Document zdRYBqL2LDkOO5BXD76mjK75R

EMISSIONS TEST REPORT NEW REACTOR D-700 CONOCO CHEMICALS COMPANY P. 0. BOX 91 ABERDEEN, MISSISSIPPI 39730 JUNE 21, 1982 VAB.0001115669 EMISSIONS TEST NEW REACTOR D-700 CONOCO CHEMICALS COMPANY ABERDEEN, MISSISSIPPI I. INTRODUCTION A. Source Information B. Testing Personnel C. Process Description II. SAMPLING RESULTS SUMMARY A. Emissions Test Results B. PVC Production During Tests III. SAMPLING PROCEDURES A. Sampling Apparatus B. Sampling Procedures IV. ANALYTICAL PROCEDURES A. Analytical Apparatus 1. Slurry Samples 2. Reactor Opening Loss Samples 3. Reagents B. Analytical Procedures 1. Slurry Samples 2. Reactor Opening Loss Samples V. CHAIN OF CUSTODY VI. APPENDIX Operating Data Sheets Sampling Data Sheets Analytical Calculations Analytical Data Standard Gas Certifications Reactor Opening Loss Calculations i A VAB.0001115670 A EMISSIONS TEST NEW REACTOR D-700 CONOCO CHEMICALS COMPANY ABERDEEN, MISSISSIPPI I. INTRODUCTION In accordance with 40 CFR 61, Section 61.67 an emissions test was conducted on June 8 and 10, 1982 for the newly constructed PVC polymerization reactor D-700. The purpose of the test was to demonstrate compliance with 40 CFR 61, Sections 61.64 (a)(2) and 61.64 (e) (1)(ii). A. Source Information The emissions test was conducted at: Conoco Chemicals Highway 2 5 Aberdeen, Mississippi 39730 Questions concerning the testing or this report should be directed to: R. A. Frohreich, Chief Process Engineer Telephone Number (601) 369--8111, extension 2239 Dave Mahler, Environmental Engineer Telephone Number (601) 369-8111, extension 2285 B. Testing Personnel The testing and analytical work was conducted by Conoco Chemicals Company personnel at the Aberdeen facility. Personnel involved in sampling and sample analysis were: Jimmy Grace - Quality Control Technician Dave Mahler - Environmental Engineer Wayne Myers - Engineering Co-Op Student C. Process Description Vinyl chloride monomer is received at the plant site in railroad tank cars and is transferred by compressors to the VCM storage sphere. The VCM is then pumped to fresh VCM batch tanks which are located in each of the two reactor areas. VAB.0001115671 A MISSIONS TEST NEW REACTOR D-700 CONOCO CHEMICALS COMPANY ABERDEEN, MISSISSIPPI INTRODUCTION (CONTINUED) C. Process Description (Continued) PVC is produced batchwise from the vinyl chloride monomer. The plant produces only one type of resin; that by the suspension polymerization process. The evacuated to remove air and inert gases and is then charged with carefully measured quantities of VCM, water and a suspension agent. The reaction is initiated with a peroxide type catalyst. Following completion of polymerization, the reaction is killed and the unreacted VCM is removed from the reactor in the recovery sequence. The recovery system is designed to recover unreacted VCM for recycle to subsequent batches. During the pressure recovery phase, VCM vapors are pulled from the reactor and compressed, condensed and liquified. The liquified VCM is routed to the recovered monomer tanks. As a part of the recovery operation, steam is injected into the slurry to aid in the removal of residual VCM in the slurry. When the reactor pressure approaches atmospheric pressure, vacuum pumps are started and the reactor pressure is reduced to a vacuum. These VCM vapors are also compressed and liquified and the liquified VCM is routed to the recovered monomer tanks. By this time the slurry has been brought to a boiling condition by action of the steam injection and the vacuum. The steam blows through the slurry and purges the vapor space above the slurry before being pulled out of the reactor by the recovery system. Cooling water is then put on the reactor in order to cool the slurry down prior to dumping the reactor. When the recovery step is complete, the PVC/water slurry is dumped through a slurry screen which removes oversize material.. The slurry is then pumped to blend tanks. After product pumpout, the reactor is rinsed to the blend tanks, which completes the reaction batch cycle. The PVC/water slurry is pumped from the blend tanks to a centrifuge in the drying area, and the extracted water is discharged to the process sewer. Wet cake is fed to a dryer in which- the resin is dried. The dried resin flows through a product sifter where oversize material is again separated and collected. Resin is then pneumatically conveyed to storage silos and eventually shipped from the plant in trucks or hopper cars. VAB.0001115672 A MISSIONS TEST NEW REACTOR D-700 CONOCO CHEMICALS COMPANY ABERDEEN. MISSISSIPPI II. SAMPLING RESULTS SUMMARY A. Emissions Test Results The following is a summary of results from sampling and analyzing the reactor D-700 vapor space and dumped slurry for each of three batches. D-700 Batch Date Resin Grade Vinyl Chloride Emissions (Lbs. VCM/MM Lbs. PVC) Vapor Space Slurry Total D-700-223 6/8/82 5385 32 82 114 D-700-224 6/8/82 5385 31 57 88 D-700-229 6/10/82 5305 96 107 203 The process employeed at this plant utilizes the reactor for polymerization and stripping. Because VCM flashes out of the slurry and into the vapor space while the reactor is being dumped, it is impossible to accurately segregate the slurry residual and the reactor opening loss. The standard specifies