingestion and high toxicity for vapor Inhalation. The maximum allowable concentration (M.A.C.) is 1 mg/cubic meter. Fire Hazard: There is no fire hazard under normal conditions.' Aroclor mixes (Xylene, Toluene, Butyl Acetate, etc.) may burn and explose at high temperatures when exposed to flames. . " COMPANY CONFIDENTIAL TRAN 009290 HARTOLDMON0026685 Dept. 246 - Process Description AROCLOR APfENDIX J 46. SAFETY & TOXICITY DATA (Cont'd.) Other Hazards: This material can cause dermatitis, systemic poisoning Prom the fumes, and yellow atrophy of the liver. There are skin, mucous membraneb and eye hazards encountered in handling this material. Treatment and Antidotes; Call a physician and remove patient from fumes. Storage and Handling: Protect the skin, lungs, and eyes by wearing approved protective clothing, respirator, and goggles. People who handle this material at elevated temperatures should have medical supervision, and the air should be sampled to insure compliance with M.A.C. There are no special storage restrictions under normal conditions except store in a ventilated area. ' - Shippingt There are no special shipping restrictions. FERRIC CHLORIDE (FeCl3) Toxicity: This material is a solid under normal conditions and is nontoxlc or has a rating as low. Fire Hazard: There is no fire hazard under normal conditions, but it will emit toxic fumes at high temperatures. Other Hazards: Some people are allergic to this material and may develop skin rash, and there is an eye hazard. Treatment and Antidotes : Cal1 a physician . Storage and Handling: protect the s.iin with approved protective clothing, avoid the breathing of FeCls dust, wear approved respirator with adequate cartridge, and protect the cyco wltn approved goggles. There are no storage regulations. Shipping; There are no shipping restrictions. DIPHENYL (C6HSC6HC,) Toxicity: This material is a solid at normal conditions and is medium toxic. The M.A.C. of vapor is 2 mg/cubic meter of air. If Ingested, the lethal uouc is 2.4 g/Kg of body weight. The fumes are not dangerously deadly, bufr-they are poisonous over a prolonged time. Fire Hazard: Diphenyl is very flammable and will burn when exposed to heat or flame or oxidizing materials. Other Hazards: the eyes. Diphenyl Is not too corrosive to skin, but it will affect ' COMPANY ` CONFIDENTIAL TRAN 009291 HARTOLDMON0026686 Dept. 2*t6 - Process Description AROCLOR ^7. APPENDIX J SAFETY & TOXICITY DATA (Cont'd . ) DIPHENYL (C6H5C6H5) (Cont'd. ) Treatment and Antluotes: Wash eyes with water and get the patient to Fresh air" Try"to";ct patient to vomit, and call a physician. Storage and Handling: This material can be stored In steel containers away from lire hazards and oxidizing agents. Wear suitable clothes and approved goggles when handling diphenyl. Ship in cars or other suitable containers with a red warning flammability. XYLENE (C6Hu(CH3)* Toxicity: This material Is a liquid under normal conditions arid Is very toxic in liquid or gaseous form, but it Is less toxic than toluene. The M.A.C. Is 200 ppm. Fire Hazard: This material Is very flammable and tne limiting explosive concentration is 1-5>J# by volume in air. it will also react with oxidizing agents . Other Hazards: This material will cause necrosis if enough is inhaled, and Is hazardous to eyes, mucous membranes, and the skin. Treatment and Antidotes : Oet patient to fresh air, and call a physician. If injested, get patient to vomit. Wash eyes and skin with water. Storage and Handling: This material should be stored In a cool well- ventilated area away from fire hazards or strong oxidizing agents. The material for storage can be steel cars or tanks. Wear approved protective clothing, respirator, and goggles. Shipping; Ship In containers of steel or appropriate material with a red label. TRICHLOROBENZENE: Toxicity; This material is a solid at room temperature and the vapors are quj te toxic. The solid is poison if Ingested. The M.A.C. is 50 ppm. Fire Hazard: This solid is flammable but is listed only as a moderate fire hazard. Will burn at M20C. or above. Other Hazards: This material will affect the liver, eyes, and mucous membranes. " Treatment and Antidotes: Wash eyes with water, and get patient to fresh _T_- (>aTi a physician. COMPANY CONFIDENTIAL TRAN 009292 HARTOLDMON0026687 Dept. 246 - Process Description 48. AROCLOR APPENDIX J SAFETY tc TOXICITY DATA (Cont'd. ) TRICHLOROBENZENE (Cont'd , ) Storage and Handling: Store this material in cool, well-ventilated area uway from hazards anu oxidizing agents. Wear protective clothing, chemical safe goggles and approved respirator. Shipping; Ship in steel containers like cars on tanks with red label. TETRA-TRI-CHLOROBENZENE Toxicity: This material is a solid at normal temperatures and is medium toxic. The M.A.C. of vapor is 50-75 ppm. Fire Hazard: This material is not a very great fire hazard, but it will burn at high temperatures and will decompose and emit chlorine. Other Hazards; This material will affect the eyes, akin, and mucous membranes. Treatment and Handling: Wash eyes and skin with water and get patient to fresh air. Call a physician. ' Storage and Handling: Store this material in a cool place away from fire hazards and strong oxidizing agents. This material can be stored in steel cars, tanks, or etc. Wear protective clothing, approved respirator, and chemical safe goggles when handling this material. Shipping; Ship this material in containers marked with a red label. LIME Ca(0H)a Toxicity; Lime is not dangerously toxic, and it is regarded as more of a nuisance. This material Is a solid or slurry. Fire Hazard; This material is not flammable. Other Hazards: Lime is very hazardous to the eyes. It will burn the skin also, and thedust will affect the mucous membranes. Treatment and Antidotes: Flood eyes and skin with large quantities of water. If lime is Ingested, get patient to vomit and call physician. Storage and Handling; Lime can be stored In steel containers, and people should wear protective clothing, respirators, and rubber or chemical safe goggles when handling lime. Shipping: There