Document 6Ranx58Q74LEE0OZQBxbR9DVR

-...... ATTENTION To be retained for purposes of litigation. DO NOT DESTROY, DISCARD OR REMOVE. For additional information, contact Corporate Law Department Litigation Group. Telephone: (314) 694-2934 N? 13839 PCB-ARCH-EXT0374604 Cj DISTRIBUTION SHEET 1. Technical Information Center 2. Technical Information Center 3* Record Center ' 4. Manufacturing Manager 5 Manufacturing Superintendent 6. W.G.K. Department Supervisor 7. W.G.K. Technical Service Department 8. W.G.K. Process Research 9. W.G.K. Library 10. D. Danna - G.O. 11. D. Danna - G.O. 12. D. Danna - G.O. 13. Extra 14. Extra 15. Extra PCB-ARCH-EXT0374605 TABLE OF CONTENTS Section I Section II Section III Section IV ' Appendix A Appendix B Appendix C Appendix D Appendix E Appendix F Appendix G Appendix H Appendix I Appendix J Appendix K Appendix L Appendix M Appendix N SYNOPSIS OF PROCESS PROCESS FLOW SHEETS PROCESS IN DETAIL COMMENTS ON PROCESS EQUIPMENT LIST SPECIFICATION PHYSICAL AND CHEMICAL DATA UTILITIES PERSONNEL PACKAGING AND SHIPPING MATERIAL BALANCE ' PRODUCT LOSSES PROCESS CONTROL VARIABLES SAFETY AND TOXICITY DATA BACKGROUND INFORMATION TIME CYCLE AND CAPACITY QUALITY CONSIDERATIONS MISCELLANEOUS Page 1 2 3 8 14 18 19 20 22 23 24 29 30 40 46 47 48 49 PCB-ARCH-EXT0374606 AMENDING RECORD SHEET PCB-ARCH-EXT0374607 Department 246 - Standard Manufacturing Process Description Page 1 MCS-1109 . SECTION I - SYNOPSIS OF PROCESS This Standard Manufacturing Process describes the production of crude Aroclor 1105 which in turn is fractionated to produce MCS-1109 finished goods. MCS-1109 is a mixture of the three isomers of monochlorobiphenyl, biphenyl and a minimal amount of dichlorobiphenyl. Biphenyl is chlorinated in the presence of ferric chloride.catalyst in a series of three continuous cascade chlorinators. Biphenyl, and ferric chloride slurried in biphenyl, are added to the first chlorinator. Chlorine is sparged into the bottom of each chlorinator. The overflow from each chlorinator is fed by gravity to the next chlorinator. The degree of chlorination in the first two chlorinators as measured by specific gravity, is maintained at specified levels by manual control. The chlorine flow to the last (third) chlorinator is controlled automatically by a densitrol unit. The chemical reaction is: ^ -f- cia --gecia------ jv, HOI biphenyl MW = 154.2 chlorine 70.9 . Cl monochlorobiphenyl hydrogen chloride 188.65 36.45 Crude Aroclor 1105 is sparged with nitrogen to remove most of the dissolved HC1. The crude is then treated with lime to convert the remainder of the HC1 to non-volatile chlorides. The crude is then distilled in a 30 sieve-tray column to give a large biphenyl forefraction, a main MCS-1109 fraction, and a residue. The forefraction is recycled to the chlorination process, the MCS-1109 Nis adjusted to specification with biphenyl, and the residue is distilled in a straight take-over still. The distilled residue is used as a raw material for higher chlorinated Aroclors. The chlorination and off-gas equipment is the same as that used for production of Aroclor 1142(crude). The distillation equipment is the same as used for Aroclor 10l6. PCB-ARCH-EXT0374608 Department 246 - Standard Manufacturing Process Description Page 2 MCS-1109 SECTION II - PROCESS FLOW SHEETS . TS-D-9^72 represents most of the equipment installed on CEA 1800 in 1968. The only portion of this equipment used in MCS-1109 production is the biphenyl, chlorination, and HC1 off-gas sections. All of the equipment on the D-2 drawing of the CEA 2417 project is required. PCB-ARCH-EXT0374609 PCB-ARCH-EXT0374610 NAT, 6A S > ct RX ?00*^ T^Lf----------- 1------------------------------------------ =i sre?M i . f*3 STtU. p V09J L ---- r\ ro lfE REFERENCE DRAWINGS MOIlCI This DtAWiMO ts in* rtOPTTir Of mowanio company AMD MUST U HTUmU. WITHOUT (('OOUCTIOW O* DUPLICATION. AT ANT TIMS UPON UOUtSl. SUT IN (VINT AT COMKJTIOM Of TKt won o# to*. WMI ik rosyiuoh or mi ttcintNi. n must u nohut SAFIOUAROCQ AOAINSI ITVCtAtiOM Ot MKLOSUai TO ant omi uccrr moss unorn who nowm it to* TH| wot* Ot TO*. TMI HCIPXNI MUST SIT* CONT'DCN. TIAl AMO MOU1H KIS IIIU UTIOIU TO Ml* COHTIMNTIAS ITU IHTOtMAIION CONTAINED HltSON. W. G. KRUMMRICH PLANT SAUGET. ILL FL OW DIAGRAM DEPT 24$ ORAWN CHECKED PROJ. ENCR. OWN. APPD. APPO. OEPT. 246 WORK NO. IDENTIIT / 20 " TS- D-??7iK Department 246 - Standard Manufacturing Process Description . Page 3 MCS-1109 . ' SECTION III - PROCESS IN DETAIL A. General 1. Nomenclature / The naming of the crude Aroclor 1105 followed a long-established Aroclor naming practice. The "11" signifies a crude Aroclor, and the "05" indicates that there is about 5$(wt.) chlorine in the crude product. The' naming of MCS-1109 appears to be random. The finished product is distilled and contains about 15$(wt.) chlorine. 2. Relation to Other Aroclor Processes The continuous chlorination and off-gas facilities for producing Aroclor 1105 are the same as for producing Aroclor 1142. For more detail of this equipment and for the receiving of raw materials, refer to the Aroclor Standard Manufacturing Process. The Aroclor 1105 process is different in that the degree of chlorination is very low, lower chlorination temperatures are , used to minimize biphenyl losses, the catalyst concentration is less critical, and the off-gas condenser is run at a higher temperature to prevent biphenyl from freezing out. B. Continuous Chlorination 1. General Continous chlorination of 1105 is carried out in three chlorinators. Each is four feet in diameter by twenty feet high, and constructed of steel. Biphenyl and catalyst (FeCl^) are fed to the first chlorinator (#6) and partially chlorinated. With chlorination the volume of the mass increases and overflows successively into the other two chlorinators (#7 and #8). The fully chlorinated Aroclor 1105 flows from #8 chlorinator to what is normally called #9 chlorinator where it undergoes the next process step. . This mode of operation is called a "cascade" continuous chlorination. To start up this operation, the crude in each chlorinator must be chlorinated individually until the approximate degree of chlorination is reached. Then the cascade system can be put into operation. 2. Temperature Control. . The chlorination reaction is exothermic and essentially instantaneous. The temperature in the individual chlorinators is controlled by circulating the batch continuously through an air-cooled heat exchanger equipped with a two-speed fan and . louvres which control the air flow. The normal temperatures are: Chlorinator #6 120C #7 120C #8 150C - PCB-ARCH-EXT0374611 Department 246 - Standard Manufacturing Process Description Page 4 MCS-1109 . ' SECTION III - PROCESS IN DETAIL B. Continuous Chlorination(Cont'd.) 2. Temperature Control , These temperatures are normally maintained + 5C. Higher temperatures do not affect quality> but do increase organic losses in the HC1 off-gas. 3. Catalyst Control The necessary catalyst concentration is 0.03$ based on biphenyl. The actual practice keeps the concentration nearer 0.05$. The higher level is critical in Aroclor 1142 production, and so to avoid possible confusion when switching the chlorinators from one product to the other, the catalyst concentration is kept the same. FeClg is slurried with Bi0 in the catalyst mix tank and is added in. brief pulse charges to #6 chlorinator. Bi0 from the Bi0 storage tank is added continuously to #6 chlorinator. Samples of the crude Aroclor in #6 and #8 chlorinators are analyzed for FeCl3 content. Frequency of sampling and normal analyses(based on Bi0) are: Chlorinator #6 Chlorinator #8 $ FeCl 0.06-0.20 0.03-0.06 Frequency Twice per week Three times per week The level of slurry in the catalyst mix tank is recorded on the control panel. Malfunctions in the catalyst charging system are thus quickly noticed and corrected. The key variable is the FeCl3 concentration in #8 chlorinator. The target is 0.04-0.05$ and the absolute minimum is 0.03$. For quick increases in FeCl concentration the catalyst may be added directly to any chlorinator. , 4. Gravity Control The specific gravity of the crude Aroclor in each chlorinator is controlled by the Bi0 feed rate to #6 chlorinator and the chlorine feed rates to each chlorinator. When operating at capacity or near capacity rates, typical gravities, and analysis frequency and methods are: Chlorinator ------5-------------- Frequency of Method of $ Cl2 X-pt.of S.G.