maximum emissions of 400 lbs. VCM/MM lbs. PVC from the slurry and 20 lbs. VCM/MM lbs. PVC from the reactor vapor space. Thus, a maximum emission of 420 lbs. VCM/MM lbs. PVC from the entire reactor is applicable to reactor D-700. The results of the emission tests summarized above demonstrate that reactor D-700 was in compliance with Sections 61.64 (a) (2) and 61.64 (e) (1) (ii) for each of the three reactor batches tested. The total emissions from reactor D-700 did not exceed 420 lbs. VCM/MM lbs. PVC produced. B. PVC Production During Tests The Aberdeen plant had a nominal PVC production capacity of 450 MM lbs. PVC/year at the time of the D--700 emission test. This corresponds to a daily average of 1,233 M lbs. PVC/day. During the two days of emission testing the plant produced 1,007 M lbs./day and 712 M lbs./day respectively, which is less than the nominal plant capacity. The maximum production rate can only be achieved in the winter time when colder cooling water temperatures are available which allow for higher catalyst loadings. Furthermore, the maximum production rate requires perfect reactor scheduling without any reactor or dryer downtime due to maintenance or other delays. VAB.0001115673 EMISSIONS TEST NEW REACTOR D-700 CONOCO CHEMICALS COMPANY ABERDEEN MISSISSIPPI SAMPLING RESULTS SUMMARY B. PVC Production During Tests (Continued) Since the plant utilizes a batch polymerization process, the plant's production rate is increased or decreased by processing more or less reactor batches per unit time. The. size of the reactor batches varies only slightly over long periods of time for any specific grade of resin produced. During the emission testing, reactor D-700 was charged with quantities of VCM which are representative of the current batch size for reactor D-700. A VAB.0001115674 EMISSIONS TEST NEW REACTOR D-700 CONOCO CHEMICALS COMPANY ABERDEEN, MISSISSIPPI A /Vl V (Jiff*IDfAf T! A 9 ** f1>#C|f f jA 1 III. SAMPLING PROCEDURES A. Sampling Apparatus Reactor opening loss samples were taken with the apparatus shown on Figure 1. The components of the apparatus are described as follows: 1. New, unused teflon tubing; 6.4 mm OD. 2. Stainless steel plug valves with teflon plugs, stainless steel hose connectors and interconnecting tubing. 3. 13 liter Calibrated Instruments multilayer gas bags. 4. Rigid container, sealed airtight with RTV gel sealant. ^. . H 5. Gast vacuum pump. 6. Calibrated MSA sampling pump rotameter. 7. Needle valve. 8. Vf Tygon tubing. B. Sampling Procedures The reactor slurry samples were obtained from a sample tap on the reactor dump line. The sample line was kept open throughout the dump period, which purged the line between ------------------ samples. The three slurry samples were grabbed 5, 10 and 15 minutes into the dump period. 2-ounce samples bottles with screwed on covers were used to collect the samples. Immediately following sampling, the sample bottles were taped shut with electrical tape and labeled with the date and reactor batch number. The samples were then stored under refrigeration and analyzed within 24 hours of collection. Reactor vapor space samples were taken immediately after the slurry dump and before the rinse. The sampling train was tightly assembled, using a sample bag which had been leak checked overnight. The sample bag was evacuated until the rotameter indicated zero flow, and the valve was shut. Reactor D-700's top manway was then opened, and the sampling line was lowered into the top of the reactor. The sampling line was purged at a rate of 1 to 2 liters per minute for approximately 1 minute. Immediately following this purge, the sample was taken. The top of the reactor, the middle of the reactor and the bottom of the reactor (within 6 inches of the bottom) were each sampled for 5 minutes, in that order. Flow through the VAB.0001115675 EMISSIONS TEST NEW REACTOR D-700 CONOCO CHEMICALS COMPANY ABERDEEN MISSISSIPPI III. SAMPLING PROCEDURES A. Sampling Apparatus (Continued) sampling train was maintained at 0.5 liters per minute throughout the sampling period. At the end of sampling, the valve above the sample bag was shut, the pump turned off and the sampling apparatus disassembled. The sample bag was transferred to the plant's laboratory and analyzed within 24 hours of sample collection. A >AL VAB.0001115676 - *._______ - ' ' - 'TM' ,m' r< -* > ' J '.4 ^V.;H'V-V- .1 r-- y* * *4 1 v* .. /^i; </. ** ..,, -;- sk ' V- '* > * ?'* J*v^S?- ; , .`r v- 1 '. V*t,. - * h . _ ** !'' ^ i, - A FIGURE 1 REACTOR OPENING LOSS SAMPLING APPARATUS / k" O.D. Teflon^ Tub ing Tygon Tubing Vacuum Pump. Needle Valve rr S.S. Plug Valves VAB.0001115677 EMISSIONS TEST NEW REACTOR D-7QQ CONOCO CHEMICALS COMPANY ABERDEEN, MISSISSIPPI A IV. ANALYTICAL PROCEDURES A Analytical Apparatus 1. Slurry Samples The following apparatus was used to analyze slurry samples for residual VCM: a) Vials, unused with Septa and aluminum seals. b) Analytical balance, with minimum sensitivity of 0.001 gram. c) Syringe, 100 jil, Hamilton #710. d) Vial Sealer, P-E No. 105-0106 e) Filter Flask, 250 ml capacity. f) Buchner funnel, 7 cm. g) Filter paper, Whatman No. 4 h) Pans, disposable aluminum i) Cork borer J) Oven, Blue-M natural draft k) Gas chromatograph, P-E F-42 Headspace Analyzer l) Chromatographic column, stainless