are no special restrictions for shipping, but the containers should have a white label, a caustic warning. COMPANY CONFIDENTIAL TRAN 009293 HARTOLDMON0026688 Dept. 246 - Process Description AROCLOR *9. APPENDIX J SAFETY tc TOXICITY DATA (Cont'd.) ATTAPULGUS EARTH: . Toxicity; Tills earth ia not toxic In general. Fire Hazard; There la no fire hazard. Other Hazards; Attapulgua earth can create a duat hazard similar to other dusts that contain silica. Treatment and Antidotes: Consult a physician. Storage and Handling: Attapulsug earth presents no special storage problem and Bhould be handled by persons wearing an approved respirator. Shipping: There are no special restrictions on shipping. HYDROGEN CHLORIDE (HC1) Toxicity: This material is a gas under normal conditions and is very toxic. The M.A.G. is 5-10 ppm and a concentration of 1500-2000 ppm would be fatal to humans in a few minutes. Fire Hazard: There is no fire hazard under normal conditions, but wet gas reacts with some metals to form hazardous hydrogen. Other Hazards: This material is hazardous to teeth, skin, eyes, and mucous memoranes. Treatment and Antidotes; Wash profusely with water, if invested, eat chalk, magnesium hydroxide, egg whites, and milk, and also administer oxygen. Call a physician. Storage and Handling: This material should be stored in a cool, well ventilated area away from oxidizing agents. This material can be stored in rubber lined, glass, or tantalum vessels. People handling this material should wear suitable clothing like rubber aprons, shoes, and gloves. Also rubber goggles or chemical safe grades and approved pack or canister gas masks. Shippings Shipping containers must have a white warning label and a non-flammable label. Ship in appropriate containers such as rail car or carboy. CHLORINE (Cl.) Toxicity: This material is a gas under normal conditions and is very toxic. The M.A.C. 18 .55 to 2 ppm. A concentration of 1000 ppm would be rapidly fatal. Least concentration with detectable odor is 5.5 ppm r" COMPANY TRAN 009294 CONFIDENTIAL HARTOLDMONOQ26689 Dept. 2^6 . Process Description 50. AROCLOR APPENDIX J SAFETY k TOXICITY DATA (Cont'd,) CHLORINE (Cl.) (Cont'd. ) Fire Hazard: There is no fire hazard under normal conditions, but there ia an explosion hazard if ohlorine is mixed with a strong reducing agent such as hydrogen or hydrocarbons at high temperature. Other Hazards: This material causes eye, skin, and mucous membrane irritation. Treatment and Antidotes: The patient should be given oxygen immediately and treated for shock. Call a physician. Storage and Handling: This material should be stored in a ventilated and cool place away from fire hazards. When handling, wear a gas mask or approved respirator, clothing and rubber or chemical safe goggles. In strong chlorine concentrations, wear canister gas masks, Scott air pack, or oxygen breathing apparatus. Shipping: The shipping containers must have a green gas label and a hon-iTammable label on. Ship In steel cars or oylinders. COMPANY CONFIDENTIAL TRAN 009295 HARTOLDMON0026690 Dept. 246 AROCLOR APPENDIX K BACK GROUND INFORMATION 51. The manufacture of Aroclors was developed quite by chance. The Indian Refining Company, dn the latter part of 1926, approached the Swann Chemical Company located In Anniston, Alabama, regarding the production of Biphenyl which the Indian Refining Company wanted to use as a heat transfer medium. The Swann Chemical Company agreed to produce Biphenyl, but first a process had to be developed. Two years later, in 1926, a pilot plant for producing Biphenyl became operative. However, in the meantime, the Indian Refining Company dropped all interest in Biphenyl. Since a process had been developed for manufacturing Biphenyl, the Swann Chemical Company started looking for other outlets for this material <, The simplest outlet was in the form of Chlorinated Biphenyls which were produced in the laboratory in 1929- The Chlorinated Biphenyls produced exhibited good electrical properties. This was reported to the Oeneral Electric Company who Immediately became interested in the product which ultimately developed into large scale consumption In electrical transformers and capacitors. The trade name "Aroclors" was adopted for the Chlorinated Biphenyl products. The properties of Aroclors vary from mobile oily liquids to fine white crystals and hard transparent resins. The excellent electrical properties, fire resistance and inertness of the Aroclors make them useful for many applications. plant equipment was Installed to produce Aroclors at a rate of >000 pounds per day or 1 million pounds per year. In the following years, this production rate was insufficient to meet the Increased sales requirements. The Swann Chemical Company was purchased by the Monsanto Company in 1955 This purchase gave Monsanto access to the patent rights for the production of Aroclors. - production Capacity needed to be expanded, and since Monsanto had a Chlorine Plant at plant"B" (now called the W. 0. Krummrich Plant), the Aroclor production was transferred from the Anniston Plant to the Monsanto, Illinois Plant, where operations at an increased productive capacity started In September, 1926. By 19*10, the Krummrich Plant production capacity was Inadequate, and in 19*11, a similar production unit was installed In the Anniston Plant. company CONFIDENTIAL TRAN 9"6 HARTOLDMONOQ26691 Mor3unto Company Monsanto, Illinois Accepted by production WBJ Messrss F. E. Heisler - WOK E. E. Martin - WGK R. W. Bucknell - Org. Res. . SAFETY REVIEW COMMITTEE Original signed by* CWR 2-19-64 ODD 2-20-64 HBF 2-10-61 January 17# 1964 " K. L. McHugh - Org. Res. Process Holders TENTATIVE AMENDMENT NO. "A" TITLE: Aroclor Standard Manufacturing Process of Dec 17, 1962 811.01 - Bll 07 . OBJECTIVE: Increase amount of Ferric Chloride Catalyst added to the Biphenyl in Dept. 246, Aroclor. PRESENT PRACTICE: Presently 1 lb. of ferric chloride is added to the biphenyl charge tank to 4000 lbs. of biphenyl. It is suggested that this amount be increased to 2 lbs. of ferric chloride per 4000 lbs. charge of biphenyl added to the charge tank. It has been shown in the St. Louis Research Reports Nos. 1640 and 2072 that a minimum level of Fe Cl catalyst is 0.0J$6 to produce stable Aroclors. Aroclors manufactured at the W 0. Krumorich plant do not meet specs. by as comfortable a margin as Anniston's Aroclors do. If we are to retain our customers for electrical-grade Aroclors at W.G.K., the quality must be Improved. Safety will not be affected in any way. This will be a permanent procedure change. W. B. Johnson COMPANY CONFIDENTIAL TRAN 009297 HARTOLDMON0026692 Tentative Amendment No. "A1 APPROVAL: Original signed by; P-. T^Heirfer^^SaiT E. E. Martin l. E."Martin - WoK" b\ B?'Hoemera?eiT~C' b. p. <i. (Cont'd.) DATE:. 