@100C Measurement Measurement in Mass Mass,C 0.982 .004 Every 4 hrs. Hydrometer 1.6-2.0 62-65 0.992 + .004 Every 4 hrs. Hydrometer 3.2-3-6 57-59 1.000 + .004 Every 2 hrs. Hydromenter 4.8-5.2 54-56 and continu- Densitrol . ously The chlorine flow rates are set manually on the first two chlorinators and controlled automatically on #8 chlorinator by the signal from the densitrol unit. PCB-ARCH-EXT0374612 Department 246 - Standard Manufacturing Process Description Page 5 MCS-1109 SECTION III - PROCESS IN DETAIL B. Continuous Chlorination(Cont'd.) 5. Rate Rate isrcontrolled by the Bi0 flow rate to #6 chlorinator. The normal chlorination rate is about 28 gallons/minute of biphenyl. This is also about 28 gpm of crude Aroclor 1105- Feed settings are: ' Biphenyl: 8o#(equal to 28 gpm) Chlorine to #6: #7: #8: 30# 500 lbs. snift gas/hr. 30# 500 lbs. snift gas/hr. 35-55# 700 lbs. snift gas/hr. The 80# biphenyl feed setting is "normal" because that rate is the crude usage rate of the fractionating column. A 100# setting could be used if desired(35 gpm). C. HC1 Off-Gas System A Brink's mist eliminator is mounted on top of each of the chlorinators. Entrained Aroclor is removed from the HC1 off-gas and immediately returned to the reaction mass via a dip pipe. All the HC1 alters a common header and goes through the shell side of a tempered-water cooled condenser. The water is maintained at 8oC f 5. The cooled HC1(75-90C') passes through a final mist eliminator(actually three parallel elements mounted in one vessel). The off-gas is then sewered because there is enough biphenyl in it to probably plug the HC1 transfer line.If MCS-1109 or a similar product is to continue to be sold, an in-department HC1 scrubbing system should be installed. The HG1 could then be used instead of sewered. ( D. Aroclor 1105 Treatment and Storage in the blowtank(#9 chlorinator) the 1105 is sparged continuously with nitrogen at approximately 150C to remove dissolved HC1 gas. Nitrogen is used instead of air because at this temperature biphenyl is well above its flash point. When biphenyl is being charged at an 8o# rate(28 gpm) to #6 chlorinator, nitrogen is sparged at a rate of approximately 20 SCFM. Average residence time in the blow tank is 30 minutes. The blown crude is pumped to the #2 Intermediate Tank, maintaining a constant level in the blow tank. The Aroclor 1105 is treated with lime by slurrying lime in Aroclor 1142 and charging this pulse-wise into the 1105 transfer line between the blow tank(#9 chlorinator) and the #2 Intermediate Tank. The important variable is that the lime concentration in #2 Intermediate Tank should be a minimum of 0.1#. Present operation is to make the 1142 slurry about 10#(wt) lime and to charge this through a timer set for 30 seconds closed and 6 seconds open. This gives a lime concentration of about 0.2# when the chlorinators are being charged at an 80# rate(28 gpm). PCB-ARCH-EXT0374613 Department 246 - Standard Manufacturing Process Description Page 6 MCS-1109 ' SECTION III - PROCESS IN DETAIL E. Distillation 1. General Good control of the specific gravity of the crude Aroclor 1105 is extremely important because the distillation cycle is controlled primarily by material balance(rather than temperature, P, etc .) . Distillation is accomplished in a 30-sieve tray column. The head pressure is maintained at 360 mm Hg. Still pot pressure will increase as the distillation proceeds, but will be approximately 460 mm during the MCS-1109 product fraction take-over. The research process calls for distillation at reflux ratios of 4:1, and later 8:1. These ratios are flow ratios inside the column. Actual operations control reflux ratio only Indirectly. The two variables that are controlled are fuel flow to the furnace which supplies heat to the column, and the forward flow 'rate(take-off rate). . Estimated Internal *-- -Reflux Ratio________ Fuel Gas Setting Forward Flow Rate 4:1 17,500 SCFH* 28 gpm - 6:1 - - 17,500 SCFH 21 gpm 8:1 17,500 SCFH 14 gpm *(2 gpm of No.2 Fuel Oil can be used instead, but this has not . been demonstrated). 2.Distillation Procedure Process Step Charge still pot Gallons of Crude Fed 18,500 Gallons of Forward Flow and Disposition b. r Inventory column and line out temperatures on t otal re flux; main - -" tain level control on pot. 1,000 -- c. Strip biphenyl at a 4:1 reflux ratio - until forward flow counter reaches - - . 10,000 counts. 30,000 30,000 - - d. Strip biphenyl at 6:T reflux ratio until forward flow counter reaches 12,000 counts. 6,000 . 6,000 gals, to biphenyl tank PCB-ARCH-EXT0374614 Department 246 - Standard Manufacturing Process Description . Page 8 MCS-I109 . ' SECTION IV - COMMENTS ON PROCESS A. Chlorination 1. Temperature Control An 80* biphenyl feed, rate(28 gpm) is the minimum rate that can be run in the continuous chlorinators when making 1105 and maintain temperature control. Even at this rate the crude is bypassed around the heat exchanger on #6 chlorinator in order to keep the temperature up to 120-125C. The heat exchangers are used on #7 and #8 chlorinators. 2. Crude Composition Typical crude 1105 analysis prior to adding the 1142 lime slurry is as follows: Biphenyl ortho meta para dichlors and higher 73.5 -75.0* 14.0 - 15-0 1.5 - 1.7 8.0 - 8.4 1.2 - 1.6 For other chlorination data refer to Research Report No. P-1620 by Q. E. Thompson dated 6/18/71. B. HC1 System The tempered water on the HC1 condenser was controlled so that the gas leaving the condenser was.8oC. At lower temperatures the condenser would freeze out biphenyl. At 8oC however, considerable biphenyl and some monochlorobiphenyl remained in the vapor. Therefore at that time(Sept.1971-Feb.1972) all HC1 off-gas from 1105 production was sewered for fear of plugging up the HC1 transfer line. Since that time there has been an edict that no more HC1 containing chlorinated biphenyls will be sewered. This means that at this writing(May 1972) MCS-1109 cannot be produced at the Krummrich Plant. The WGK PR&D group is working on an HC1 scrubbing system which may allow HC1 to be sewered in the future. C. Treatment of Crude Seven pairs of data points from the last continuous chlorinator and from the blow tank indicate the following average acidity: Crude 1105 unblown 1105 blown with N2 0.24 mg KOH/g. 0.05 mg KOH/g. As stated in the "process in detail" section, the lime concentration is normally kept about 0.2$; This lime concentration probably makes it unnecessary to blow the crude 1105 with nitrogen. A similar situation is present in the Aroclor 1016 process, except that air is used instead of nitrogen. A process amendment is being circulated for approval to discontinue the blowing step. This would be done to reduce PCB losses to the environment. PCB-ARCH-EXT0374616 Department 246 - Standard Manufacturing Process Description Page 9 MCS-1109 ' SECTION IV - COMMENTS ON PROCESS C. Treatment of Crude(Cont*d.) A question can be raised as to why crude 1142'is used for slurrying lime into 1105. The reasons are several. The slurry tank is an unheated tank that is opened on occasion to manually add bags of lime. At temperatures below about 54C 1105 freezes. At temperatures above about 113C 1105 is in the flash point range. Crude 1142 has neither of these drawbacks. A last reason for using 1142 is that it improves the recovery of monochlorobiphenyl in the distillation batch. A certain minimum level is necessary in the still pot to maintain good circulation through the furnace. As the end of a distillation approaches, the 1142 from the lime slurry supplies part of the bulk. Because of the minimum level requirement, recovery of the para-isomer of monochlorobiphenyl is poor. Without the 1142 present, recovery would be even worse. D. Distillation 1. Column CyclefRefer to Research Report P-1621 by D. R. Cova dated 6/15/71). a. Biphenyl Stripping(forecut) Biphenyl vs. ortho - content of the forward flow during the earlier part of the biphenyl stripping was observed only on the initial run of MCS-1109. It was as expected and therefore .ted. (One J,count" is about 3 gallons of forward flow) Date Time Counter Bi0 0 9/9/71 9:30 a.m. 0 9/9/71 2:45 p.m. 2256 9/9/71 6:30 p.m. 3700 9/9/71 10:30 p.m. 5400 9/10/71 2:30 a.m. 7100 9/10/71 6:30 a.m. 8800 9/10/71 10:30 a.m. 10725 9/10/71 12:30 p.m. 11640 99-91# 0.09# 99.86# 0.10# 99.85#'0.08# 99-68# 0.32# 99.58# 0.4o# 92.1 % 7-9 # 88.6 # 11.4# The above data was taken under conditions somewhat different than later adopted. The column head pressure was 280mm instead of 360 mm and the forward flow rate was 20 gpm instead of 28 gpm. b. Forward Flow Rate While Stripping Biphenyl When biphenyl is taken off at a 28 gpm rate, orthobegins to come over with the biphenyl in significant amounts after about 10,500-11,000 counts(31,500-33^000 gallons). If the crude were stopped at this point and a product cut begun, the batch would be smaller than desired. Therefore at 10,000 counts the forward flow is reduced to 21 gpm(about 6:1 reflux ratio). At 12,000 counts the crude feed is stopped and the forward flow changed to 14 gpm. Biphenyl stripping continues because if the product cut were begun at 12,000 counts the finished goods would contain too much biphenyl. PCB-ARCH-EXT0374617 Department 246 - Standard Manufacturing Process Description Page 10 MCS-1109 ' .SECTION IV - COMMENTS ON PROCESS ' D. Distillation(Cont'd.) c. Product