steel 2 m X 3.2 mm, containing 0.4% Carbowax 1500 on Carbopak C. m) Thermometer, minimum range 0-100C, minimum sensitivity 0.1 c. n) Sample Tray Thermostat System, Haake Model N3B. o) Integrating Computer, Spectra Physics, SP 4000. P) Barometer, sensitivity 0.1 mm Hg. q) Thermometer, accurate to 1C, near GC. r) Recorder, Houston Instruments potentiometric strip chart recorder set on 1 mm full-scale response and 1 cm per minute chart speed. Reactor Opening Loss Samples I The following apparatus was used to analyze gas bags for VCM: a) Gas chromatograph, HP model 5711 A with a 1.0 ml heated sampling loop in a manual sample valve and flame ionization detector. b) Recorder, Perkin Elmer potentiometric strip- chart recorder set on 1 niv full-scale response and 1 cm per minute chart speed. i VAB.0001115678 i I - - - r. hi ^ *`f l t l H- ** ,s EMISSIONS TEST NEW REACTOR D-7Q0 CONOCO CHEMICALS COMPANY ABERDEEN, MISSISSIPPI IV. ANALYTICAL PROCEDURES (CONTINUED) A. Analytical Apparatus (Continued) 2 Reactor Opening Loss Samples (Continued) c) Chromatographic column, stainless steel, 2.0 m X 3.2 mm, containing 80/100 mesh chromosorb 102. d) Flow meteir, rotameter type with 0-200 ml/minute capacity, with control valve. e) 6 gas regulators, dual stage brass. f) Thermometer, mercury type, accurate to 1 C, mounted near the sample loop. 8) Barometer, accurate to 0.1 mm Hg. h) Pump, ITT diaphram. i) Tubing, teflon, 6.4 mm O.D. %; ,1 kij j) Sample bags. Calibrated Instruments multilayer bag of aluminized Mylar. k) Data Processor, Spectra Physics SP4000. 3. Reagents The following reagents were used to analyze slurry samples and gas bags for VCM: a) Nitrogen Gas, b) Hydrogen Gas, zero grade. c) Compressed Air, zero grade. d) Calibration Gas, 496 ppm VCM e) Calibration Gas, t VCM Calibration Gas, l VCM B. Analytical Procedures 1. Slurry Samples The following pro VCM: a) Sample Storage Slurry samples must be stored under refrigeration. Analyses will be performed after sample has cooled to at least 30C and within 24 hours of collection. VAB.0001115679 4 ' h't EMISSIONS TEST NEW REACTOR D- 7Q0 CONOCO CHEMICALS COMPANY ABERDEEN. MISSISSIPPI IV. ANALYTICAL PROCEDURES (CONTINUED) B. Analytical Procedures (Continued) 1.. Slurry Samples (Continued) b) Slurry Samples eal and record weight, and inum pan (label pan). Set up vacuum aspirator and filter flask assembly. Pour slurry into funnel and start vacuum until steady stream of water stops (15 sec.). Remove vacuum. Use the cork borer transfer about 1.5 g. to the vial and seal it. Take another plug for solids and transfer to an aluminum pan. Quickly weigh and record the pan and save this sample for determination of tota solids. Weigh and record the vial weight. c) Preparation of Gas Chromatograph Flame should be lit at least one hour prior to analyses. Nitrogen pressure of 1.4 kg/cin gives 32 cc/minute. Set hydrogen at 2.1 bar and air at 2.8 bar. The oven should be set at 65 C, the neddle at 150C, and the injector and detector at 150C. d) Programming the Chromatogrpah Set "'1M at 3 seconds, "A" at 07, "BF" at 09 and "S" at 2 minutes. Set "Analysis + Backflush Times" toggle switch __ at "XO.1" position. Both range and attenuation should be at a value of "1". e) Preparation of Sample Turntable The bath should have been on at least 4 hours prior to use. Check the temperature in the turntable to insure it is at 90 + 0.5 C. Insert vials in turntable as follows: Positions 1 and 2 are old standards in the vials from a previous run; positions 3-6 are the calibration standards; positions 7-30 may be samples of any type.- Condition all samples including standards at least one hour (not to exceed five hours) before analyzing. After conditioning, start the chromatograph program and recorder. VAB.0001115680 cr EMISSIONS TEST NEW REACTOR D-700 CONOCO CHEMICALS COMPANY ABERDEEN, MISSISSIPPI IV. ANALYTICAL PROCEDURES (CONTINUED) B. Analytical Procedures (Continued) 1. Slurry Samples (Continued) A f) Determination of Total Solids Place the label aluminum pans in the oven. The oven should be at 110+5 C. Allow the samples to dry for 45 minutes. Remove and cool to room temperatures. Record the weight and calculate the fraction of total solids (dry weight divided by wet weight). Record this value on the data sheet. g) Calibration Standards __ \____ Calibration standards are prepared by filling the vials (at least two sets per series of samples) with the vinyl chloride/nitrogen standards, rapidly seating the septum and sealing with the aluminum seal. Use only stainless steel lines from the cylinder to the vial. The sample line from the cylinder must be purged into the hood prior to filling vials. After line purging, place the end of the tubing into the vial near the bottom and allow purging of the vial for one minute at 1000 cc/minute. (Hold the vial with finger tips only to minimize temperature affect of hand). Slowly remove tubing and quickly cap the vial with the septum and seal. Inject 100 ul of deionized water into vial. 2. Reactor Opening Loss Samples t The following procedure was used to anlayze reactor opening loss samples for VCM: a) Sample Storage Samples must be kept out of direct sunlight during storage. Analysis will be performed after the bag has equilibrated to laboratory temperature and within 24 hours of sample collection. b) Sample Recovery Connect the sample bag to the GC sample valve inlet direct with Teflon ferrules. Prepare the equipment such that the sample gas will pass through the bag, through the sample loop, through the pump, rotameter, and flow7AT2 nnnm^Asi control valve at a rate of 100 ml/minute. 