2/11/64 I5aTe -D-ajtei/n/M ,, , 2/1*1/611 Date . W9/b* Date COMPANY CONFIDENTIAL TRAN 009296 HARTOLDMON0026693 DISTRIBUTION LIST: 1. H. L. Minckler/R. S. Wobue - Oen. Offices 2. R- E. Soden - WOK 5- T. W. Dalton - WOK 4. . J. R. Kellogg - WOK 5-6. st. Louis Research 7. Vital Records Center 0. WOK Standards Department 9. WOK Technical Services 10. Vault Copy 11. England 12. England 15l4. Anniston - R. 0 Moody 15-16. Extra . May 9, 1965 ' TENTATIVE AMENDMENT NO. A PROCESS DESCRIPTION FOR THE MANUFACTURE OF AROCLOR IN DEPT. 246 "DE^MBER'TTTTggr'^nyTir. KrUmmAiUFTLa^t, Monsanto, Illinois SUB-TITLE: Preparation of Aroclor 1252 by the direct chlorination process common to Aroclor 1242, 1248, 1254, 1260 and 1262. PRESENT PROCESS: Aroclors are the reaction products formed by the chlorination of diphenyl in the presence of iron chloride catalyst. The crude Aroclor, produced in the chlorinator, is air blown, distilled over calcium oxide treated with Attapulgus earth, filtered, and transferred to storage PROPOSED CHANCE: Amend the existing manufacturing process to include the production of Aroclor 1252, which contains high percentages of dichDorobiphenyl, to be used in the large scale preparation of MCS 177, a 700-800c>F. heat transfer fluid. Aroclor 1252 is prepared by the direct chlorination of diphenyl to a specific gravity of 1.252 to 1.256 at 050/15.5C. in the presence of iron chloride catalyst. The crude Aroclor 1252 is air blown, and distilled over calcium oxide prior to transfer of the product into storage containers at 50 to oOC. Insoluble isomers, present in this special Aroclor 1252, slowly separates out of solution upon prolonged standing at room temperatures and are very difficult to redissolve. Since this product is a starting material for the MCS 177 process, the Attapulgus treatment and final filtration are optional but not necessary. COMPANY CONFIDENTIAL TRAN 009299 HARTOLDMONOQ26694 -2- Tills special Aroclor 1252 cannot be back-blended If the finished product is off on its prescribed chlorine specifications The JncorporatIon of excess monochloroblphenyls Into the product will increase the volatility of the MCS 177 and the addition of trlchloroolpheny1b will drastically raise the pour point of the finished heat transfer fluid. Abnormal compositions of this Aroclor 1252 are readily detectable by gag-liquid chromatographic analyses. Approval 18 requested to demonstrate this change as a source of the necessary starting material for Monsanto's candidate, in the lucrative field of high temperature heat transfer applications. ORIGINAL SIGNED BY: ' Written by J. D. Sullivan J. J)."Sullivan Date_________ 5/9/65 Approved By: Original signed by; W. R. Richard_________W. R. Richard p. E. Heisler P. E. Helsler E. E. Martin_______ E. E. Martin Safety Review Committee; COMPANY CONFIDENTIAL TRAN 009300 HARTOLDMON0026695 1. R. S. Wobus 2. C. Barbre 2. T H. Becker 4. J. Soffranko 65-. St. L. Res. Lib. St. L. Res. Lib. 7. Plant B 8. England 9. P. 0 Marsh 10. Plant B 11. Plant B 12. Plant B 12. H. L. Hubbard 14. J. Mltoray TENTATIVE AMENDMENT AROCLOR PROCESS January 22, Dept. 246, Plant B This amendment provides for the addition of anhydrous FeCls, 0.}# by weight of biphenyl, to the chlorinator as fortifying catalyst for the production of Aroolor ll60 This change in process operation is' a result of a complaint submitted because of the presence of green color in Aroclor 1260. Research work has indicated a trend toward improved color when anhydrous Fed* 1b used either alone or in combination with plant steel catalyst. To cite an example, using 5# by weight plant steel catalyst, an untreated Aroclor 1260 was prepared in the laboratory having a color of $6% Transmission (Fisher Electrophotometer, filler 425B), whereas from a batch in which the same catalyst plus 0 2# by weight anhydrous FeCls was employed, an Aroclor 1260 of 72# Transmission was obtained. Extensive analyses of the Aroclor 1260, which was prepared using plant steel in conjunction with 0.2# by weight anhydrous FeCls, did not indicate any abnormalities or deviations from usual quality material. A complete summary of the Research work is presented in a memorandum to Dr. R. M. Hitchens, January.24, 1951. It is proposed to condut a plant demonstration which will comprise the production of three to four chlorination batches of Aroclor ll6o using 0.2# by weight of the bjphenyl charge as anhydrous FeCls. Depending on the outcome of this plant trial, that is, if a color improvement is observed and a normal quality product is retained, a run of longer duration will be planned to study further the effect of anhydrous FeCls catalyst on the color of Aroclor 1260. This may Include variations in the amount of FeCls charged to the chlorinator. In January 24 1951 APPROVED: Original signed by: Original signed by: ' j. p. Mltoray -j y Mltoray - COMPANY CONFIDENTIAL riwr1- iasSh T. WT,bait'monl&wi C. Barbre C. Barbre __________ 6/25Z51________ Date n. B. Hosmer E>. B. Hosirier-------- Paul q Marsh P. G* . MaFrsih/ 1 TRAN 009301 HARTOLDMONOQ26696 SAFETY REVIEW COMMITTEE Original signed by s _10,,R_el7 ___ JLJLJL. ,,10-0e,7 ___ -__________________-JLQ-Q-C'7 September 27# 1957 Distribution: Dr. 0. J. Welnkauff - Research R. S. Wobus - Roberts Bldg. T. M.Patrick - Research A. M. Ellenburg - Research T. W. Dalton - WOK J R. Kellogg - WOK Process Holders TENTATIVE AMENDMENT NO. B Title: Aroclor - Standard Manufacturing Process Objective: This amendment covers changes in the chlorination step of the Aroclor process; In particular, it suggests that the batch of biphenyl be circulated in the chlorinator during the entire period of chlorination, and that a temperature of 1J0-150C be maintained during the whole chlorination Previous Practice: In the Manufacturjng Process, no definite temperature is described for the start of the Chlorination. For the biphenyl measuring tank a temperature of at least 85C., is recommended and as a "finishing temperature" a range of 120-1J5C is described for Aroclor 1242 and 1248, a "finishing temp erature " of 120-150C., for Aroclor 1254, 1260 and 1262. The circulation of each batch in the chlorinator is started after the first four (4) hours of the chlorination (approximately half of the total chlorination time of Aroclor 1242). Proposed Amendment: The biphenyl charge will be heated to at least 115-120C., in the measuring tank. After charging the chlorinator, circulation will be started before the chlorine feed is begun to allow distribution of the ferric chloride catalyst. The temperature of the chlorinator should be brought up to 1J0C. in a minimum time usually 20 to JO minutes after the chlorine introduction The chlorination of bJphenyl to all liquid Aroclors should be carried out at a reaction temperature of 1J0-150C. COMPANY CONFIDENTIAL TRAN 009302 HARTOLDMON0026697 Tentative Amendment No. B -2- September 27, 19^,7 Proposed Amendment (Cont*d.) NOTE: In order to mechanically reduce losses due to sublimation and en trainment, It la suggested that the circulating line introducing the charge into the top of the chlorination be extended to the surface level of the biphenyl charge. Thli will prevent the reaction mix ture from being sprayed into the exit gas stream and should ell mlnate some entrainment. Justification; Laboratory experiments and actual plant runs have Indicated that catalyst concentration and reaction temperature are Imperative for the production of an end product of good quality. (Final Report No. I6M0, October 22, 1956 "by H Merten, Progess Report No. 5; Job No 3*128 Code IND PL, of August, 1957 by H Merten and A. M. Ellanburg. Circulating each biphenyl batch from the beginning of the chlorination should facilitate the production of a more uniform material, since a better contact of the biphenyl charge with the catalyst at the start of each chlori nation is made possible. The catalyst will be distributed more evenly and hot spots will be eliminated. The production of Inferior Aroclor caused by too low a chlorination temp erature of deficient catalyst distribution would be avoided by changing the present Manufacturing Process according to this amendment. In addition to the data obtained by laboratory experiments (described above) the following Table I Illustrates the effect of temperature changes on the quality of the end product of actual plant runs (shown by stability chloride values). Table II indicates the improvement In the stability of different Aroclors produced by circulation of the batches during the whole chlorination period compared to runs carried out with catch circulation after the lapse of a four-hour chlorination period. TABLE I Batch No. Temperature Low . High Stability Chloride ppm./l6 hrs 319 9k 116 320 110 129 321 133 1*5 0.80 0.71* 0.M9 COMPANY CONFIDENTIAL TRAN 009303 HARTOLDMONOQ26698 Tentative Amendment He.___ B -3- September 27, 1957 TABLE II Circulation Aroclor No. after 4 hours after 4 hours entire period entire period after 4 hours after k hours entire period entire period . 125ft 125^ 125^ 125^ 1260 1260 1260 1260 Lot No. T-631 T-632 T-635 T-6>6 T-104M T-1045 T-1048 T-10^9 Stability Chloride ppm./16 hrs. .85 .89 .*5 .52 .57 .39 .*5- precautions: No Increased toxicity or safety hazards will result from this procesi Extent of Demonstrations: It is suggested that this amendment be incorporated in the standard Manufacturing Process as soon as possible. Original signed by* h. L. Merten H. L. Merten Research Department In Approved: Original signed byj j. R. Kellogg *---------- J. R. Kellogg" A. M- Ellenburg A. M. Ellenburg T. W. Dalton T. W Dalton T. M. Patrick, Jr. f. M. Patrick COMPANY CONFIDENTIAL TRAN 009304 HARTOLDMON0026699 Safety Review Committee ORIGINAL SIGNED BY: H. L. Hubbard 5/18/ 57 R. H. M. 3/16/57 R. E. Howard 5/18/57 March 15, 1957 Distribution: Dr. a. J. Welnkauff - Research R. S. Wobus - Roberts Bldg. H. L. Hubbard - Research A. M. Ellenburg - Research T. W Dalton - WOK J. R. Kellogg - WOK Process Holders Tentative Amendment No. A Title: Aroclor - Standard Manufacturing Process for Department 2*16, W. 0. Krummrich - Revised 5/15/55 - 0. N. Schwartz. Objective: This amendment covers process changes in the chlorination step of the Aroclor Process, Section V Part B, concerning the Catalyst. Present Practice: The biphenyl charge is dropped by gravity to the #1 2, 5 4 or 5 chlorlnators. The chlorlnators are constructed of steel and are 5 feet in diameter x 16 feet in height. For catalyst, they contain an 8 foot bed of coarse steel turnings which have been burned free of oil and moisture over an open gas flame prior to their introduction Into the chlorinator. Additional catalyst is added to the chlorlnators as required. Normally, this is not necessary more than once a year. Proposed Amendment: In addition to the present catalyst source, each chlorinator batch of 5600 or *1000 pounds of biphenyl will be charged with 2 pounds of an hydrous ferric chloride before the chlorination begins. Justification: Experience has shown that various degrees of unstable Aroclor can result at times from the present method of supplying catalyst to the chlorination step. The use of FeCl has been investigated and found to give a very stable product when used in the suggested purport ion The complaints from Oeneral Electric Company on Aroclor 12*12 re garding the instability of certa n material produced in July and August, 1956, make it mandatory that we maintain our Aroclor quality at its maximum at all times. TRAN 009305 HARTOLDMON0026700 March 1? 