Fraction . - : The cut point between biphenyl stripping and the product ' \ fraction can be determined by any one of three variables: (1) X-Pt. of the forward flow (2) Specific gravity of the forward flow (3) Head temperature in the column For details, see logged data on Batch #2 at the back of this "comments on process" section. In summary, it is evident that crystallizing point or specific gravity of the forward flow would be most accurate in making the product cut at a certain biphenyl/ortho- concentration. However in MCS-1109 this : -- provision is not necessary. As the ortho- content increases the column head temperature will increase by ten degrees in a one hour time period. The product cut is normally begun ... when this temperature break has become obvious(2-30C increase). ...... In practice the end of the product fraction has been determined by volume of residue(10$ level in still pot). As long as the - other variables are in control, primarily crude composition, this is adequate. If a more positive control method were needed, crystallizing point would probably be a good choice. Specific gravity or head temperature are changing only slowly and therefore are of little value in determining the end of 'the distillation. For the first five batches produced, the last 6-9$(600-900 gallons) of the product cut was held in a receiver before adding it to the product storage tank. After the receiver ; was analyzed, it was in each case made a part of the product. The ranges for the various components on the last 6-9$ of product distillate was: Biphenyl prtho meta para dlchlors and higher 0.0 - 5.5$ 3.5 - 8.0$ 15.6 -17.9$ 69.2 -75.8$ 2.5 - 4.6$ 2. Reflux Measurement The_..Aroclor column project(CEA 2417) called for a rotameter to be installed in the reflux line. This was done but it did not work properly. It would cycle widely, perhaps from 20$ to 80$ of scale every 15 seconds. A second "low-head" rotameter was installed, but it too exhibited the same characteristic. A sight glass was installed in place of a rotameter and no visible fluctuation can be observed. No further work was done. This leaves the process without reflux measurement. The process is controlled by fuel input and forward flow rate. No problems have been encountered, but this arrangement assumes a constant fuel efficiency which over the long run is a poor assumption. PCB-ARCH-EXT0374618 Department 246 - Standard Manufacturing Process Description Page 11 MCS-1109 SECTION IV - COMMENTS ON PROCESS D. Distillation(Cont'd.) ' 3. Corrosion ' \Most of the column is constructed of 316 s.s.,originally built for the phthalic anhydride unit in Chocolate Bayou. This material .of construction makes it extremely important that a minimum of moisture enter the column. Vacuum is always broken with nitrogen instead of air. 4. Freeze-Ups The process equipment installation was designed for Aroclor 1016. Comparatively, MCS-1109,especially the biphenyl fraction, is very prone to process freeze-ups. Biphenyl freezes at 70C. Numerous process upsets have occurred because of inadequate tracing and insulation on the process lines. 5. Column Change-Over Between MCS-1109 and Aroclor 1016 Switching column production from Aroclor 10l6 to MCS-1109 is no problem as far as cross-contamination in the column is concerned. During the column heat up and total reflux, the 1016 hold-up in the column is displaced by the lighter biphenyl. The Aroclor 1016 ends up as part of the 1109 residue. Contamination is a problem, however, when switching from MCS-1109 to Aroclor 10l6. The first 1000 gallons of forward flow is directed to the residue tank because it is really just purging the column para-rich monochlorobiphenyl from the just completed MCS-1109 production run. Normal Aroclor 1016 Run: Forward flow after - Biphenyl ortho meta para dichlors & above 50 counts 0.54# 20.22 0.76 3.85 74.60 200 counts .- 99.72# 400 counts 98.60# First Aroclor 1016 Run After Making MCS-1109: Forward flow after 400 counts(about 1000 gallons) Biphenyl ortho meta para dichlors & above 1.0#2.8 1.4 15.4 79.4 i .1 PCB-ARCH-EXT0374619 Department 246 - Standard Manufacturing Process Description Page 12 MCS-1109 ' SECTION IV - COMMENTS ON PROCESS D. Distillation(Cont'd.) 6. MCS-1109 with Low Biphenyl Content . , \0n two occasions the .process was altered slightly in an attempt to demonstrate how low the biphenyl content could be made. As the point approached where monochlorobiphenyl distills over at a forward flow rate of 14 gpm, the rate was reduced to 7 gpm. Biphenyl continued to be stripped a little longer. The flow was sent to the biphenyl tank until the "temperature break" on the top tray was complete. Only then was the flow diverted to the product tank and the rate increased back to 14 gpm. On each of the two batches the biphenyl content was reduced to 2.5-3-0%. \ ' I PCB-ARCH-EXT0374620 Department 246 - Standard Manufacturing Process Description Page 1^ MCS-1109 . ' SECTION IV - COMMENTS ON PROCESS Appendix A Equipment List t v EQUIPMENT INSTALLED BY CEA 2417 - AROCLOR COLUMN Item Equipment No. Name_______ Equipment No. ~ Description 301 Fractionating 30-0478 Total length is 69'. The top 36'9" and the bottom 6'9" of column is 316 SS. The intermediate 7'6" and an 18' skirt are carbon steel. There are 30 sieve trays. The upper 22\and No.3 are 318 S-S. Trays 1,2, and 4 thru 8 (numbered from bottom) are carbon steel Blanking strips are on trays no. 1-25. . Design pressure is 30 PSIG max. to full vacuum. See drawings SK-2417-1- 301-1, Rev. 2, and SK-2417-1-301-2, Rev.l. 302 .... . . Column Condenser ___ _ ....................~ . 38-6026 . . . Length 17',diameter 37". Heat transfe area i 2400 square feet. The shell is steel, the tubes and vapor side bonnet are 316 SS, the condensate bonnet is aluminum. The 1220 tubes are 10' long, 3/4" dia.,14 gauge. Tempered water on the shell side, product through tubes. Design pressure is 75 PSIG max. to full vacuum. 305 Still Pot 21-5325 Length 28'0", diameter 12'6",volume 26,000 gallons, steel construction. " . ....... . ...........\...... ........Sump is 36" dia. and approx. 30" ' ' - - deep. The distributor pipe is 8"sch. 80 pipe, about 8' in length. 306 Still Pot ~ Pump ~ 63-68947 . Dean Bros., 8 x 6 x 15* model SXR-30, 15" impeller, 750 gpm. Mechanical sea. is flushed with side stream from pump discharge. Flush goes through a cyclone separator and seal guard unit (cooler). 306. Still Pot 001 Pump Motor 52-57059 Lincoln, 40 HP, 1150 rpm. 307 Furnace 43-0026 Relocated from WGK Dept. B-257. Rated at 10M BTU/hr. 3 burners, uses gas or No.2 fuel oil and steam. Pilot burners use gas. Coil is steel, 6" diameter. PCB-ARCH-EXT0374621 Department 246 - Standard Manufacturing Process Description Page 15 MCS-1109 ' SECTION IV - COMMENTS ON PROCESS . . Appendix A v Equipment List ' . EQUIPMENT INSTALLED BY CEA 2417 - AROCLOR COLUMN Item Equipment No. Name . Equipment No. Description 308 Column Vaccum 35-5372 Worthington, 2-stage, non-condensing. Jet Model N10-12. Cast steel head,monel nozzle,cast iron body, monel bushing. 312 Residue Tank 21-5337 Carbon steel horizontal tank, l6'0" length, 11'0" diameter. Volume is 12,000 gallons. Distributor pipe is 141 long, 4" Sch. 80. One inch hair pin steam heating coil. 313 Residue Tank Pump 313. -...Residue,, Tank 001 Pump Motor 314 #17 Storage Tank 315 \ 315. 001 #17 Storage Tank Pump #1 Storage Tank Pump Motor 316 Fuel Oil Tank 317 Fuel Oil Tank Pump 317. 001 Fuel Oil Tank Pump Motor 320 Lime Slurry Tank 320. Agitator _ 001 ((Speed Reducer) 52-70325 52-56859 Durco AVS, 3 x 2 x 13, 1750 rpm. 11 5/8" impeller. 350 gpm at 98' TDH. Casing is ductile iron,impeller is 316 SS. Allis-Chalmers, 25 HP, 1800 rpm. 21-5338 52-70355 52-56859 Aluminum, 12* 6" dia., 24' 0" high; equipped with plate coils and eductor Durco AVS, 3 x 2 x 13, 1750 rpm. 12 7/8" impeller. 150 gpm at 172' TDA. Casing and impeller is 316 SS. Allis-Chalmers, 25 HP, 1800 rpm. 21-3373 52-77521 52-55510 Carbon steel, 13'0" diameter, 20'0" high. Volume is 20,000 gallons. Worthington rotary gear pump, model IGA,iron contamination. Allis-Chalmers, 3/4 HP, 1150 rpm. 21-5339 52-86887 Carbon steel, 48" O.D., 63" straight side, 500 gallon volume. Carbon steel, 2-4 bladed impellers,6" diameter. 320. 002 Agitator Motor 52-55980 General Electric, 3 HP, 1150 rpm. PCB-ARCH-EXT0374622 Department 246 - Standard Manufacturing Process Description Page 16 MCS-1I09 . SECTION IV - COMMENTS ON PROCESS Appendix A Equipment List EQUIPMENT INSTALLED BY CEA 2417 - AROCLOR COLUMN Item Equipment No. Name Equipment No. Description 320. 003 Lime SlurryTank Scrubber Schutte & Koerting type 7009 Vent Scrubber. Described as special fitting X-14 in project. 322 #17 Storage Tank Product Filter 65-0774 Alsop, filter Pak 125-4, 316 SS construction, Viton A gaskets.(2 units) 324 Vent Cooler 38-6029 Overall length 10'2"; shell is 6" Sch. 4o carbon steel pipe; single pass; 20 baffles, 26 - 3/4" monel tubes 8' long; 40 square feet surface. 