'VAB.0001115681 r * %. EMISSIONS TEST NEW REACTOR D-7QO CONOCO CHEMICALS COMPANY ABERDEEN, MISSISSIPPI IV. ANALYTICAL PROCEDURES (CONTINUED) B. Analytical Procedures (Continued) 2. Reactor Opening Loss Samples (Continued) c) Analysis The GC should be previously prepared such that the column oven and sample loop are equilibrated at 130C n and 100 respectively. The hydrogen flame should be ignited : at least one hour prior to analysis using constant and previously optimized flow rates for both hydrogen and air. Carrier flow at 30 ml/minute should also be established at least one hour prior to analysis. (leave instrument on overnight during routine use.) Observe the baseline to determine both noise level and drift at the 1 x 10^ sen sitivity are acceptable. % With the recorder on and an attenuator setting of 1 x 102 , purge the sample loop with the sample gas at least 30 seconds at 100 ml/minute. Stop the pump, and when the rotameter just indicates no flow, activate the sample valve to inject the sample gas. Mark the injection point on the chart and read the loop temperature and laboratory pressure and temperature. Record all conditions on the chart. Start the SP4000. With the laboratory pressure and temperature, determine the water content of the sample at analysis from a water saturation vapor pressure table (assume 100% relative humidity in the \___________________ sample ). d) Instrument Calibration l Fill evacuated Calibrated Instruments bags with the standard gases, always using the sample bag for the same concentration, daily. Use only stainless steel or the appropriate Teflon tubing connectors. Allow bags to equilibrate to laboratory temperature. Measure each standard gas in duplicate each day using the same GC conditions and procedures described in the above analysis section. Record all conditions as described earlier for each analysis. VAB.0001115682 EMISSIONS TEST NEW REACTOR D-7QO CONOCO CHEMICALS COMPANY ABERDEEN, MISSISSIPPI V. CHAIN OF CUSTODY Slurry samples and gas bags were handled as follows: Slurry Samples * Sample Run No. Taken By Transported By Analyzed By 1 Wayna -Myers Wayne Myers Jimmy Grace 2 Wayne Myers Wayne Ifyers Jimmy Grace 3 Wayne Myers Wayne Myers Jimmy Grace Reactor Opening Loss Gas Bags Sample Run No. Taken By Transported By Analyzed By r 1 Wayne Myers Wayne Myers Jimmy Grace 2 Wayne Myers Wayne Myers Jimmy Grace 3 Waybe Myers Wayne Myers Jimmy Grace A VAB.0001115683 EMISSIONS TEST NEW REACTOR D-700 CONOCO CHEMICALS COMPANY m ABERDEEN, MISSISSIPPI VI. APPENDIX The Appendix of this report contains the raw data and calculations used to obtain the sampling results. This information is presented in the following order: Operating data sheets for reactor D-700 during the three batch sampling period. Sampling data sheets. Reactor opening loss and slurry residual analytical calculations integrator printout data Standard gas certifications Reactor opening loss calculations. A VAB.0001115684 LARGE REACTOR BATCH SHEET CONFIDENTIAL t TYPE DATE FORMULA DURA SEAL Water Tk. % <^j^Counts OiT Level Inches VCTink^J % Catalyst / ^ Cli. unts FVCM j2i^-Type Counts RVCM Oil Seal Water Seal Water Press; /^ro Psig * GPM Psig Pre-charge Amps Running Temp. JL A Pressure r> & nrif PVAIN. 2. Before / TIME INITIAL Reactor & Material OX For Charge Evacuation Start After Net Standard 10 Minutes Evacuation Actual Dev Charge Start Standard 11 Minutes Charge Complete Catalyst Start Time Reaction Temperature Reached Catalyst Complete Turn Around Time His. ML Recovery Start Run Time Recovery Complete Amt Recovered To. /* Dump Start To Tank. 7^7 Rlrif' Mn Actual Dev Standard 3 Minutes Actual Dev, Standard 30 Minutes Actual Dev, Standard 25 Minutes Dump Stop Chem Wash Start Chem Wash Finish Rinse Start Rinse Complete Swirl Start Swirl Complete Total Stripping Steam d * time Reaction Killed t &7J > Actual Dev Standard 25 Minutes Actual Dev Standard 10 Minutes Actual Total Std. m* Dev Dev ** Comments: npj/lnf. VAB.0001115685 A*4 w ,`l * .. <, >> * ." SN-V/ J'J ]* * f` ' .. t i '' ^ . -- ' -p 1 ' * V+ V ":V; 1 1. . + ^ / ** - 1 > -' t ' `H *. ^H ' v' >P * r.t :. : i.^ ** - k ,1p fc t-* *' **.. 4i -1 .` V,'. . - -krT . r* :,r- ' *; - ;:-\~*V ^ - i- v1 .s - 1_ #* H ^ *Vjt*W>yi;* r-r 1 t i * i . -` ^ Il ^ >r,lv^. i-`t ^T. ,* * -- --*4,\v~ -.-- ,. -- ' ->' - - " ?!*** *^ "*" - ' i -bi j ,'^',|> '-"z:'* ** ^ **- C-. .' *v' : * "'': ^ - I/,*'* ,/ '. * * '** '. ^ ''> " m > - * - W,* <*& 1 I I I I < V1 si%A H I I f J l A i" ,,**i t l + I 4 J / f L_" I * < * I r. k- + +* r - ; -*t \. - ** ^ 1 i* *\ -7 -v , - J> +* * i 1 - b' - | L . -v . ^. tJ - ._ -P" % ^ --- ' '. 