1957 Tentative Amendment No.A Precautions: No Increased toxicity or safety hazard will result from this process change Ferric chloride Is highly hygroscopic and Is acidic In nature, therefore care should be tanke to prevent contact with skin or clothing. Extent of Demonstration: The process change has been demonstrated at Anniston. This amendment will be a permanent change and should be Incorporated in the next revision of the manufacturing process. Approved: Original signed by J. R. Kellogg J. R. Kellogg A. M. Ellenburg Organic Research Group Leader A. M* Ellenburg A. M. Ellenburg T. W. Dalton T. W. La1ton In F. B. Zienty >19-57 T. M. Patrick for t* M. Patrick COMPANY CONFIDENTIAL TRAN 009306 HARTOLDMON0026701 Monsanto, Illinois June 8, 1959 CC: C. M. Edelblut - AnniBton J. Clegorn - Anniston Safety Review Committee Original signed byj T.M.P. 6-12-59 R ff.H 6.-12-59 .R*JLJLu <*-15-59_______ Messrs. T. W. Dalton T, m. Patrick - Research M. Ellenburg - Research H. S. 'Scott Process Holders PROCESS AMENDMENT - AROCLORS geprrrw- w, q nrrTOwr-- Title Modification of chlorination temperatures for Aroclor production Purpose *0 provide chlorination temperature ranges that are more compatible with plant conditions Old Procedure Biphenyl chlorination is performed at tenperature range of 150 to 150 C. Proposed Procedure Initial" chlorination of Biphenyl may be started at a minimum temperature of 95C. provided that 120^0 is reached within 1/2 hour. Chlorination may be continued for the next tow hours at a temperature no less than 120C. Completion of the batch will then be controlled between 150 and 150C. Reason and justification 0 Formal Biphenyl storage is maintained at approximately 95 0. to keep safely below the flash point. Therefore to adhere strictly to the process would require heating of the batch to 150C. before chlorination. This results in production delays and increased Biphenyl pluggage in chlorlnator off gas lines. Based on plant experience most chlorinators are recharged while still hot from the preceeding batch; this normally yei Ids a starting temperature in the range of 120C. However, occasionally delays cause charging to a cooler chlorlnator where the net temperature may approach 95C. This proposal would allow chlorination to start immediately under these conditions The batch temperature would then rise rapidly from its own heat with water being applied later to line out the temperature somewhere slightly above 120C. A lower temperature range 120 to 150C. is needed for the first two hours to reduce Biphenyl carry-over into the off gas lines. COMPANY CONFIDENTIAL TRAN 009307 HARTOLDMON0026702 -2- ThJb proposed process ammendment has tentative approval from Research. In Original Signed by? ' T. W Dalton T. W. Dalton -------------- A. M. Ellenburg M> Eiienbiarg " J. R. Kellogg _________J. R. Kellogg ` J. ft Kellogg T. M. Patrick 6-12-59 T._M Patrick COMPANY CONFIDENTIAL TRAN 009308 HARTOLDMONOQ26703 Dept. 246 - process Description AROCLOR APPENDIX L TIME CYCLE 52. The design capacity of the department Is 1,700,000 (2,400,000 after August, 1964) pounds per month, or 20,400,000 pounds per year. Figure 1 of this section Illustrates the flow pattern of the Aroclor process and lists the approximate time needed to complete each process step. The time table for the Aroclor process Is summorlzed below: Operation Equivalent pounds Time (hours) of Finished Product Charge Chlorlnator Chlorination 1242 1248 1254 1260 Transfer to blow tanks Aeration D3 stlllation 1242 1248 1254 1260 Blending Filiering Dropping to Storage .25 8.70 9.20 11.10 12.50 .25 2.00 1.75 1.75 1.75 1.75 2.00 2.00 2.00 6550 7200 8o40 9100 The time required to make completed batches of the various Aroclors are tabulated below: Aroclor 1248 1254 1260 Batch Time 19.45 21.55 22.55 (hrs.) --------- Process operations including filter press cleaning, sampling, etc. are independent of the batch completion time cycle because production time is not lost. COMPANY CONFIDENTIAL TRAN 009309 HARTOLDMON0026704 r Figure 1. AROCLOU f'OV SHEET "IT1! MATCH CITE AH" WITS | Cl, BJ Ml phenyl Change Tank rw (la 8. 5 Clilorlnaton To Plow ~anks 3300 Cal. Two M! I Is J TR"ece I vers 1000 Cal. 1.7 ^ Lbs,/Mo. HATE ' : . Charge: *000 lb. *70 *a8 ! for 11*3. 11*8, 119* i ans ll6o. Takes li minutes to charge and discharge. . ! Capacity: 700 Oat. ' L ; . 3.5* 5 RATH 11*3 II-.R . ;*-o l.T S l.hs./ln. UQ OST _ f.*oo a. . 990 oa:.. is hi". 'i *> nrnJ . *.-' 'I Oil.. 13UHI-. I. a . . . - oil.. t . . ' j;!^. * - * *L` 1 . *-*- ' . , I III . rtn. o ..n, '**. * t-rr Charge: *,Hi0 Uri. *70 <Jal11'.:*: .*.: Ml l. .*0 *. |S !> . 1:s : *.: * .*. ; #.. * ft 1 1 * * 1 i . 8. -.I'. P! "> . 1 imj! r . '. * *i b ft- I.f ^ 1 , /Mu. 0~T I */ 5 T>* ,/Vo. yOf QT.T AVWF. F^ch batch ts blown Tor ? is*?: 53.5 htb . :*o'.ooo O'!i *-*'11 oro tn hour4*. cine Ismt 5 a a *low or 13,000 Col. irr:7^6 7n?o 5*50 i>5O0d t*nv en-S one tank I ?**,: 5/ .2 H>!> . 150.000- 13*';:''* ?r'30 5'50 63000 - ! ! I.- U... or 13,800 Cal. 135*:307 3' 3': *900 6500(1 I?*.': MM.'J HI n - I'Ml.OOO I36C:'03 3' 30 *050 CXXXf !!., or 1*.>00 Cal . I7ji.; /mn urn 15,300 O t.i-s. vo. (T.T lc., or 15,300 dal CC 5 8:s.SmSbcf ' 175^-; T.".r r'.-: *0.9 hi n ' '!?*?:510 8^0 7*50 fttooc 1 13*5:*o* 58 60 8500 85BOX 13*.* : >.-.c III h ' I35*:3<3 8160 7CK50 8BO<X ' 1 ?f>: *y. 0 HIP l3^0:3^3 58 GO 6750 0bO<X ---S--i-x---L--e-a--d--in--g--11 , , . |two m t Stations JP- 1111 ' Sis Storage Tsro.3 - # 1 To Product Tanks 3000 qnu^-- "TwoTfeikl Tanks 3000 Cal. 1 Hn Dram Off It lake.-. hners One Tank Trailer , to ml X I.'sex* OS I . Hour Tank Car(One for Wnloadlng) 13*3: *; and fj, 15CU0 Oal. Each Capacity: 13 MfD of 3000 1.7 ^ Lt-s./Ho. 90? onr ' 13*.1: 3 ). JOO 0*1. 13*.*: *. 16. 