325 Tempered Water 52-69243 Relocated from Phenol Dept., Durco Pump 4 x 3 x 8. 3/4, 8 1/2" impeller, capacity 650 gpm. 325. 001 327 328 Tempered Water Pump Motor 52-56560 Product Filter 65-0775 at Loading Dock #3, Track 11 Light Ends Receiver 21-5340 Allis Chalmers, 15 HP, 1750 rpm. Same as Item 322 except only one unit. Carbon steel, 102" O.D., ll'O" on straight side, volume 5000 gal.,plate coils on bottom dish. 329 #2 Intermediate 21-3556 Carbon steel, 10' 6" diameter, 31' 0" Tank on side, 20,000 gal. volume, plate coils, 2 eductors. 330 330. 001 #2 Intermediate 52-70750 Tank Pump #2 Intermediate 52-56360 Tank Pump Motor Durco, 4 x 3 x ,13, 300 gpm capacity. Allis-Chalmers, 10 HP, 1150 rpm. 331 Light Ends Receiver Pump 331. 001 Light Ends Receiver Pump 52-69835 52-56109 Durco AVS, A-50, 3x1 1/2 x 10, 75 gpm capacity, 316 SS(had been Item 544 from CEA 1800). Lincoln, 5HP, 1750 rpm. PCB-ARCH-EXT0374623 Department 246 - Standard Manufacturing Process Description Page 17 MCS-1109 . SECTION IV - COMMENTS ON PROCESS . . Appendix A Equipment List ' Item No. EQUIPMENT INSTALLED BY CEA 2417 - AROCLOR COLUMN Equipment Name Equipment No. . 340 #18 Storage Tank 21-5341 Same as Item 314. 341 #18 and #19 65-0776 Same as Item 322. Storage Tanks Product Filter 342 342. 001 343 348 349 350 N #18 and #19 Storage Tank Pump 52-70355 #18 and #19 Storage Tank Pump Motor 52-56859 #19 Storage Tank 21-5342- #5 Absorber #5 Absorber Filter 21-5343 . 65-0778 Column Receiver 52-69960 Pump(1016 Absorber pump) Same as Item 315- Same as Item 315*001. Same as Item 314. Same as Items 532, 539, 540, and 545. Same as Item 322 except only one unit Durco AVS 316 SS, 3x1 1/2 x 13, 25 gpm at 148.6 TDH; 12 3/8" impeller. 350. 001 353- 352 Column Receiver 52-56559 Pump Motor Tempered Water 21-4432 Flash Tank Lime Slurry Pump 52-69815 Allis-Chalmers, 15 HP, 1750 rpm. Carbon steel, 36" O.D., 7'0" on side, 410 gallon volume. Durco, 3x1 1/2 x 10, 9" impeller, 40 gpm capacity. 352. 001 Lime Slurry Pump 52-56109 Lincoln Motor , 5 HP, 1750 rpm. . - PCB-ARCH-EXT0374624 Department 246 - Standard Manufacturing Process Description M'CS-1109 SECTION IV - COMMENTS ON PROCESS Appendix B Specifications A. Raw Materials Material Code Raw Material 82601 81064 33500 38800 43101 Biphenyl Chlorine Ferric Chloride Lime, hydrated Nitrogen B. Finished Goods 81112 MCS-1109 Page 18 ' PCB-ARCH-EXT0374625 Monsanto ORGANIC CHEMICALS DIVISION RAW MATERIAL SPECIFICATION PRODUCTION A, E, Lelsv PROCUREMENT J. Leyerle OSNCNAL DESCRIPTION MATERIAL COOS 82601 plant WGK DATE EFFECTIVE ,10/23/70 MATERIAL DIPHENYL (BIPHENYL) USING DEPTS. 246 SUPPLIER Anniston Plant APPROVALS RESEARCH JL--EL__R1 nha rri QUALITY CONTROL (Chief Chemist) R- Blowers CHEMICAL PORMULA mol wt. 154. 20 SUPERSEDES SPEC* OP 2/6/69 CHARACTERISTIC ample por analysis 2 x 16 oz, W. M. Bottles UNRESTRICTED INFORMATION (R) Appearance and Color Light Yellow Cryst, Solid (R) Crystallizing Point (R) HzO GENERAL INFORMATION 68. 70C. , min. ppm max. Distillation Range: _ . % First Drop to 2. 5C. , max. Dry Point Must include 255G. within range ISSUED B Y ^ Shaulter/G., METHOD 10, 252 10,298 13,155 10,299 This specification is the property of Monsanto Company and is for internal use only. (R) Routine An air. le, All othere Ahelyeod by fequeei fftfy. PCB-ARCH-EXT0374626 ionsanto W. G. Krummrich Plant RAW MATERIAL SPECIFICATION PRODUCTION A , E,. Leisy PROCUREMENT j: Leyerle GENERAL DESCRIPTION MATERIAL CODS 33500 ' MATERIAL Ferric Chloride Anhydride PLANT J WGK USINO OEPT3. 233 DAT P rFFECTIVF SUPPLIER Jan. 31, 196$ McKesson k Robbins APPROVALS RESEARCH . W. R. Richard f"!*< it v control (Chlml Chemlat) R. Blowers T, Bell - CHEMICAL FORMULA mol wt, 162.21 SUPER?ED^SPEC3 OF r/m Fe Cl3 SAMPLE FOR ANALYSIS 1x8 oz. W.M. Bottle C HARACT ERISTIC UNRESTRICTED INFORMATION Appearance Assay Sulfates Ferrous Salts % Solubility: ' 10:10 of Water 10:10 of Formula 30 Alcohol Black powder or Granules 97.0%, min. 0. 05%, max. . Trace, max. Complete to slightly, turbid, max. Complete to slightly turbid, max. ISSUED BY Higgerson/Stites METHOD J.F.Q. 16-A 22-570 120-570 S-570-1 112-B (R) Routine Anmlytia, Alt otheta Analyaod by rewkt onJy. PCB-ARCH-EXT0374628 Monsanto .ORGANIC CHEMICALS DIVISION MATERIAL CODE 38800 PLANT MATERIAL Lime, Hydrated USING DEPTS. RAW MATERIAL SPECIFICATION W.G.K. DATE EFFECTIVE . 4/7/70 287, 750, 246 SUPPLIER Mississippi Lime Co. APPROVALS PRODUC TION RESEARCH A.,E. Lelsy T. W. Dalton W. R. Richard PROCUREMENT ^ QUAUIT Y CONTROL (Chlei Chemist) J. Leverle R. Blowers________________________________ GENERAL DESCRIPTION , CHEMICAL FORMULA Ca (0H)2 SUPERSEDES SPECS OF 8/1R/6Q CHARACTERISTIC Appearance Assay (Ca(0H)2) Carbonates as (CaC03) Magnesium Sulfates (as S03) . SAMPLE FOR ANALYSIS 1 X 16 oz. W.M. Rnttlp . LIMITS Fine white or slightly gray powder, free from lumps or gritty material. 92.00$, min. 3.00$, max. 0.50$, max. O.3O%> max. ISSUED B Y METHOD 10,188 10,191 10,193 10,192 10,189 Supplier's certificate of analysis to be sent on day of shipment to: . Chief Chemist, Monsanto, Sauget, Illinois s (R) " Routine Analysis, All others Analyzod'by request only. WCK-314 PCB-ARCH-EXT0374629 MATERIAL CODS MATERIAL , , _ '............. . , Ill 43099 / Nitrogen Gas ORGANIC CHEMICAL^ &tV<SION PLANT USING OBPTfe. ` . ' RAW MATERIAL WGK See Below (3) DATE EFPBCTIVE SUPPLIER. SPECIFICATION ,3-429/68 Air Reduction Sales Co. ssosucrioN J W>Mt APPROVALS T. W.D. r esq arch R> H- Mills ODeG. O.D. D. PROCUREMENT " E. D. M. H. Lanser . J.M. C. ' E. L. M. . J.A.S. QUALITY CONTROL (dftM CAoatItO W. J; Gresham ' OSNOHAt Oe&CRIPflOM ... -. > CHEMICAL FORMULA i Grade - O. P. Special Nitrogen uRERSEoac #*>eo op__________________________ 2/18/65 .. .V ` characteristic dAMPLE row ANALYSIS . m m . o \ . . ISSUED IV L. E. Hornback LIMITS 1 METHOD Assay (T) Oxygen Hydroget} Dey Point Nitrogen > * Argon Oxygen Carbon Dioxide Acetylene r i ; ! 99. 9%, min. ' 0.1%, max. ., 0% -76#F. Typical Analysis 99.78% 0.12%. 0. 1% . . . 00005% '.00005% (2) V (1) Nitrogen plus inert tare gases -- , | r (2) ... Any analyses to be obtained from supplier on request. i- ; or 213, 244, 246, 247, A-255, A-256, 259, 267, 270, B-270 & 281. ; : (tl) ftMdbo AMljmto. All AeaJrcwJ dr nu mi* i M*MH&J[UwW.>igOgBEgT|Wl.lTfHI JB333HKfi5g35BBBMPC3BWBBBBCBHB3BHBBBB^BMi i . we**ou "" . t , PCB-ARCH-EXT0374630 Department 246 - Standard Manufacturing Process Description Page 19 MCS-1109 ' SECTION IV - COMMENTS ON PROCESS Appendix C Physical and Chemical Data Physical constant data sheets which are available are listed following this page. PCB-ARCH-EXT0374631 1* PHYSICAL CONSTANTS DATA "SUBTTXSTE- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 826P1._PJUPHEN.YL_ rouPa-nrrrwrFIMe^ne'r '2/12743 HevT DATE STRUCTURAL FORMULA <0-0 NAME Formula Molecular Weight Aooearance . Boiling Point at 760 mm Boiling Point at^Q /jrm Boiling Point at mm Boiling Point at mm Crystallizing Point Melting Point Solution Point 0 Soecific Gravity 77/4 C Specific Gravity <? 20/4C Pounds per Gal. a 77 C Coefficient of Expansion Refractive Index 77.1 Cn 3 infra Red Spectrum (Referenct) Ultra Violet Spectrum (Reference) Viscosity 100QC Viscosity 70C Surface Tension 129. 2C Solubility in Water (3 80C Solubility inabs.ASc. 19. 5 C Solubility in 100% Methanol 19.5C Benzene (3 27. 9C. Heptane <3 26. 5C. CfiHpi CrH* 154.20 Monoclinic 255^C. hr SOURCE & DATE L'hem. Rubber Handbook ------- n rr i341 '92 Tnt Crit. Tables 1928 Swann file #1 37 1.9 35 69 0"C 69 ur 0. 9896 1 041 fi 28 Ihs per gal; D = 1.58822 Swann Curves 1934 Tnt Crit Tahles 1928 Int. Crit. Tables 1928 II II II It Swann File #137A 1930 Int. Crit. Tables 1928 28.8 Say. Sec 31.2 " " 29. 5 dvne/cm Insoluble 9. 98 g./100 g. solvent 6.57 g. / 100 g. solvent 137 g.y 100 g. solvent 25. 1 g. /100 g. solvent Swann File #137A 1.930 If II 11 M Tnt. Crit. Dow Seidell " " " Tables 1928 1943 1941 1941 1941 1941 Flash point F (Method) Fire Point 0 (open rnp) Heat of Combustion kg-ral(i6) Heat of Formation Thermal Stability fcal.Ag/min.) Latent Heat of Fusion Latent Heat of Vao. <3 255C Soecific Heat Critical Temperature Critical Presses Dissociation Constant Latent Heat of Fusion --235F - clb-5'ed_ciip-----------270^' ' Pcn euP ' per gm mol - 1 604 4 Ind. & Eng. Chenl. 1S40 33 883 __________________ Swann"File #137 A (1Q41L Tnt C^it, Tables '928 136. 5 RTTJ/lh. 0 48 RTTT/lh Tn 528C 41 4 Atm ahcolnte Swann File #137 A (19281 R&E CR 964 M 9561 Rev Sci, Instrument 1 663 " " " ~T 19 3 0 28 8 crm-cal ner am Lange Handbook 1937 ( 53. 