4 ' n _t f ^ # , , ** -' - -- 1 .J . V * -* * * I VAB.0001115686 LARGE REACTOR BATCH SHEET CONFIDENTIALA REACTO FORMULA TYPE DATE DURA SEAL Water Tk. % /// Counts OiT Level Inches Colloid VC Tank Catalyst A2- Hal Pre-charge Amps Running Temp. Inches 'Counts FVCM Counts RVCM Hd A F Pressure 12&psig TIME INITIAL Reactor & Material O.K. For Charge Oil Pressure Seal Water Seal Water Press: PVA IN. 0. Before After Net GPM Psig Evacuation Start Standard 10 Minutes Evacuation Stop Inches Hg. Actual Dev Charge Start Standard 11 Minutes Charge Complete Catalyst Start Time Reaction Temperature Reached Catalyst Complete Turn Around Time Recovery Start Run Time Hrs. 3? Mi Actual Dev Standard 3 Minutes Actual Dev. Standard 30 Minutes Recovery Complete Amt Recovered To Actual Dev Dump Start To Tank Bldg.* No. Standard 25 Minutes Dump Stop a Chem Wash Start Chem Wash Finish Rinse Start Rinse Complete Swirl Start Swirl Complete Total Stripping Steam MS D m Time Reaction Killed Actual Dev Standard 25 Minutes Actual Dev Standard 10 Minutes Actual "Total Stdr Dev Dev. *4*0 Comments VAB.0001115687 1 -- I- - r " > ' J , _ ' I* - " t ' ' T # " * 1"* T* 4 ir - 1i ^ -* 1 4I tIt ;;j i: 1 l I > wT !l!0 I t < 1 trH+f p' ti j 1 I ** -' V v ' * ,-.v/^Ov* V-**-*- 9+ '* '^ 1 ' J _ r *' TM p* :*'- w v-V.v .-J' |P * .t ;j * >j t -- .+ ` * . - /v;V v -* , -* * >B .* > iV-s'-f' 4U. * - -"1' f- ** b.- 1 t X,-*' J v>>ii Uv fc h n J7:*-> ***-" * .r ^ srit* *--;: i* 1s 1* 7r:--> :j * * -p - - : \* * L 1 -B " V ._ -* ,r> p< I I 'I : M ovn1 I 1 j!i! : ; i I -. I i1i ` PJ ii ir i i r 1 _ H. B! 1 ii % | - + t ( i i i i Hi! I '!i 1 ' - 4/ ; - - - d - + v / 4p r* * : . I. '. t t *. iv r-'*'`f * T-. 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TYPE S3 oX DATE <P--l FORMULA DURA SEAL Water Tk. % ZZlCounts Oil' Level Inches VC Tank J2HjSh Inches /A~ <2 ,Counts lZ-FVCM. O Catalyst / ( Cal Pre-charge Amps t/Q A Counts RVCM Running Temp, f CTA F Pressure pag TIME INITIAL Reactor & Material OJC. For Charge Oil Pressure Seal Water Seal Water Press. 3 la^O PVA IN. ~7 i 1 .'m Before After Net GPM Psig \ X 0-0 o Evacuation Start 2. a Evacuation Stop, Inches Hg. Standard 10 Minutes Actual _ nv Charge Start Standard 11 Minutes TMb3>Q Charge Complete Catalyst Start Time Reaction Temperature Reached <s><>3 Catalyst Complete 07 iJ Turn Around Time //VST Recovery Start Run Time /3S~0 m1 /3S~i7 1 ) 4 3D I JY &4r\ bA Recovery Complete Amt. Dump Start To Tank Dump Stop SH Chem Wash Start __ /sr*iH 1 S'.ysH &*< | Chem Wash Finish Rinse Start Rinse Complete c-/Hh- 7-0 Mi :no.243/ Total Stripping Steam <P /1 m Time Reaction Killed Swirl Start Swirl Complete * Actual _ ... Dev p Standard 3 Minutes Actual Dev Standard 30 Minutes * Actual Dev _ Standard 25 Minutes Actual Dev Standard 25 Minutes Actual Dev Standard 10 Minutes Actual Total Std. * Dev _ Dev Comments /i,, t, VAB .0001115689 -i;^> v>,>'^:A>^^; v.-i ti' f - *: - * - *. " V * ." '' - "* ' *. : '* ' - * '" '- ' 1' ;` ' - f:- . , - ^ " ;^\m ^ *% ^ ., . i , \ - f:- " r , - * : N'. * - *v* -* /< ^; .- ** ,/- - . .. - _ ,,J - . . .- - -J * * -- .' .' * -- ** * ` v' w * I V - V *,jm. *-*> - 'r7^.-.;*-v'. V- -** _ , -- ,, v '--^,r-jJji; :' -Wi> -. A -V^.vv .*-, - '--m. *-* y. ,->: . ... - %' h m '. . - \_V ,S' s - 1* k *" T L 1 ? '|.^t ^ ` /k1,. , r + ,r* . ."- i*#th ^ |,`J v . - lV - ' * '' -T^ 1 * ' . . A -. ` * *- **. H* .r. 1 +d mX m.u:*4 ` + - - > ^ .; r : ^ ?_ ., * -^"*4. -a t>v;;^-4. ;-'v ^-'v^vv V v::V * : ` m. m .. a < _ ,r " . -..... / - ' ' - fV ,p -. -. * .;..- ' . -- ^ *r - - . . 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J* _*' -i >,, _hl . ^TAA,\\ "tV* *^, ' -, * -4A ^'i* - ^ *. _ ^ -M- 4` '-p . - %- . , 4.-V * *,'*' -f"4' / . .# . .. * .^ r V - 1 . f* *+.. *, ,*m .- ;'*' l' ' : .. .* ,m - * * * ' ' , V *-- + * v w Z~w r- > + rr* ~*t **. 1-- .V 1:^V .V .'* ' `4 - . -H . -.>~ * `w ! ti j ' ,J . *-- 'k * ' . .>.Vv1*.f-'..'^*''*>':-* - v/..* * *_ .- ^ ** ' *-.*./ T w* ^ . "b ^ V' , ..' - ;* / 7 * .* - * -v*:, ^ 4 -- -- - -J - /> --- '^r --. ^, 1 ' ^ ` --- ,1 - - f - f ' *.. * ^ VAB.0001115690 A4 CONFIDENTIAL REACTOR D-7QO COMPLIANCE TEST DATE: <z/?6.Z BLEND NO.: RESIN: r t ,* - - b: h: 4 SLURRY SAMPLES DUMP STARTED: /<3 '/o /fM -**1 .j ***** * k " -* r;>N- m - ;> .ry.\;# *-"/!->rf * + l' \r . :i^- V ^ p . . ' -: . * *****Sample ^4- Time Taken By V^L " t *- ..-i ^ * J'!1 -4 * ,> . 1 r-*"*-; . V -kj * ra-r eoift (**/** A :<2Jl#f .5 fy** Transported By Analyzed By Uteyit*- /tytrs" 3?to**y' &vce_^ JrAnGt^/ Iw l/My/* (to REACTOR OPENING LOSS Time Started /o : Taken By /y&Ks Analyzed By J iP Tr i VAB.0001115691 A 4 CONFIDENTIAL REACTOR D-700 COMPLIANCE TEST DATE: BLEND NO.: RESIN: SLURRY SAMPLES DUMP STARTED ^7/fr f T> -r * "j I* 4 V v- r ! : I 1r r * TM r .. t j* , 2 *- Time Taken By A. Transported By an i**/*1 ty** fy*cs .'y 7$ tMayf* PAy** fytrS 6:5ZM! ty-*'* 0*j**-ffy*s Analyzed By <r>*f 3'<z**y REACT0R~0PENING1L0SS Time Started 7/ Taken By IA^y/4 tfytrr Transported By ffy&vs* Analyzed By ZTr^^ VAB.0001115692 REACTOR D-7Q0 COMPLIANCE TEST DATE: BLEND NO RESIN: SLURRY SAMPLES DUMP STARTED: Jf g;rc rfy Way/* ft/trS /Yy** ZTrC*y (fror* REACTOR OPENING LOSS Time Started :^S/T1 Taken By tfysss Transported By /t/vys* /^s'cr Analyzed By <*** VAB.0001115693 PPM, VCM IN AIR BAG SAMPLE ID: DATE: Sample Loop Temperature for Standard (Tr) Sample Loop Temperature for Sample (Ts) Barometric Pressure for ^Standard (Pr) Barometric Pressure for Sample (Ps) * Water Vapor Content of Bag (B) Response Factor (Rf) - Area Standard Area of Sample (As) C vcm - As X PR X Ts X 1 S3: Ps Tr ITS Bag Temperature (B) A CONFIDENTIAL i * VAB.0001115694 I CONFIDENTIAL* ANALYSIS OF PVC SLURRY AND WET CAKE FOR PPM. VCM SAMPLE TYPE: `Tjrf'____________ DATE: 6 ~ 9- /P2-____________ REACTOR: LOT #: 60 ) P, Response Factor (RF) Area of Sample (As) Whole Sample Weight (SW) Dry Weight -f- wet weight (TS) SW x TS - Resin Weight (RW),, RW ~ 1\4 - Resin Volume (RV) SW - RW * Water Weight (WW) RV + WW * Sample Volume (SV) 23.0 - SV * Vial Volume (W) Lab Barometric Pressure at the Time the Standards were Prepared (P) Lab Temperature at Time Standards were Prepared in K * C + 273 * (T) 1 - TS * Water Fraction (TW) A P-O*? 