500 Oal. I3C0: * , 30,000 Oal. ' * i Cal. I Two Race I -.era to a Batch. ' 3000 Cal. Batches - 3 HP!) . J BPD ~nr*icEf:n r Cxcacttyi 13 *1D j __ . _ _ __ _ . _ 3.V* C ;<b/ko. '-fft OST HI M f Hours l-er Match I. Charge, chlorlnolc and er>t ty. -3. A still Latch la 33 ehlortnaVor 01 h - f*"T n\ M |':!1 I1 ": .3" lillrln. Matches I i-r *>.y 8 n Tim; O-i'. . |..r < r.irrte (ur 1.1; . ! -r ,, 1 uui.Jj ic:* ja. to-: - /i 11 COMPANY CONFIDENTIAL TRAN 009310 HARTOLDMON0026705 51. Dept. 246 - Process Decription AROCLOR APPENDIX M QUALITY CONSIDERATIONS . The Aroclor compound* are among the most versatile chemically-made materials in industry, Aroclor* are useful in many way* because of their outstanding inertness. Aroclors are used alone for particular physical jobs such as insulating, heat transfer, sealants, and expansion media; and they are used as com , ponents or extendors in elastomers, adhesives, paints, lacquers, var nishes, pigments and waxes. Aroclors must be highly pure, with dependably minimal traces of electro lytes for use in electrical applications. Electrical grade Aroclors must pa** numerous stringent specifications. The following tests determine. Aroclor quality: Hydrolysis stability Measure of chemically unstable chlorine compounds. Munch or Monsanto Stability Test Measure of thermally unstable chlorine compounds at elevated temperatures. Thermal Chemical Chloride Developed by the General Electric Co. to measure chemically and thermally unstable chlorine compounds. Resistivity Measure of insulative properties. Power Factor Measures power loss due to current through a capacitor. Dielectric Constant Measure* the capacitance of a standard such as air compared to the capacitances of Aroclor. Specific Gravity, : refractive index Measures of chlorination level. ' The stability and electrical properties of electrical-grade Aroclors are paramount in quality considerations. The chlorination step of the process is most critical because many properties of the final product are deter mined by the properties of the crude Aroclor, Condition* in the chlorinator needed for a good quality product are: 1. Chlorination Temperature - The chlorination temperature must be greater thanU20*G4``At the beginning of the chlorination reaction to produce stable Aroclors. Results of research tests indicate that ' product stability is better as the initial chlorination temperature is increased. COMPANY CONFIDENTIAL TRAN 009311 HARTOLDMON0026706 5. Department 246 - Process Description AROCLbR APPENDIX M QUALITY CONSIDERATIONS 2. Ferric Chloride Concentration - Research ha* found that the ferric chloride concentration must be at least 0. 03% to form stable products. Research recommends 0. 05% ferric chloride. Lower catalyst ratioB result in increased "addition" chlorination as opposed to "substitution" chlorination, indicated by higher chloride values and lower yields. The isomeric distribution of the final product is a function of the type and concentration of the catalyst used in the reaction. Homogeneous suspension of the catalyst is extremely important. Good catalyst contact can not be attained without homogeneous suipension. Since ferric chloride does not mix well with biphenyl, the dry catalyst must not be poured into the chlorinator. 3. Geometry of Reacting Vessel - The shape of the reactor affects the circulation and flow pattern of the reactants, It is suspected that the chlorine ga6 channels through a void space. in the existing catalyst basket. This problem is presently being studied. The reactor must be designed such that circulation of reactants is rapid and homogeneous and local over-chlorination does not occur. 4. Cleanliness - The ferric chloride catalyst settles to the bottom of the chlorinator. Areas of the packed bed become plugged with ferric chloride and channeling of reactant flow may result, A steam clean-out of the chlorinator may be an expedient method to remove the ferric chloride. This method was tried in the department, and evidently was successful. Further tests by the laboratory will verify the effectiveness of a steam clean-out. 5. Sparging - The sparger controls the gas distribution under the cata lyst hold-up plate and the size of gas bubbles. It is not known whether the catalyst basket or sparger or botlvare^the critical fa^ter^^in achieving the proper flow of gas through the reactor. It is believed that the sparger should distribute small bubbles give good gas dis tribution throughout the chlorinator. The small bubbles have a greater surface area per unit volume of gas for mass transfer,` and this should increase, the'rdafetidn rite'.. .* : 6. Raw Material Purity - The purity of raw materials can affect the quality of Aroclors. Sulfates are particularly harmful in the chlorine gas. It is suspected that sulfates poison the ferric chloride catalyst and Sulfonate .some of the biphenyl. If the ferric chloride cata lyst is . poisoned, the effective catalyst concentration i^reduced atfd^thue un- _ stable aroclors will be produced. The chemistry and mechanism of o catalytic poisoning are not known for certain. Sulfonated biphenyl is carried-over during distillation and is not removed by earth treating. TRAN 009312 COMPANY WFIDENT/AL HARTOLDMON0026707 55. Dept, 246 - Process Description AROCLOR APPENDIX M QUALITY CONSIDERATIONS 6. Raw Material Purity (Cont 'd.) Sulfonated biphenyl has ionic properties which lowers the resis tivity of the finished product. A Brink Mist Eliminator has been installed in Dept. 246 to eliminate the chlorine impurities. 7. ,, Earth Treatment - The factors affecting stability also influence the electrical properties of Aroclors. An absorbent will be inef fective if the Aroclor was not prepared in a manner such that a stable product was formed during the chlorination reaction. However, research has found that absorbents are very effective for improvement of electrical properties by removing ferric chloride and tars carried-over during distillation, provided the crude Aroclor has good stability. The absorbent used in Dept. 246 (after distillation) is Attapulgus Earth; .. the concentration should be 0.05% for Aroclor 1242 and 0.1% for other Aroclors, The earth must be heat treated at 250*C. for a minimum of 4 hours before addition to the Aroclor. Heat treatment reduces the moisture and activates the earth. * * \ 8. Lime Treatment - It is important that proper amount of lime (250 pounds per still run) be added to the still to prevent sublima tion of ferric chloride. 