1 BTU/lb m cm m g 0 g O NQTE: - Flies of W. P. Metzm ^r. St. Louts Toxicity (Give Reference) (1 V*. Dr. Me Lester, Anniston ` 3lant. Report copy in __ St__ T .oiils nhvsirianls fll 2_____________________ -_____L13JL NOTE: Thee data nhould not of Mbn PCB-ARCH-EXT0374632 ! PHYSICAL CONSTANTS DATA tUBITAWCg------- - CHLORINE ATRUCTUPAUrORUULA COUKIIUP UT W. H. Demaree NAME Formula Molecular Weight Aooearance Boiling Point at 760 mm Boiling Poirt atlOC^mn finilins Point A KLmn Boiling Point at 1 mm DAT s'" ii 11 1 ' ' -% 70.914 -34.05 -71.32 -100.06 -120.44 SOURCE ft PATE_____________________ API Ref. 1_______________________ :________________ Ref. 1 Ref. 1 Crystallizing Point Meltinf Point Solution Point Specific Gravity 0C (gas) Specific Gravity # 20C Pounds per Gal. <* C -100.98 2.49 . 1.408 Ref-_J2_____________________________ __________ Ref. 2 Lange Coefficient of Expansion Refractive Index a 0C . n5 1.47 Ref. 2 infra Red Spectrum (,Reference) Ultra Violet Spectrum /Reference) Viscosity*' . * ....... . - Viscosity 1? * ^Surface Tension . Sdlubility in Water -- --------------------------------- -- ... Solubility in ' Solubility m ~...............* Specific gravity @ 30#C . v- ' 1.377 . Lange - - . --------------------------_ ------ - - ------------------------- ------------- _ ,, ... _ ------------- ..... "Flash Point F method) " Fire Point C - - -------- Heat of Combustion . ' Hoat of Formation Thermal Stability fcaL/kg/min.) Latent Heat of Fusion Latent Heat of V. ................ . . Specific Heat Critical Temperature Critical Pressure Dissociation Constant 144C 76.1 atmos. . . Ref. 2 . Ref. 7 .......... ..... ' . Ref. 1 - Calc, from det. data Ref. 2 -.Monsanto.Chlorine me* s tv (A C ... . ` O O ------- ----------- -J - ... . ............... *> O . ~~ . . . ~..kxity (Give Reference) - . I * ( T I ' -I IIIHI hi luijtnli-hr rrl_u%rtt uufyuietif Ahtnttutitt ('.hemtenl (: tiin/umy. I `i t mliintunul \ h III . if . ' ---------- ,f.... * } '%i r*!* * ...... .. ` ' " . ,. l- -f,~ PCB-ARCH-EXT0374633 IN fit 38800 PHYSICAL CONSTANTS DATA 'SU&'STAnte--------------7--;-------------------- :-------------- STRUCTURAL FORMULA - HYDRATED LIME (Calcium Hydroxide) MinjVFFippi Lime Company cLeo J.T Hoog, M.L.C. ^ A. M. Ellenbure Revised NAME Formula Molecular Weight Aooearance Boiling Point at 760 mm Boiling Point at mm Boiling Point at mm Boiling Point at mm Crystallizing Point Melting Point Solution Point Soecific Gravity @ 20C @ Specific Gravity <> 20 Pounds per Gal. C Coefficient of Expansion s Refractive Index n g Infra Red Spectrum (Reference) Ultra Violet Spectrum (Reference) <? Viscosity & Viscosity Surface Tension Solubility in Water Solubility in Solubility in DATE 1-25-57 7-12-57 Ca(OH) 74.10 White powder SOURCE & DATE Ref. 1 Ref. 1____________________ Ref- 2____________________ Decomposes 2.2 4 wD 1. 574. Ed 1.545 Ref. 1____________________ i Ref. 1 Ref. 2_______________ ____ Ref. 1_____________________ .185% @0C. . 077% & 10 0C Ref. 1 Soluble in acids and NH4 21 Ref. 1 . Rash Point F (Method) Fire Point C Heat-of Combustion ------------ Heat of Formation Thermal Stability (cal.Aa/min.) Latent Heat of Fusion ' Latent Heat of Vao. Specific Heat---------- Critical Temperature Critical Pressure Dissociation Constant ----: - ' References: - mC M oeo I )' jewAs) o 1 , Langes Handbook, Ed. f r 1956 2. Information bv Vendor . Toxicity (Give Reference) _______________________________________ ,________________ NOTE: These data should not be released outside of Monsanto Chemical Company. Use additional sheets if necessary. PCB-ARCH-EXT0374634 Department 246 - Standard Manufacturing Process Description Page 20 MCS-1109 gECTIOITTV - COMMENTS ON PROCESS Appendix D . Utilities Utility usage is as appears on the 1972 Cost Standard for production . of 1.5M# lbs. MCS-1109/mo. Actual production was for such a short period of time that actual utility usage is meaningless and therefore not included in this report. 1. Power Consumption A. Electricity - 440V, 3 phase, 60 cycle Cost Standard usage - 1200 CKWH/month The following equipment uses electricity: Item No. Motor Iff jHP 208 402 4 03 405 407 4o8 411 412 415 4l6 419 420 428 431 434 306 313 317 320 325 330 350 352 #10 Storage Tank Pump 10.0 Biphenyl transfer pump motor 5.0 Catalyst mix tank agitator motor1 7.5 Catalyst mix tank circulating 5.0 pump #6 Chlorinator pump 15.0 #6 Chlorinator heat exchanger 2.0 fan #7 Chlorinator pump 15.0 #7 Chlorinator heat exchanger 2.0 fan #8 Chlorinator pump 15.0 #8 Chlorinator heat exchanger 2.0 fan #9 Chlorinator pump 15.0 #9 Chlorinator heat exchanger 2.0 fan Off-gas condenser water pump 5.0 Off-gas condensate tank pump 5.0 . City water pump 20.0 Column Still Pot Pump 40.0 Residue Tank Pump 25.0 Fuel Oil pump 0.75 Lime Slurry Tank Agitator Motor 3.0 Tempered Water Pump 15.0 #2 Intermediate Tank Pump 10.0 Column Receiver Pump 15.0 Lime Slurry Tank Pump 5.0 Total 239725 B. Electricity - 110V, 6o cycle Lighting, instrumentation, and miscellaneous uses. 2. Natural Gas Cost standard usage is 6000M BTU's/month, the only use being in the column furnace. The natural gas to the furnace is interruptible The furnace is equipped to use No.2 fuel oil when necessary. PCB-ARCH-EXT0374635 Department 246 - Standard Manufacturing Process Description Page 2.3 MCS-1109 SECTION IV - COMMENTS ON PROCESS . Appendix F Packaging and Shipping ' 1. Tank cars and trailers - MCS 1109 has been shipped in steel tank 'cars and trailers. The only customer has been the Anniston, Alabama plant. All bulk shipments of material are sampled from the final container. That is, all tank cars- and tank trucks are sampled and analyzed after loading. Tank cars and tank trucks are inspected by supervision to be sure they are free of dirt and water or other foreign material before loading. Heels are drained before loading when their quality is questionable or when it is incompatible with the ; material to be loaded. Car washing, when necessary, is done by the repair track. Tank cars are sealed with a numbered aluminum seal by repair track personnel. The cars and trailers should be equipped with steam coils as the . crystallizing point of MCS-1109 is in the range of 8-l6<->C. 2. Drums - Drums of MCS-1109 have not been sold, but the recommended container would probably be.a 55-gallon, unlined, double-chine, all 16-gauge steel drum. Net;weight would be 500 pounds. PCB-ARCH-EXT0374638 Department 246 - Standard Manufacturing Process Description Page 24 M'CS-1109 ' ' . SECTION IV - COMMENTS ON PROCESS Appendix G' 'Material Balance , On the following pages are the material balances for the chlorination and distillation of MCS-1109. They are from the Research Reports P-1620 and.P-l621. Limited experience in the plant would indicate no major differences. The components of crude 1105 are actually closer to the composition shown in the "comments on process" section rather than those shown in the material balance. PCB-ARCH-EXT0374639 FLow 6M-EE.T - Cf?L/DE. *Ro<i\oR llt> off Ga.S> CtfODE j\ftotlo% lloS Py-0cJjU.c4" Page PCB-ARCH-EXT0374640 f|| V- ;;vv' >.- ;a ' ^ ..- ' ;:s;' .-. -;;. .: :": .V V V W0^W^i0^s:'W':' " :' ' v V:V % S "':/ :f' F-'F:;- & ' *. CoNfE*<*TE j /5 (? ^OT` Ga? 6PARC.B-P A rocl 0* ^RU o 1 p.0CLoR HO 5 FoRecuT Fro DUCT yic.s/10 9 Co LU mM Fe*1 OU E . S.T.O, Pi t rulATE TV Cni.6 MS A T !OAf i'age 1 PCB-ARCH-EXT0374642 F/LovJ 5 // EZ.T Fo/Z (1%F'o criLoeo 6//v/&a/yC - \kcs - //? r) Ft PAL ; Rem pue I / ' 1 r: > o/*PS&Af T Bir"evyi. tfAreHtAL 0AlAmc ran. MC3f/6$ F>. r* n, 6', * (V) a p ,4/r jp< o, n eT ~^r~ ~W~ ~W~~ ~w~ 5/>/t r Hot i*A 5 L >tie A pact ,'fl *>fAF*u hiz ARat.ta* Lint: Sturm -&r- Ttetyr* Cp u.rr <2> F" ff; <2e> Cmtte 3? M3 -- 0.96 K - 310.1 s . -- 380.(5 253.fi m.n\ "izr- VtntT L-o<f -T" FoFrcu 7 "55" AfOJ //0J ~W~ */ t/MM Pfrft nr f.<TS.O> . "3F" ~2ZT- "W^ n**L Pefi*+r 0CF4/*> prt>m*-r. - 360.25 mo -- --. - 0.03 0.15 0-Cu>to etPHrvn 67.80 - 0.e>8 - \ ti : 17.7a. -- ' 67.7i MSA 5 xt.sn - 8.9+ 50.88 o.lo o.lo - -- o.oQ ~h - Cn to* o 9 / m e* 11 6>.?8 - 0.0/ - -- 6.97 -- 6.97 4-65 a.3d -- - H-.oto a.?/ 2.9/ - - 0.0/ f-- -ML ato PirHEMiL +V.I+ - 0.0+ - - HH.IO -- 44./0 2?.(f0 -- -- ii.Sl 21.5/ 27.5/ - -- 0.0+ pii:,ienepifhe#YL 9.43 -- . . - 1.13 9.63 1.13 /0.76 7-/7 3.59 - - 0.57 /0./9 10.11 - --- Hi tiu ctf L / * r --) ~ ~ UAL - 6./6 6./6 ii-.ll a..o5 -- - . 6./6 4-54 I.io __ -KOJ' -- -- -- 0.60 -- o.6o 0.4 9 0.55 o./6 -- - - 0.4? -- 0.47 -- -- Hcu o.84 -- 0.73 - -- 0.11 ---- ---- -- - '-- ---- - 0.73 - Ca Cl, Hz o V* -- -- -- - -- ---- ---- -- 3.6a. 3.U -- -- o.l 7 0.// -- - ' - o.n - O.I7 - - -- ... 0.05 0.03 0.2.