2SLL s/.z RVCM :<dry) RVCM of Sample Dry Basis As P 22 I VAB.0001115695 $ ^HflDEHTlAL ANALYSIS OF PVC SLURRY AND V7ET CAKE FOR PPM. VCM * SAMPLE TYPE: DATE: 4 0 REACTOR: - 7 &<> LOT #: ___ / /S Response Factor (RF) Area of Sample (As) Whole Sample Weight (SW) Dry Weight wet weight (TS) SW x TS Resin Weight (KW) RW -j- 1:4 * Resin Volume (RV) SW - RW Water Weight (WW) RV + WW Sample Volume (SV) 23.0 - SV - Vial Volume (W) Lab Barometric Pressure at the Time the Standards were Prepared (P) A Lab Temperature at Time Standards were Prepared in K - C + 273 (T) 1 - TS * Water Fraction (TW) KVCM )(dry ) VV x 10 -3 ~BB + (tS x 2.36 x 10"3) + (TW x 1.82 x 10-3) RVCM of Sample Dry Basis 4*7. ? As P ; i VAB.0001115696 CONFIDENTIAL ANALYSIS OF PVC SLURRY AND WET CAKE FOR PPM, VCM SAMPLE TYPE: DATE: PJEACTOR: LOT #: "7 00 /C~ Response Factor (KF) Area of Sample (As) Whole Sample Weight (SW) Dry Weight --- wet weight (TS) SW x TS * Resin Weight (KW) ^ RW -J* l.*4 * Resin Volume (RV) SW - RW * Water Weight (WW) RV + WW * Sample Volume (SV) 23.0 - SV - Vial Volume <W) Lab Barometric Pressure at the Time the Standards were Prepared (P) Lab Temperature at Time Standards were Prepared in K * C + 273 (T) 1 - TS = Water Fraction (TW) RVCM (dry) W x 10`3 1 + (TS x 2.36 x 10"3) W RVCM of Sample Dry Basis s As P k V VAB.0001115697 .r t ,4 m PPM. VCM IN AIR BAG HouSAMPLE ID: DATE: (P Sample Loop Temperature for Standard (Tr) Sample Loop Temperature for Sample (Ts) Barometric Pressure for" Standard (Pr) Barometric Pressure for Sample (Ps) % Water Vapor Content of Bag (B) Response Factor (Rf) - Area Standard PM',' VCM "In Area of Sample (As) C vcm As X PR X Ts X 1 RF Fs Tr Bag Temperature 20C 21 (B) .022 .025 24 029 25 031 26 033 27 035 28 037 ' - - - -h.-- -L` . *+ 1 * J \ >1- , A NFIDCNTlAL ICO 100 . ozc, 10 VAB.0001115698 i. .1 .- ;* - - ** "v."1' ,, \ -f '.-V t 'i` ; > . i ^ r ' "> ,, ^ i , -# 'i A CONFIDENTIAL ANALYSIS OF PVC SLURRY AND WET CAKE FOR PPM. VCM SAMPLE TYPE DATE: REACTOR: LOT #: ~?&0 <3 & Response Factor (RF) Area of Sample (As) Whole Sample Weight (SW) Dry Weight -f- wet weightu (TS) SW x TS * Resin Weight (RW) RW 1.4 Resin Volume (RV) SW - RW * Water Weight (WW) RV + WW Sample Volume (SV) 23.0 - SV * Vial Volume (W) Lab Barometric Pressure at the Time the Standards were Prepared (P) Lab Temperature at Time Standards w Prepared in K ** C + 273 (T) 1 - TS Water Fraction (TW) r?4 2.2 .c,z O. 3$ RVCM j(dry) RVCM of Sample Dry Basis 34' } As P t VAB.0001115699 * f "t- ' H -. W * - => ' ' h! : ) i ' H*i '" 4 ' ^^ -1 +* . *> " ** ' /* ** r ' Vn >#W . .'Viv1" A hi1 *V ' *** 1 *: *.r .I," -J ri- -' A CONFIDENTIAL ANALYSIS OF PVC SLURRY AND WET CAKE FOR PPM. VCM SAMPLE TYPE DATE: ^ 3STS ifz. REACTOR LOT #: Response Factor (RF) Area of Sample (As) Whole Sample Weight (SW) Dry Weight - wet weights(TS) SW x TS * Resin Weight (RW) RW 1.4 Resin Volume (RV) SW - RW * Water Weight (WW) RV + WW * Sample Volume (SV) 23.0 - SV * Vial Volume (W) Lab Barometric Pressure at the Time the Standards were Prepared (P) Lab Temperature at Time Standards Prepared in K * C + 273 (T) 1 - TS * Water Fraction (TW) A o'99 a. c.2. - 979 ,4 99 .Loo a *99 e? A ?Oi ^9 s RVCM (dry) W x 10-3 \ + (TS x 2.36 x 10 -3J) W RVCM of Sample Dry Basis + (TW x 1.82 x 10-3) As P VAB.0001115700 ANALYSIS OF PVC SLURRY AND WET CAKE FOR PPM. VCM SAMPLE TYPE DATE: REACTOR LOT #: Response Factor (RF) Area of Sample (As) Whole Sample Weight (SW) Dry Weight wet weight. _(TS) SW x TS - Resin Weight (RW) RW 1.4 Resin Volume (RV) SW - RW * Water Weight (WW) RV + WW ** Sample Volume (SV) 23.0 - SV Vial Volume (W) Lab Barometric Pressure at the Time the Standards were Prepared (P) Lab Temperature at Time Standards Prepared in K - C + 273 * (T) 1 - TS Hater Fraction (TW) RVCM (dry) VV x 10 -3 K57------- + TS x 2.36 x 10 RVCM of Sample Dry Basis a. /. 0) . a? 7 0-37 + (TW x 1.82 x 10'^ As F 3(*'0 I VAB.0001115701 PPM, VCM IN AIR BAG SAMPLE ID: DATE: Sample Loop Temperature for Standard (Tr) Sample Loop Temperature for Sample (Ts) Barometric Pressure for 'Standard (Pr) Barometric Pressure for Sample (Ps) % Water Vapor Content of Bag (B) Response Factor (Rf) Area Standard PPM, " VCM in Area of Sample (As) P C vcm - As X PR X Ts X 1 EF Fs Tr FT Bag Temperature (B) 20C .022 25-- ---------- .031 26 .033 27 28 .035 .037 VAB.0001115702 I J- jr ; "4^;-, 4 L' P rr- >1 . r b m i _ A ^ I i "" 'n -*' '* J . *-* ANALYSIS OF PVC SLURRY AND VIET CAKE FOR PPM. VCM 1 ".*/ ^+ %-* "pi1 ;*<>11 *pff. ^ rt A SAMPLE TYPE: DATE: C // %2-- REACTOR LOT #: 7&V Response Factor (FF) Area of Sample (As) Whole Sample Weight (SW) 4m f * Dry Weight -f- wet weight ITS) SW x TS " Resin Weight (RW) RW 1.4 Resin Volume (RV) SW - RW Water Weight (WW) RV + WW ** Sample Volume (SV) 23.0 - SV Vial Volume (W) ii Lab* .'flu * * Barometric Pressure at the Time the Standards were Prepared (P) * Lab Temperature at Time Standards w Prepared in K - C + 273 * (T) 1 - TS Water Fraction (TW) RVCM (dry) VV x 10'3 I + (ts x 2.36 x 10 RW RVCM of Sample Dry Basis a/ . 