9. The blend tanks, finished product tanks, and Aroclor 1242 and 1254 storage tanks are blanketed with nitrogen gas. Nitrogen blanketing maintains the electrical properties of the Aroclors by preventing corrosion of the equipment. ,, , In summary, the chlorination step of the process is the most critical. A good quality Aroclor can not be produced if a stable compound is not formed during chlorination. Once a stable compound is formed, other techniques such as use of lime, absorbents, and nitrogen blanketing are used to maintain and improve electrical properties. Cr&PANY C0HFiDENTlAL TRAN 009313 HARTOLDMON0026708 Dept. 246 - Process Description AROCLOR 56. APPENDTY M QUALITY CONSIDERATIONS (Cont'd.) Absorbents Numerous absorbents have been screened in the laboratory at various contact temperatures' for their effect on resistivity of plant untreated Aroclor 1242. The most satisfactory absorbent pound for improving the resistivity of Aroclor 1242 was LVM attasorb. Table I of this section lists the laboratory results of the different absorbents used to treat Aroclor 1242. Degradation of Aroclors Degradation of Aroclors, which leads to loss in eleotrical resistivity, is one of the short comings of using Aroclor as a dielectric, especially since only a very minor degradation can cause a serious breakdown in electrical equipment. The thermal degradation of fractionated Aroclor has been measured at 250C. and the amount of Hydrogen Chloride liberated was measured. The results of these tests are listed in table II of this section. 0 * Aroclor 1242 has been degraded by ultraviolent light, and the decrease in electrical resistivity with irradiation time was measured. The plot of resistivity versus time of irradiation (Figure 1 of this section) resembles a conductivity versus oonoentration curve for a weak electrolyte. It is possible to remove the conducting material brought about by photo-degrad ation, and restore the resistivity to its original value by passing the degraded material over activated alumina. Thermal degradation of Aroclors is minor compared to photo chemical degradation. Thermal treatment causes release of a small amount of hydrogen Chloride Initially, but this evolution ceases after a short time. Such behavior is attributed to thermal degradation of impurities. If Aroclor is irrodiated, then exposed to a thermal treatment, appreciably more HC1 is liberated. COMPANY CONFIDENTIAL TRAN 009314 HARTOLDMON0026709 Dept. 246 - ProccBB Description AROCLOR APPENDIX M 57. QUALITY CONSIDERATIONS (Confab TABLE I ADSORBENT SCREENING DATA Adsorbent Adsorbent Pretreatment Contact Temperature C. Volume Resistivity ; 1 at 100c. ohm-cm. x 10 LVM Attapulgus Earth ' None LVM Attapulgus Earth LVM Attapulgus Earth. LVM Attapulgus Earth. Attasorb - LVM Heated at 250C 12 hours. Heated at 350C 12 hours. Heated at 350C A hours. None Attaclay None Activated Alumina (Alcoa Grade F-3 -325 mesh) None Voclay 325 (Western Bentonite) Panther Creek (Southern Bentonite) Filtrol Grad 1 Zeolex 7 (Zeolitej Florite 00 mesh (Activated Bauxite) Suprex L-G (Kaolin) Attasorb - LVM Attasorb - RVM . None None None None None None Heated 350C.12 hours. None 60 80 100 120 60 Bo 100 120 6o 80 100 120 60 8o 100 120 60 8o 100 120 80 100 120 60 80 100 120 BO 100 120 80 100 120 80 8o 100 ^< ss 100 oO 100 100 TRAN 009315 34 oo 2000 2800 2900 4200 6400 7200 6100 9500 9000 6300 6300 2400 5600 6000 5700 9700 12,100 13.700 17#800 10,200 5400 6000 2100 2500 2800 3100 5700 380 9700 6200 11.300 6100 2600 7000 3600 4500 12,200 '6,200 HARTOLDMON0026710 Dept. 2^6 - Froceae Description aroclor APPENDIX M 58. QUALITY CONSIDERATIONS (Cont'd . ) . Adsorbent Linde Molecular Sieve Type 4-A Laminar Alumina (Dayton) TABLE I (Cont'd.) Adsorbent Pretreatment None Contact Temperature C. 60 None 60 Volume Resist at 100C. , ohm-cm. x 10 2100 900 Note: Resistivity of Aroclor before treatment -lx 1CT ohm-cm. COMPANY CONFIDENTIAL TRAN 009316 HARTOLDMON0026711 Dept. 246 - Process Description AROCLOR APPENDIX M QUALITY CONSIDERATIONS Aroclor 1221 1252 1242 1248 1254 TABLE II THERMAL DEGRADATION OF AROCLORS AT 250 C. gm. of HCl/gm x 10^ 3.35 6.73 11.07 3.91 6.42 9.81 5.96 9.58 13.00 3.61 5.44 8.48 3.^3 3.?6 6.43 . Heating Time 1 hr. 2 hrs. 5 hrs. 1 hr. 2 hrs. 5 hrs. 1 hr 2 hrs . 5 hrs. 1 hr. 2 hrs. 5 hrs . 1 hr. . 2 hrs . 5 hrs . 59. COMPANY CONFIDENTIAL TRAN 009317 HARTOLDMON0026712 f*)*Io HARTOLDMON0026713 COMPANY CONFIDENTIAL. i t j120 IKO IcO 60. Dept, 246 - Procen Description AROCLOR APPENDIX N MISCELLANEOUS REFERENCES 1. St. Louie Report No. 2694, Job No. 171-1028, February 15, 1952. Title: Operation of Aroclor Still# At Increased Pressure For Increased Rates ~ Summary: Distillation runs were mads at 20 to 30 mm Hg. The rate of Distillation of 1200 series Aroclors increases with pressure. 2. St. Louis Report No. 2755, Job No, 2-02-760. 01 - 3948-3 March 6, 1961. . Title: Improved Aroclor 1242 Studies Summary: Studies were carried out to determine the effect of temperature, chlorine content, and catalyst concen tration in chlorinated biphenyl mixtures. 2, 4-dichlorobiphenyl is the percursor of the high dielectric constant, trichlorinated components. 3. St. Louis Report No. 2072, Job No. 2-02-750. 01-3428, May 4, 1958. Title: Final Report on Aroclor Process Studies. Summary: Purity of raw materials, catalyst concentration, reaction temperature and rate of chlorination were the variables studied with respect to their influence on the stability of the finished product. 4. St. Louis Report No. 2540, Job No. 171-616, December 28, 1958. Title: The Effect of Prolonged Heat on the Electrical Properties of Aroclors, Summary: Aroclors 1232, 1242, 1248 and 1254 were held at 130*C. The power factor was periodically measured. 5. St. Louis Report No. 2234, Job No. 171-451, June 14, 1956. Title: Evaporation Loss of Aroclors. Summary: The evaporation loss of Aroclors was determined at 100*C. under static conditions. COMPANY CONFIDENTIAL TRAN 009319 HARTOLDMONOQ26714 Dept. 246 - Process Descrlption AROCLOR APPENDIX N MISCELLANEOUS REFERENCES 6. St. Louis Report No. 2790, Job No. 171-1028, July 3, 1952. Title: Increased Production of Aroclora by More Rapid Rate of Chlorination. Summary: Chlorination rate was increased from 400 pounds per hour to 770 pounds per hour. Aroclors produced at increased rate was within specifications. 