~ 0.05 -- -- - -- - --- -- ... -- -- -- -- - -- - - 3.62. -- (0 'TA L 5I0.5Z. 3.6a. Ff ru* rr, iht, ri.j Uo 76 o 7i r; fr.'t : *Fi. ' P. /5o 25 5.46 76o ISo 0.6o 76 o a5 7. a? 5o8.48 7.99 5/6.57 3yy.3? r/a./F 0.05 368.9? t OO. oo 47.53 MS. 27 2.26 n<oo 76o 76o 740 76 o 76o 36o 34o 'iLo MLo 40 40, ILo ISO ILO /ro ISo /5y 70 330-235 osszU a?2. /?7-270 3oo 4.38 /.OB 76 o ILo '1 7o no 7 Page 28 Department 246 - Standard Manufacturing Process Description MCS-1109 . SECTION IV - COMMENTS ON PROCESS Appendix I Process Control Variables Page 30 PCB-ARCH-EXT0374645 PCB-ARCH-EXT0374646 Process Area Variable Or Description of Parameter As It Or Step Parameter Affects Safety, Quality, Yield Rate Or Other ;> / 1. / MATERIALS a. biphenyl (1) ppm H20 (in tank car or truck) Quality and Maintenance Costs (2) Crystallizing Quality Point b. Chlorine (1) $ C12 Quality * \ c. Ferric (l) loride vxvuhydrous) Assay Quality (2) Particle Size Quality d. Lime, Hydrated (1) $ Ca(0H)2 Quality e. Nitrogen (1) Assay Quality MCS- L09 Range For Best Frequency Known Process Of Monitoring Performance Measurement of Variable quency ~ Method Accuracy Interaction With Other Variables How Control Variables Page 31 Comments 250 ppm max. The normal range is 30-100 ppm. Every tank car or truck. rery tank 13,155 ir or rucji. - 2.5 ppm 68.7C min. 68.8-69.0C is normal. I Every tank car or truck. irery tank 10-298 ir or 52 ruck. - 0.1C 80-l>0$ but constant within 1-2$. Not monitored Not anitored 97.0$ min. Not monitored i! .Supplier s analysis accepted.) 97.0$ of Not monitored. particles less than 100 microns is typical. ton^hly Visual only 92$ min. Not monitored. Not (Supplier1 j analysis onitored acce >ted.) 99*9$ min. Not monitored. (Supplie 's analysi i accepted.) hydrates FeCI3: to Heat and blow witi Produced at Anniston, a non-catalyst; N2 or air to Ala. absorbs HC1 to form lower H2O content a corrosive acid. Insufficient active catalyst results in an unstable product. C.P. is an indi cation of purity; any interaction would depend upon the particular impurity. Accept or reject material. If assay fluctuates Assay cannot be badly, specific controlled in gravity cannot be Aroclor depart controlled closely, ment; shut down thus shifting the if too erratic. isomer distribution In general, revapor ized Cl2 contains less air than DeNora Cl2* Assay affects Accept or reject $ FeCl^ in reaction material. mass. Manufactured by: Pennsalt Packaged by: McKesson & Robbins Total catalyst surface area is important as well as concentration. Accept or reject material. Insufficient active catalyst results in poor stability. A rather wide range of particle size is acceptable, however. Assay affects $ Ca(0H)2 in disti llation mass. Accept or reject material. Manufactured by Mississippi Lime Co. The lime should be "vertical" lime; that is, lime that has been produced in a vertical kiln. Presence of 02 Accept or reject Purchased from Air degrades Aroclqr. material. Products Corp. Process Area Variable Or 1 Or Step Parameter ! 2^C,HL0RINATI0N Description of Parameter As It Affects Safety, Quality, Yield Rate Or Other REACTION (CONTINUOUS) a. Raw Material . Charging (1) I0 in Bi0 Feed to #6 Chlorinator Quality and Maintenance Costs (2) $ FeCl3 in Bi0 slurry in catalyst mix tank. Quality (indirectly) (3) $ FeCl3 in #6 Chlori nator Quality 1 (*> $ FeCl3 in #6 Chlori nator Quality t i ! (5) Bi0/Catalyst Safety , l Mix Tank 1 Temperature i . 1 1 ' i. 1 ' __ MCS Range For Best Frequency Known Process Of Monitoring Performance t f 4ea6urement of Variable j> ;ncy Method Accuracy 250 ppm max. (compare to tank car analyses) Approx. 0.5$ by weight is normal. Not monitorel routinely. ! Monitored only by inventory to see that FeCl3 is being used. .lured. 13A55 - 2.5 ppm Typical values . are 0.06-0.20$ by lab analysi 5. No limits have been set. Weekly jee!4y | 0.03$ is mini mum; typical values are 0.03-0.06$. ' 1 Three times week. rt. c. per ' ;e t je |ik f . Ij T-2262 T-2262 1 0.01$ 1 0.01$ 95-105C Weekly Ltitinuous TI A 1C Interaction With Other Variables How Control Variables Page 32 Comments Hydrates FeC13 to If Bi0 tank car non-catalyst;' analyses are o.k. absorbs HC1 to Tom inspect steam a corrosive acid. coils for leaks. Internal steam coils are in both Items 401 and 102 (biphenyl tanks). Concentration of Normally 4 lbs. slurry will of FeCl3 are partially determine charged for each length and frequencjy 10$ Bi0 level j of the slurry added to catalyst charge to #6 mix tank. chlorinator. The concentration of FeCl3 in the Bi0 slurry is not critical However, if the con centration is too high, suspension of the FeCl3 is difficult and frequent pluggage may occur. If it is low, the mix tank has to be recharged frequently. Overconcentration Control by vary The measured concen will have no effect ing the length & tration is rather underconcentrafion frequency of the erratic because good will result in ja Bi0/catalyst slurry sampling is less stable product charge or by difficult. varying the slurrj concentration. Serious overcon centration would increase pluggage problems in the Densitrol unit which controlsthe specific gravity of the crude. (Same as above.) (Same as above.) Variables affecting No adequate contr . There is a steam c temp, are: Bi0 as of this writing with control valve o stg. tank temp., (6/1/72). tank, but heat has amount of steam to never been needed, circulating loop problem has been to tracers, and rate keep from getting tc at which slurry is hot. Flash point ol used. Bi0 is 113C. Jr Measurement of Variable Accuracy Interaction "Mith Other Variables Bow Control Variables Page 37 Comments Manometer in field - 2 ram Hg + 20C i 2$ - 2$ settings are changed, adjust damper to new setting to maximize temp, differential. As pressure' increases, temps, in still pot and column will increase. Maintain proper Not actually used as column head a control tool. pressure and vapor flow rates. Dependent upon pressure in still pot. Maintain proper Using the AT of the column head furnace coil shown in pressure and 4a(3) above, the temp, vapor flow rates. at the coil discharge at the end of the batch will be 3l6-324C. If the controlled Use proper set level were point on level increased and all controller and other factors occasionally (counter numbers, check against etc.) remained the intermediate tank same, the finished outage. product would probably be low in para- content. If the level were decreased, dichlor-] content would be too high. Boildown must proceed far enough to get the paraisomer in specifi cation, but not so far as to make the dichlor concen tration over 1$, max. . Keep instrumen On one occasion a tation working finished batch was properly and run redistilled. Since distillation very little poly consistently from chlorinated material batch to batch. was present, the batch was boiled down to a 4$ level. - 4mm Hg As pressure ! increases, column temps, increase. Keep vacuum jet The initial run of . in good condition MCS-1109 was made Eliminate air with a head pressure leakage. Dead of 280mm. head <10mm. DEPARTMENT 246 - STANDARD MANUFACTURING PROCESS AROCLOR APPENDIX J (Cont'd) Page 43 SAFETY AND TOXICITY DATA (Cont'd) III. B. 5. (Cont'd) of the eyes and mucous membranes of the nose and throat is followed by cough, a feeling of suffocation and later pain and a feeling constriction in the chest. If exposure . has been severe, pulmonary edema may follow with rales being heard over the chest. 6. Fire Hazard: Moderate - can react to cause fire or explosion upon contact with turpentine, ether, ammonia gas, illuminating gas, hydrocarbons, hydrogen and powdered metals. 7. Explosion Hazard: Present by reaction with reducing agents. 8. Disaster Control: Dangerous; emits.highly toxic fumes; will react with water to form toxic and corrosive fumes . of HCl; is heavier than air - gas will hug the ground. People without adequate protection should go across wind until out of the affected area. , C. HCl Off-Gas (Code 828.51) Synonyms 1 Muriatic acid, Chlorohydric Acid, Hydrogen Chloride. Description: Colorless gas. FormulaT HCl. Toxic Hazard Rating: " Acute local: Irritant 3, Ingestion 3, Inhalation 3 Acute Systemic: U Chronic local: Irritant 2 Chronic Systemic: U M. A. C. : 5 ppm in ai"r for 8 hr. day. Toxicology: Hydrogen chloride is an irritant to the mucous membranes of the eyes and respiratory tract. Concentration of 35 ppm causes irritation of the throat after short exposure. Concentrations of 50 to 100 ppm are tolerable for 1 hour. More serious exposures result in pulmonary edema and often laryngeal spasm. Concentrations of 1000 to 2000 ppm are dangerous even for brief exposures. Mists of HCl are con sidered less harmful than the anhydrous form since the droplets have no dehydrating effect. 7. See Hygienic Guide Series on "Hydrogen Chloride". > PCB-ARCH-EXT0374658 DEPARTMENT 246 - STANDARD MANUFACTURING PROCESS AROCLOR . APPENDIX J (Cont'd) Page 44 SAFETY AND TOXICITY DATA (Cont'd) III; (Cont'd) D. Ferric Chloride (Code 33500) 1. Description: Granular solid. 2. Formula: FeCl3 (Anhydrous) 3. Constants: Mol. Wgt. = 166.22, Melting Pt.=sublimes, solubility in H2O = very soluble with heat rise. 4. Toxic Hazard Rating: Acute Local: Irritant T; Ingestion 1 Acute Systemic: U Chronic Local: Irritant 1 Chronic Systemic: U .5. Fire Hazard: There is no fire hazard under normal conditions, but it will emit toxic fumes at high temperatures. 