97/ , (*94 6 2/ ). 3/i o?9J 0/39 + (tw x 1.82 x 10 -3 As P * VAB.0001115703 f 4 ANALYSIS OF PVC SLURRY AND VIET CARE FOR PPM. VCM SAMPLE TYPE: 3 30 ^ DATE: ________ & ////$ X. REACTOR: LOT #: 4 0D Response Factor (RF) Area of Sample (As) Whole Sample Weight (SW) Dry Weight -J- wet weight (TS) SW x TS Resin Weight (RW) RW -J- 1.4 - Resin Volume (RV) SW - RW * Water Weight (WW) RV + WW Sample Volume (SV) 23.0 - SV Vial Volume (W) Lab Barometric Pressure at the Time the Standards were Prepared (P) Lab Temperature at Time Standards were Prepared in K * C + 273 (T) 1 - TS ** Water Fraction (TW) RVCM (dry) VV x 10 -3-j + (tS x 2.36 x 10-3 RVCM of Sample Dry Basis TW x 1.82 x 10 As P VAB.0001115704 ANALYSIS OF PVC SLURRY AND WET CAKE FOR PPM. VCM SAMPLE TYPE: DATE: REACTOR: ^ J3CL^ Response Factor (RF) Area of Sample (As) Whole Sample Weight (SW) Dry Weight -f- wet weight (TS) SW x TS = Resin Weight (RW) RW -- 1.4 * Resin Volume (RV) SW - RW - Water Weight (WW) RV + WW * Sample Volume (SV) 23.0 - SV - Vial Volume (W) Lab Barometric Pressure at the Time the Standards were Prepared (P) * Lab Temperature at Time Standards were Prepared in K C + 273 (T) 1 - TS Water Fraction (TW) FVCM fw x 10"3 1 + (tS x 2.36 x 10'3 (dry) J\ EJJ J RVCM of Sample Dry Basis As P WTT % * 4 * VAB.0001115705 * * < : - * r* L _ i 0 Sample _ Pressure Loop Temp. _ Column Temp. Flow Rate Attenuator Chart Speed Zsg!3_ p% ' - ' ' . k J ` * ' * T- - .' h ROL VCM CHANNEL 1 INDEX NAME df . , VftCM * M TOTALS 1 " RUN 31 CALIBRATION 1382 MRV FILE 5 CONC 4052 4052 RT 273 * RREfi 63102 S9102 NEW FILE NAME VCM J r w* % CO o I *o VAB-000111570<- Sample _ Pressure Loop Temp. Column Temp. Flow Rate Attenuator . Chart Speed /*t> ROL VCM CHANNEL 1 INDEX 2 NAME VCM TOTALS s. 1982 M A V 3 n q-r qq d.f> RUN 82 FILE 5 METHOD 5 * CALIBRATION CONG RT 4052 4052 273 1 AREA S417S E417E tc'r: 1st 15. 84 NEW FILE NAME VCM RT fe'pr A%% \ Spectra-Phys VAB.O <* ' P ,, * fc. - * L *. Sample _ Pressure Loop Temp. . Column Temp Flow Rate _ Attenuator . Chart Speed lv 1.I ' i- V*.' ft',' \ t ROL VCM CHANNEL 1 INDEX NAME VCM 2 totals RUN 83 CALIBRATION 1982 MAV 3? OS': 37 : H9 -- ---- d FILE 5 ME Tvno i1 ^ A, r> CGMC 4052 4052 RT 278 AREA S6847 S :f 7* yc C c; NEW FILE NAME VCM A 4S 1 t Tn(CDJft Q> "0 VAB.00011157(& * t -*v. * v-i i m* Sample _ Pressure loop Temp. Column Temp. Flow Rate Attenuator . Chart Speed ,.. J, a v i i *?* * A 09E ROL VCM CHANNEL 1 INDEX 1 NAME 1 VCM * TOTALS RUN 84 * CONC 51. 28 51> 23 -s 1882 MAY FILE 5 i METHOD RT 4? 273 - AREA 54 844 QOO Spectra-Physics VAB.OUUU 78 r . x hT* Jl1 '*'**/* :V ^4 ;J' ^ fry >* v- .v- * * Sample _ Pressure Loop Temp. Column Temp. Flow Rate Attenuator . Chart Speed ^ v- . i-' *i . ? > *z : w,- v-t- 4t 4 ROL VCM CHANNEL 1 INDEX NAME V ... .- h -U-- " r,`T 1 VCM 2 W H -- 4- A. Ud -LM. . ^ / , TOTALS RUN 37 CONG 47.57 * 47.57 p 198:Z MRY 39 tD7: 17:12 FILE 5 7 ME'r!!r*0 ^ RT RREP 47 278 11 783 827 iS* 4t Spectra-Physics VAB.00011157 4I 47 273 'V Sample Pressure Loop Temp. Column Temp. Flow Rate Attenuator Chart Speed ROL VCH CHANNEL i 1 INDEX 2 NRME 4 1 VCM TOTALS RUN 38 CONC ' 44. 78 44. 73 199*2 M A V 79 97 27;52 FILE * 5 METNOD 7 RT 47 278 R REA *^ 777 7i * 7r- p - * IS.4S Spectra o VAB.00011157fiL Sample Pressure Loop Temp. Column Temp. Flow Rate Attenuator Chart Speed n* * *10 v ROL VCM CHANNEL INDEX 4 *. I I NAME Ip b VCM * 6 TOTALS RUN CONC 503 ?8 FILE o mm * * ft* RT 278 RRER VAB.0001115'9-2 Sample Pressure Loop Temp. Column Temp. Flow Rate Attenuator Chart Speed JO _ ,.. I . "V - ' A \ 103 1to * J K NFIDENTIAL I QL VCM CHANNEL 1 INDEX 2 NAME ^ ' i r M 3TALS RUN 90 CONC 466 466 1992 WAV 33 07:49- * _ FILE I1 RT AREA W 1 '* -ms I b + %l IS. 46 cn T> o<0 HM * Q> T3 K0 VAB.()011^5713 V '* - * * f-'. < - - J-i - 1 * ''Vi' " '-'**'* '"' ^ - . 1 L. ` * '*. J ', Sample ____4_ 9C Pressure ___ *7it t. Q Loop Temp. _ tto Column Temp. Flow Rate Attenuator Chart Speed 4 p % I- i i -\ * + - 3, * ' -' ^ ** - ** * ROL VCM CHANNEL 1 INDEX 3 NAME VCM TOTALS - RUN 91 CONC 484. 2 484 2 - 1992 MAY 39 07.37 : US * FILE 7 METHOD W% RT 278 AREA 7969 7Q^q a _m *_ejr * r ' * 1 4S % * 4 Spectra-Phyftcs VAB.00U1113 * k Sample _ v?J88 Pressure - ILLS. Loop Temp. _ LM Column Temp. Flow Rate Attenuator Chart Speed / a+*r s, RQL VCM * CHANNEL INDEX Jf: Name vcm TOTALS RUN 92 A CONC 2171 H FILE +* 1 no .I IE. 4E Spectra-Physi VAB.00011157$5 Sample #/S8 Pressure Loop Temp. f*i-o tot} Column Temp. To Flow Rate _ Attenuator _ Chart Speed / ^i Up *** A 107 ROL VCM n .`CHANNEL 1 INDEX 6 NAME VCM ^TOTALS RUN b 94 1982 FILE MAV 39 88.2 5 : 07 A Til y rn - 5 HETrOO CONC 2075 2075 RT AREA . 278 24148 4" 24148 1* S% Ti ? 16. 46 - Spectra -P hysic n .* * -- -S. v1- V*1- -r j. 1' 1 --------------------v*-V 'K-*>' , r . -. -r / '*-'V.-VT. '4 Sample __ Pressure Loop Temp. Column Temp. Flow Rate Attenuator Chart Speed *V >'**.'