7. St. Louis Report No. 1842, Job No. 2-02-750. 01-3368 July 12, 1957. Title: Use of Ferric Chloride as Catalyst for Production of Aroclor 1242. - Summary: The Comparison of stability chloride values revealed no difference between the product made with iron turnings as catalyst and ferric chloride as catalyst. ` 8. St. Louis Report No. 2096, Job No. 2-02-750. 01-3202, June 6, 1958. Title: Resistivity Improvement of Aroclor 1242. Summary: Numerous absorbents were screened at various contact temperatures for their effect on resistivity of plant untreated Aroclor 1242. Heat activation of Attapulgus Earth was also studied. 9. E. E. Martin, OPERATING INSTRUCTIONS FOR DEPT. 246, W. G. Krummrich Plant, 1961. " - 10. E. E.'Martin, PROCESS DESCRIPTION FOR MANUFACTURE OF AROCLORSTTfST; 1" 11. E. Mather, PROCESS DESCRIPTION FOR MANUFACTURE OF AROCLORS, 1955^ ' ' COMPANY CONFIDENTIAL TRAN 009320 HARTOLDMON0026715 Dept. 2*46 - Process Description AROCLOR APPENDIX N MISCELLANEOUS 62. The following table shows the results of tests which measured the evaporation losses of the various Aroclors. Aroclor Evaporation Rate gins ./cmf/hr ./100C. Aroclor 1221 .0017*4 - Aroclor 1222 .00087*4 Aroclor 12*42 .000228 Aroclor 12*48 .000152 Aroclor 125*4 .000052 Aroclor 1260 .0000088 Aroclor 1262 .0000122 From the above results, the evaporation rate for Aroclor 1262 Is greater than that of Aroclor 1260. This unexpected result may be explained by some difference In the conditions of which the two lots were prepared. The reaction products in Biphenyl Chlorination differ with the type of catalyst used. Results of research Investigations are listed below: Catalyst Fe Cl 9 Sb Cl Ti Cl4 Sn CI4 Isomer Distribution of Aroclor 1232 iEZ" 2751 ~tttt- 15* 11 11 2*4 7* 15* 0.7 20 0 20 1 16 6* 3* 3.6 38 2.2 46 2.3 38 *4,*4 11* 18 14 18 tri 9* 9 7 1.3 COMPANY ' CONFIDENTIAL TRAN 009321 HARTOLDMON0026716 Dept 246 - Process Description AHOCLOR APPENDIX N MISCELLANEOUS (Cont'd.) 63. Some of the typical operating dlff cultles In department 246 and possible remedies art given below: CHLORINATORS Trouble Chlorlnatora operating against too much back pressure. Cause Plugged off-gas lines Remedy Open lines and steam them out, Dry out lines with air before resuming operation. Chlorlnator slow In picking up gravity 1. Low Chlorine pres 1. Call Chlorine Dept. sure or low chlorine for more gas gas concentration 2. Check Biphenyl 2. Wet Biphenyl storage tanks for moisture. Blow tanks stacking off BLOW TANKS Operating chlorinators with vent open. Close chlorlnator vent; possibly reduce air to blow tanks STILLS Not enough vacuum 1. Ejectors not pull ing properly 2. Coke scrubber Contains water 1. Check Ejectors 2. Drain Coke scrubber Foreign material . In filtrate samples ' 36" SPARKLER FILTER Dirty filter or broken paper Clean it re-paper press COMPANY CONFIDENTIAL TRAN 009322 HARTOLDMON0026717 ' V wwoucnoM cost stakes JNW " TNW m pnoeucTiOM>ou*Mtity |lIHM>IOUHT MATBAiAL COtT tcaw BLBCVNICIYt ewiiwiB tin *1lll>fUeNUIB MI \ #B \ |OT3rWS7 Tb*r* **/\.At> TfePy/S|^ Cm* UnH liw. UnM Cod iNm4C-gKgCTfpf -. IMVSNTONV lAMIf (l HMiir fHIK ClIUTINt * NBC BIT NOMB AMAMNT MMIT COSTp_JABMOPU*NT . UM\It^! cC>tl coo>WNT umit|co'i| aiawv** avu_ _ <L*A_ _% 3A \*A 2vw*i t A ___ aa* sax. . % KS? -LIAW 6\A aeA mmMl Z^3 evet.`t &s 4K H) 35E BSBSf SBBTfgfl. i2- mn.n>nutTyiin ltul FACTPAY IWUH ciotmihb lbuxpwt BKOS. (PT. (MT. BBf>, tschnicbl svies MICH. e*i>. Vkiw aa \ oo 1/4 \Wu M? ivH i>A 4e.& (A? V ^tc ?e MHZS Avslw Mi jLloA, m& \Uk. a/Ro THrfrA ___ WMi. MM MaM. COMPANY CONFIDENTS Tmml DM Cenrarotem PSNSSCIBTIttN fit -AlAil \ \\0AA^ _A-S10I-rAV . AM \Sp* 33S55L aSm felaf IMisvet Gnvmlm> MLw^r riw fwtei c>f .. N SSZZjEiSI __k. MvJ________ WNIT UNIT BN MAMTITY OUAMTfTY ubmtitt t A*OA Mount UABQA A ATI J LA PA aaa MEM SEE S.ls A. ^ \x* A. Ai XJl TEAM LtcTAieirv CWBIHI& Am WATB AUfcCM ABBO M lA C AIM iSs ttlAU ,MA ***% ^2 \AA 3AO\AA.U . ASAX WAT BA* At AWT Al IS @&u W BA JOS V*a .......ivk _ FWIkOIL At* RKFRIMRATIM ?$! ' ICC t Aft* t A B7ANMT I SSB aaaa ouamt.ty 8anaj &il>-- - -- HUWM OD UNIT* BOWINMSMT USSDl DINT.MO DIPT. NO. % VO S S .. \frCt_L. S Asjl *T IHIItl H3* 8 NSV. / llOOf aaa aaa TRAN 009323 l ____ ,, . 3 HARTOLDMON0026718 S* ' . PRODUCTION COST STANDARD Tt I MT, MO. Aj-^ 1 c_A^*etTr\^ag_fcaa. ** \ mr V ^00. c ?v\\ rs>Y iWa \ \*>A COM MAMC rwant it T PIR WMIT TMIORT Vvnkft-- {l * tfbLoO ^C&U._CViA.v^ 03. _______ lbftjuA. 5hjJti*AjKv ^v4A <A U\AIa <<0A _______ frQ.Aao - ^l*,v A 0*4-^ ^Uv \*> K\. . ___ _l3Li-L M.o >s* i<k __JhSe ft V cA 2a*_j .foil <i&Uo\ v*'trlLM'V k^ Cov \ wsA \v U \H> ft _e>v \>Wi., .^J.\S eC As 3ft__ _______ *kS W4* \*T \W 01 * juft- SXSaX__ <k\\03_____ 1 ftV ____________ IK ->St v*lN| *T>* ^\OCV LWa%vR* Vfjst' .t>n YV*1 <lUn\ <v(A 4\\ \< a . la^ AN V*A tin 33 'V*o to* .0 - MttN A WiA Nv*N VS*-A Vv W %W*> feAet-WL Svfr^ VM**< Ao U Q s > Ac Ao Vv> 0 | ooiei H kl. E3TC Os^ \*Uo MAfU P^cfV ' OVAlo ' \SV aiAiii OV#A% 'A^V iA\^V % WMIT CO*T ^ OdC boT" OOvX A 3? V \ `h ^ a a . AA N 3 *vn< *X * ' -3 a 'A'fA a AlV A> 1 3*\ \ V* | COMPANY CONFIDENTIAL RAW MATERIAL ARIMOUSIN0 1 HANOLINO OROM TOTAL MATERIAL* T-PRODUCTf ^.it.SA \Xt.S_ L.VV 8, dM_ & jQirto SAO.V VowO*X * JtAv iNAAH '.AJ- >-v ^VaC cPi* /t VO V.,* ****.+ * vv-u^uivc /jl Y! <V jk& CVa. X<4i. A \.Q%^ y i i MIT TOTAL MATERIAL* i.... CLAIMPICATtON orcut *mut-con AMOUNT COOT OF OTANO-OT l*t op *tartwp ' COtT TO MOVE A MAN ~eeiT OP CMAMOIOVIR ___ * amount *v f ....... OOoCUCTION COOC CARACITT ' ^\\.v ' ,n^A\ oACls *.- PTV* L " "X ^ \\ %% < < ..... OVcsVA ^W.tA On\T. .0<u%i Vo^ \ ^<\s . onsets <U>\ . Iota ________ _d * { Xtvo%/A < *MLj 4 A V" K ty X ^'V 'V g jft-3 ^ JT A14A > 0*V4ii. ^ ~W~I'--_____ Cnf > Vlb------------------- ------------------ ---------------------------------------------- r-- '* * ^,. HARTOLDMON0026719