6. Handling: Protect the skin with approved protective clothing, avoid the breathing of FeCl3 dust, wear approved respirator with adequate cartridge, and protect the,eyes . with approved goggles. . ..There are no storage regulations; however, it. should "be stored in a dry place as heat is, released upon solution in water and wet ferric chloride will not catalyze the chlorination reaction. E. Lime (Code 38800) (Calcium Oxide)* 2 3 4 5 6 7 . 1. Description: Fine white or slightly gray powder, Rhomeric Trigonal crystals. 2. Formula: CaO. . 3. Toxic Hazard Rating: Acute local: Irritant 3; Ingestion 1; Inhalation 3. Acute Systemic: Ingestion 2; Inhalation 3; skin absorption 0. Chronic local: Irritant 3; Inhalation 2. Chronic Systemic: Ingestion 2; Inhalation 3; Skin absorption 0. 4. Toxicology: Has a caustic reaction and, therefore, is irritating to the skin. As a dust it can cause dermatitis and irritation of the eyes and mucous membranes. It is a general nuisance type of dust. 5. Fire Hazard: None. 6. ' Explosion Hazard: Virtually none. 7. Handling: , Dust respirator, adequate protective clothing, including rubber coated gloves, optional rubber full cover apron and full cover plastic goggles should be used when PCB-ARCH-EXT0374659 Page 45 DEPARTMENT 246 - STANDARD MANUFACTURING PROCESS AROCLOR . APPENDIX J (Cont'd) ' SAFETY. AND TOXICITY DATA (Cont'd)1 2 3 4 E. 7. (Cont'd) ` handling lime (dust). Adequate ventilation and dust removal equipment should be used in the handling area. Lime is added to the stills to neutralize any liberated HC1 and prevent sublimation of the FeCl3 catalyst1. It is handled in 50# bags. , F. Nitrogen (Code 43099) 1. Description: Colorless gas 2. Formula: N2 3. Constants: Mol. Wt. 28.02; M.P. - 2lOC; B.P. - 195.8C.; Density 1.2506 gr/liter at 0C. 4. Toxicity: None. In high concentrations it is an ** asphyxiant. : PCB-ARCH-EXT0374660 Department 246 - Standard Manufacturing ProcessDescription Page 46 MCS-1109 . SECTION IV - COMMENTS ON PROCESS . Appendix K Background Information During the first quarter of 1971 it was. decided to produce MCS-1109 as. a dye carrier for Geigy. At this point in time the design work for the Aroclor column(CEA 2417) was complete* and so it was modified to accomodate MCS-1109. The additional cost was estimated to be $45/000. ' The first product was made in September 1971 and the last in February 1972. It was made alternately with Aroclor 1016 on the Aroclor column. A total of about 1.2M lbs. of MCS-1109 were produced. Geigy did not purchase MCS-1109 because of possible environmental problems. It was used to replace Aroclor 1221 in the 6000-series blends at the Anniston* Alabama plant* where it was called Aroclor 1221B. Sales of the 6000-series blends were discontinued on 3/31/72. To date there has been no other use for MCS-1109. PCB-ARCH-EXT0374661 Department 246 - Standard Manufacturing Process Description Page 47 MCS-1109 SECTION IV - COMMENTS ON PROCESS Appendix L Time Cycle and Capacity A. Chlorination(continuous) Normal Capacity Biphenyl charge rate 13j000#/hr. l6,300#/hr. Chlorine charge rate l,500#/hr. l,875#/hr. Aroclor 1105 production rate 13j750#/hr. 17,235#/hr. HC1 Off-Gas 750#/hr. 94o#/hr. Within the chlorination step, the biphenyl charging rate is the - limiting factor. An instrument change is all that would be necessary to increase the crude 1105 production rate. For the entire process, however, distillation is the bottleneck. Distillation(batch) Process Step Volume # Gallons of Forward Flow Gallons of Crude Fed and Residue Forward Flow Time,Hrs (1) Charge still pot 18,500 0 0 20 (2) Heat up and line- 1,000 0 out temperatures on total reflux 0 4.0 (3) Strip biphenyl at 4:1 reflux ratio to 10,000 counts. 30,000 . 54.1# 30,000 18.0 (4) Strip biphenyl at 6:1 ratio to 112,000 counts. 6,000 10.8# 6,000 5.0 (5) Stop crude,strip 0 biphenyl at 8:1 to temperature break. 8.1# 4,500 5-0 (6) Distill MCS-1109 0 18.0* 10,000 12.0 (7) Pump out residue 0 9.0 5,000 1.0 Totals i 55*500 gal. 100# ' 55,500 gal. The 10,000 gallons of product is adjusted with an average of 1000 gallons of biphenyl. The finished goods is thus 19-8% of the total crude. 47.0 hrs. JAPACXTY * 111Q'00"gal.MCS-1109 x 720 hrs . x 9.5# x 0.93 OST = 1.5M#/mo. 47.0 hrs. | mo. gal. PCB-ARCH-EXT0374662 Department 246 - Standard Manufacturing Process Description MCS-1109 SECTION IV - COMMENTS ON PROCESS Appendix M Quality Considerations Page kQ PCB-ARCH-EXT0374663 Department 246 - Standard Manufacturing Process Description MCS-1109 SECTION IV - COMMENTS ON PROCESS . . Appendix N Miscellaneous Page 49 PCB-ARCH-EXT0374664 Monsanto FROM (NAME & LOCATION) R. M. McCutchan - WGK REFERENCE December 16, 1971 :aroclor column start-up " FINAL REPORT TO : W. R. Richard Q. E. Thompson R. H. Munch D. R. Cova J. R. Savage H. S. Bergen P. J. Holzapfel N. B. Wolk A. E. Leisy G. L. Bratsch V/. A. Krull W. C. Engman V. Brawley/T. Carrico 0. A. Meyer SUMMARY . . Construction of the--Aroelor Column project (CEA 2417) began in / January 1971 and start-up began in August. The start-up cost account was closed on 12/1/71. Costs were as follows: Construction - Capital Construction - Expense Start-up Expense Budgeted Prior to MCS-1109 $820,000 70,000 100,000 Actual As of 12/9/71 $825*868 94,857 50,650 Start-up costs amounted to about 5.5$ of construction costs. Quality specifications were met on both new products, Aroelor x 1016 and MCS-1109. As a result of these fractionated products, ' Aroelor 1254 and 1260 are now made from column residue. This caused a shift in two properties of the 1254 and 1260. The specifications will have to be amended;. Design capacities were demonstrated on both Aroelor 1016 and MCS-1109. Aroelor 1016 column capacity can be increased by 15-20$. by simply changing the operating procedure. No easy increase in MCS-1109 column capacity is known. The pollution control objectives were met. In the details section of this report are further details on the project objectives, comments and data on the processes, and comments on the equipment installed. /Ol r/[ R. M. McCutchan ! r 1 ap PCB-ARCH-EXT0374665 J --.-DETAILS ........ ...... !.' PROJECT OBJECTIVES A. Cost Objective: Stay within budgets on construction and startup costs. 1. Construction (Summary Only) . . . Capital Expense Appropriation Made Prior to Decision to Produce MCS-1109 $820,000 $70,000 Actual Cost (as of 12/9, N. B. Wolk) 825,868 9^,857 . At the time it, was decided to provide facilities to . produce MCS-1109 in addition to Aroclor 1016, it was ' estimated that the additional cost would be $45,000. 2. Startup . ' Budgeted vs. actual startup costs are shown below: . .. Item..... f. :... Actual Budgeted Raw Materials Utilities Wages - -- - Salaries Wages and Salaries O.H. Supplies Laboratory Clothing, Laundry, Safety TSD Mechanical Expense Miscellaneous ..Contingency $ 265 500 7,692 15,600 4,185 376 6,277 0 4,613 11,281 - 43 0 $ 7,800 8,050 9,920 19,800 6,200 1,000 11,500 1,000 3,080 22,000 1,500 8,150 Totals $50,630 $100,000 Some of the factors which helped reduce the startup costs were: l) No unsaleable material produced. 2J Three operators added to department instead of four. 3) Used two startup foremen instead of three. . 4) No major process or equipment problems. PCB-ARCH-EXT0374666 2. PROJECT OBJECTIVES (Cont'd. ) B. QUALITY Objective: Meet specification qualities on all Aroclor products affected by CEA 2417, which includes new products Aroclor 1016, MCS-1109 and Aroclor 1221, and existing products Aroclor 1254 and 1260. All specification were met on the new products, and only two (refractive index and dielectric constant) were not met on the existing products. Some of the critical properties are shown below, . Property AROCLOR 1016 Specification Average' of 18 Lots Penta/Hexa , Thermal Chemical Chlorides Resistivity, x 109 Power Factor at 60 cycles 0. 4$ max. O.65 ppm max. 500 min. 5.0$ max. 0.25 0.19 10,900 fold method) 1.33$ " It Property MCS-1109 Specification Range on 5 Lots Biphenyl OrthoMeta-' Para-.. ....... DichlorsC.P. 18-22$ 50-70$ 0-5$ .12-23$ 1$ max. 10-l6C 18.4-21.2$ 60.6-62. 4$ 4.0-4.6$ 12. 2-15. 4$ 0.30-0.64$ 9. 2-11. 0C Only one batch of Aroclor 1221 (Capacitor 2l) has been produced. All properties were within specification. The only quality problem encountered was the refractive index and dielectric constant on Aroclors 1254 and 1260. These two products are now made by chlorinating distilled column residue. The lower homologs are not present now as was the case when they were made from biphenyl. There fore,- the specific gravity vs. refractive index correlation has shifted. Chlorination was tried at 190C (instead of 150), but this did not help. New wider refractive index and dielectric constant specifications will be set for Aroclor 1254 and 1260 as soon as sufficient data is available. . PCB-ARCH-EXT0374667 PROJECT OBJECTIVES (Cont'd.) ' ` . C. CAPACITY ' Objective: Demonstrate design capacity of 54 M#/yr. of Aroclor 1016 and 18 M#/yr. of MCS-1109. 1. Aroclor'10l6 The 54 M#/yr. rate ha-s been demonstrated_and the Bracket II capacity has been set at 4.5 M#/mo. on the 1972 ' cost standard. Design operating conditions call for 58,270 gallons of 1016 to be produced during a 60.0 hr. cycle. Actual operations average 59^0,000 gallons produced in a 62-65 hour cycle. . . I 2. MCS-1109 The 18 M#/yr. rate has been demonstrated_and the Bracket II capacity has been set at 1.5 M#/mo. on the 1972 cost standard. Design operating conditions call 7 for 9>335 gallons of 1109 to be produced during a 57.5 ; hr. cycle. Actual operations average 11,000 gallons produced during a 44 hour cycle. This is the same production rate, just a larger batch (see process section). . . 5. -Flexibility ...... On 11/12/71, Aroclor 1242 was produced in the batch 7 " chlorinators for the first time in three years. Its quality was comparable to that chlorinated continuous. This allows us to make 1242 while making MCS-1109. Two ' " ' or three products can be produced simultaneously as ` ,, follows: . Two products: 1. MCS-1109 2. Any one other Aroclor except 1016 Three products: 1. Aroclor 1016 (but not MCS-1109) 2. Aroclor 1242 5. Any one other Aroclor Bracket_II capacity for the take-over distilled Aroclors is 2.0 M lbs./mo. , which assumes either Aroclor 1016 or MCS-1109 is operating at a Bracket II rate. PCB-ARCH-EXT0374668 4 I. PROJECT OBJECTIVES (Cont'd. ) . D. POLLUTION CONTROL ' . Objective: No increase in PCB's leaving Dept. 246 via sewers and no more than 1.0 lbs./day additional to atmosphere. 1. Sewers For a period of time after startup, the lime slurry pump and residue tank pump had leakage problems. The . leakage went to a trench sewer and through a settling basis. The leakage has now been corrected. There was no detectable increase of PCB's in the sewer leaving the department during or after startup. 2. Atmosphere The exhaust from the vacuum jet under normal conditions is as follows: , No. of Samples 5 4 City H20 to Vent Cooler On Off Ave. EM. 6.9 12. 2 Ave. Lbs. /Day 0.09 0.16 The loss of PCB's to the atmosphere from the vacuum jet-is low whether the cooling water to the vent cooler Is on or off. It will normally be left off because it presents a freezing problem during the winter. Under certain upset conditions, emissions can occur. The need for a catch pot in front of the jet will be evaluated. The present procedure in the case of an upset (usually inadequate cooling water to the condenser) is to immediately put the column on total reflux and close the block valve in front on the jet. PCB-ARCH-EXT0374669 5 II. COMMENTS ON PROCESS .. . A. AROCLOR 1016 1. The process calls for 97.3 of the distillate to be taken off while crude 1142 is being fed to the still pot on level control. Residue was to amount to 18$ of the total crude. Actual practice is to feed crude on level control while the column inventory is being established, and then while 98.0-96.5$ of the distillate is being taken. Residue amounts to about 20$ of the total crude. The likelihood of being out of specification on penta/hexa is too great when residue is reduced to 18$. To date, there has been no problem in using up the residue. Some Aroclor 1254 and 1260 is still made from biphenyl. 2. , . If a lower penta/hexa specification were desirable, say 0.2$ maximum instead of 0.4$, residue would amount to 21-22$ of the crude.- This assumes no other process change. Most of the penta/hexa comes over after the crude feed is stopped. A composite of the last 2$ of distillate (800 gallons) shows an average penta/hexa concentration of 2-6$. 3. Column capacity can be increased by approximately 15-20$ by simply running longer at a 3:1 reflux ratio and a shorter period of,time at 5:1. On one occasion, 80$ of the distillate was taken at a 3;1 reflux ratio instead of only 50$. The amount of residue and the penta/hexa concentration in the finished goods were normal. . . 4. The highest temperatures .reached on any 10l6 run to date is 300C in the still pot and 317C in the . circulating loop returning from the furnace. Still pot pressure is 145-150 mm at the end of a run. B. MCS-1109 1. Typical crude 1105 analysis prior to adding the 1142 , lime slurry is as follows: . Biphenyl orthome taparadichlors and higher 73.5-75.0$ 14.0-15.0 2. Seven pairs of analyses show that the acidity of the crude 1105 in #8 chlorinator averages 0.24 mg KOH/gm. , and after it is blown with nitrogen in #9 chlorinator, it averages 0.05 mg KOH/gm. PCB-ARCH-EXT0374670 6. II. COMMENTS ON PROCESS B. MCS-1109 (cont'd.) 3. The process distillation cycle was altered to accomplish two things: a. Increase the finished goods batch size by increasing the amount of crude charged and by minimizing the amount of ortho- stripped back to the biphenyl storage tank. b. Decrease the amount of biphenyl in the unadjusted finished goods batch so that it is always safely below the 22. C$ maximum. . ' ORIGINAL PROCESS Operation Gallons Vol. 1) Biphenyl stripped at 4:1 reflux ratio while feeding crude 34,060 64.8 2) Biphenyl stripped at 4:1 reflux ratio ~- not feeding crude 4,750 9.0 3) Take product at 8:1 reflux ratio; . producjt will average 18-20$ Bi^ 9*335 17.7 4) Pump out residue Total Crude 4,475 8.5 52,620 100.0 CURRENT PROCESS ' Nfc. * * Operation Gallons Vol. $ 1) Biphenyl stripped at 4:1 reflux ratio while feeding crude 2) Biphenyl stripped at 6:1 reflux ratio while feeding crude. At a 4:1 ratio, ortho- starts coming-off with the biphenyl at about 32-33*000 gallons. 30,000 55.1 6,000 11.0 3) Biphenyl stripped at 8:1 reflux ratio while not feeding crude. This is done to lower the biphenyl content .in the-product 4,800 8.8 4) Take product at 8:1 reflux ratio; product will avez'age 10$ 3i0 9*700 17.& 1 PCB-ARCH-EXT0374671 7 II. COMMENTS' ON PROCESS . B. MCS-1109 (cont'd.) Operation Vol. Gallons $ . 5) Pump out residue 4,000 7.5 Total Crude 54,500 100.0 The product is adjusted with an average of 1500 gallons of biphenyl. The finished goods is thus . 20.2$ of the total crude. , 4. In the above operation, steps (l) and (2) are . terminated using the counter (volume of distillate). Step (5) is terminated when the C.P. of the distillate indicates that ortho- is beginning to come over; that : is-, when the C.P, has dropped 2-5* C below the 68.8C C.P. of biphenyl. This cut point could also be made by specific gravity but C.P. is more convenient. The temperature at the top of the column also breaks sharply enough that with experience it could be used as the indicator. Step (4) is ended when the pot . level.reaches 10$, a level determined appropriate by ' distillate analysis. Column temperature, C.P. and specific gravity of the distillate are all changing very slowly at this point. .. 5. The specification on dichlors and higher in the finished goods is 1.0$ maximum. This specification cannot be lowered without- making it very difficult ' to achieve the 12.0$ minimum para- content in the finished goods. A higher reflux ratio is of no value. 6. On one occasion, 1109 residue was checked and found to- contain about 56$ (wt. ) chlorine. About 20-25$ of this residue was 1142 from the lime slurry used to neutralize and provide excess lime in the 1105 crude. 7. The highest temperatures reached on any 1109 run to date is 285C in the still pot and 517C in the . ^circulating loop returning from the furnace. Still pot pressure is 465-470 mm at the end of a run. 8. (See copy of memo attached to this report.) PCB-ARCH-EXT0374672 8 III. COMMENTS ON EQUIPMENT . A. REFLUX RATE , , ; The only serious problem is our inability to measure, the reflux flow rate. Two different rotometers have been \ used, and .each gives a widely fluctuating reading. At this writing, it is not known whether the instrument is causing the fluctuation or simply indicating the actual flow. B. LIME SLURRY PUMP ' The seal on this pump failed repeatedly. Apparently the small cyclone on the seal flush line was not separating out enough of the lime in the 1C$ slurry. It is now being flushed with crude 1142 from #1 Intermediate Tank. C. CONDENSER . The condenser capacity seems to be marginal when producing MCS-1109. What would appear to be relatively small process upsets causes the condenser to overheat and steam to form . in the tempered water loop. D. --OIL/GAS CHANGEOVER ' . Currently the Jfurnace must be shut down to change from a gas to an oil supply. Alterations will be made so that each of the three burners can be switched independently, . thus avoiding a shutdown. E. BLOW TANK LEVEL CONTROL ' Controlling the 1142 level in the blow tank by controlling the flow in the circulating line does not work. The last compartment in the tank stays empty. This has not caused a problem, but a means must be found to reestablish level control. , F. PIPING/INSULATION . Tracing and insulation is adequate for Aroclor 10l6 production but not adequate for MCS-1109. Numerous biphenyl freeze-ups have occurred, primarily at bare flanges, nozzles and instrument connections. PCB-ARCH-EXT0374673