**'*: -V ' * , ' "t : ' . o . N. J * ROL VCM CHANNEL 1 INDEX NAME. *$ * 1 VCM TOTAL RUN 96 COMC 9140 9140 1982 MAV 39 11:35:30 FILE Mr^vn^s ;i i t(*.4 w RT 182 278 AREA 150442 150658 IV 1 fa 4 u. w* ' I* w \ \ Spectra-Physics VAB.0001115717 I* 1 4 Sample _ Pressure Loop Temp. Column Temp. Flow Rate Attenuator Chart Speed 1, t *,m r 4 h \ i4 i i ) ROL YCM CHANNEL 1 - INDEX 7 HRME 1 VCM TOTALS RUN 37 *9% 193 2 PRY 33 11: 42 : 56 FILE 5 PETHD 0 5 - CQMC 3864 3867 RT 182 - 273 REE :rf 213 145390 14 10 3 KE 16. 46 r A \ + Spectra ^Physics 4 VAB.0001115718 11 .I1 f V. ll'. '--I *'I j i' -* < . .f M 4 % f *P >* C-r ; / - 'V ,' * j p Sample _ t Pressure Loop Temp. Column Temp. Flow Rate Attenuator so Chart Specs I ROL VCM CHANNEL + INDEX 8 NAME i VCM TOTALS RUN 98 CONG 198 j MET*-! ** RRE'.-l 2HQ 147104 -f . -u "+ i * Spectra-Physics VAB.0001115719 Sample Pressure Loop Temp. Column Temp. Flow Rate Attenuator Chart Speed ROL VCM CHANNEL 1 INDEX * 1 NAME 1 VCM TOTALS RUN 99 CONC 3770 3770 pectra-Physics VAB.000111572U I I Sample Pressure Loop Temp. . Column Temp Flow Rate _ Attenuator . Chart Speed IM / ROL VCM CHANNEL. i INDEX 2 NAME 1 VCM TOTALS R'JH 101 COHO 8452 3451 i Spectra-Physi VAB.00011157218 Sample HOL. Pressure Loop Temp. Column Temp. Flow Rate __ Attenuator Chart Speed 1 4 1 RUN 10 CONC 1992 MOV FILE 5 r- * '4 f ". I i i f ) . 4. . *4h * ' +1 "P- *1 *4h. * \ 4 1 Sample _ Pressure Loop Temp. _ Column Temp. Flow Rate _ Attenuator . Chart Speed y / ROL VCM CHANNEL 1 INDEX 9 NAME VCM TOTALS 1982 MRV 40 13:24:41 RUN 107 FILE 5 METHOD If CALIBRATION 4 CGNC RT t 4052 284 RREfl 61060 Kc 15.07 4052 51060 HEW FILE NAME VCM P.T 281 KF IS. 3 < \ % i Spectra- cn VAB.0001115723 8  Sample Pressure Loop Temp. Column Temp. Plow Rate Attenuator , Chart Speeo \ % ROL VCM CHANNEL 1 INDEX 10 NAME VCM TOTALS 1982 MAY 40 13:22 : 57 RUN 108 FILE 5 METHOD CALIBRATION CONC RT 4052 284 RREA S4160 r KF 15. 83 4052 - G 4160 NEI4 FILE NAME VCM RT 282 KF 5. 23 \ ( I, l 4 Sample Pressure Loop Temp. Column Temp. Flow Rate Attenuator Chart Speeo ROL VCM CHANNEL 1 * RUN 109 1982 M R V 40 12:1j 5:29 FILE 5 METHOD 5 INDEX 11 CALIBRATION - 'W NAME J4 f VCM CONC 4052 RT 284 AREA 62677 KF -i 15. 47 TOTALS 4052 62677 HEW FILE NRME VCM * RT 283 * \ 4 Spectra- Physics VAB.0001115725 mm IT 284 Sample Pressure Loop Temp. . Column Temp Flow Rate _ Attenuator . Chart Spceo /&o V 1^6 / ROL VCM CHANNEL 1 INDEX 12 NAME \ 1 VCM * - i r TOTALS - RUN 110 CONC 50. 38 50. 38 188 2 MAV 40 13:59:57 FILE 5 METHOD 5 - RT 47 284 * RREft ., k 52 815 8S7 p KF IS. 18 t i Spectra-Physl VAB.000111^26 1 * Sample _ Pressure Loop Temp. . Column Temp Flow Rate _ Attenuator . Chart Speed \ 1 RUN 112 coni: 43. 65 JUN CS i RREfl t + t'cr * h ' L. + * , *+ ' ' ' ^ l ** -',d - v. ` *, ' Tr * - \ . " * *** *w\-' ,nr . - ." ' *4 .k * >.**. rt - * * *v.-'-r ' - .- * . - J * k* > -* ; . - ,. ' h v,H-. : -.P ... V.- - ./V . ij -- V' - ..** d/ *- v v- j. iu. *' : > V \ - . .. # *. * : ' *' ^ T- ta '1 '. ^V- viV 3. w-'r-7 -.`j' 4 ^ * V*" " * * J ' . , V, ** t.l l* ' - * *. ." * * ` * 1 * V* *..!- ..: - --v v/ ; v< *j - % - , \r : ./ -*:* * *l*; >.v' - - ' *+ r :1-*: V* ;r ^ V 1 T` M * ' / % ' " - fc r' *- 'f&AfjtxSS?4* . 1* i_ r f qb Ef-'^C .* * .' 4 *.4 * ,9*'r 't * _r * . - 4- - * V .. : . %vr--:- .t .**: ,. p-* * * ' - . __ +*+ h ^ , . y-i '* - v " 1 + # +.. < i V H. Iv-** . -p __ J1 T r< % * "',, ' * : iA ti' r*, *7 w * * ^ - ;V ^ "V -A * * * i., -p-, v '.V \; r>b r. tr f +^ ' ,'>e` <* ^ T * < r* * ^, ;. V p* V * / -'..t 1 **'" ** ^' *. , * V^ < r # h Sample _ Pressure Loop Temp. Column Temp. Flow Rate Attenuator Chart Speed 129 1 i f< 4r . y -4 RUN 113 CONC 50. 75 50. 75 RT 47 284 AREA 47 821 8E3 .. K*7 16. 13 t h% * Sample: Pressure Loop Tcmp. Column Temp. Flow Rate Attenuator Chart Speed / I ROL VCM CHANNEL :1 INDEX 16 NAME VCM TOTALS RUN 114 CONG 445. 1 445. 1 1982 .TUN FILE 5 METHOD AREA 7200 Jr'ir *d 4O J Spectra-Physic VAB. Sample Pressure Loop Temp. . Column Temp Flow Rate _ Attenuator , Chart Speed / h f r % * (' V-*' '-*^1 * to # / * M' 4 ROL VCM CHANNEL 1 INDEX 18 NAME H 1 L Li ;r.. . .^1 " , VCM TOTALS CQNC 28. 6 3. 6 * RT RREA * TCJD to O to V VAB.0001115^0 n Sample Pressure Loop Temp. Column Temp. Flow Rate Attenuator Chart Speed d ROL VCM CHANNEL , 1 INDEX 19 NAME VCM TOTALS RUN 117 CONG 423. 3 423. 3 19S FILE JUH 09 15': 1 O 5 METHOD RT PREA V Spectra-Physics # IT) VAB.000111 ."1 , 4. -* - 1- --, 4_ , V k- -L !.**# # Sample Pressure Loop Temp. . Column Temp Flow Rate _ Attenuator. Chart Speed ROL VCM CHRHHEL # 1 INDEX 20 NRME VCM TOTALS RUN 113 CONC 1943 1943 FILE JUN 0 3 METHOD RT 302 RRER 3150$ 3159S *O _w i- * k * > * CO ooo &l> 2 g VAB.0001115732' * - p 1i m. H > ' \ r 4 - m" r *"* Vi - + >i <* J S wi* L *'*+ 4' 1 3 r '\ * Sample t Pressure Loop Temp. Column Temp. Flow Rate Attenuator Chart Speed /f ROL VCM CHANNEL 1 INDEX Ji NAME t- VCM 21 TOTALS RUN 119 CONC 1948 1948 1982 J'JN 29 3 :22:29 FILE METHOD RT 302 AREA 3131.9 i- Spectra-Physic VAB. 4 * b <1 '11 . I Sample Pressure Loop Temp. Column Temp. Flow Rate Attenuator Chart Speed ROL VCM i CHANNEL 1 INDEX 22 NAME VCM TOTALS RUN 120 CONC 1796 1796 Spectra >Phy$ics V'AB.OOOl115734 ROL vcm CHANNEL . 1 INDEX 31 RUN 129 name 1 2 VCM totals CONC p - 1------------. - ._ 26870 ,26870 197 293 JUN 10 1 nq 5 METHOD BRER 4 , *I - 65 348 434624 4 % "'k TC3"2,f VAB.0001115735 147 ROL VCM CHANNEL . 1 RUN 130 INDEX 32 NAME 1 2 VCM CONG p 24640 TOTALS 24640 198 2 JUN 1 0 15:16 : 50 FILE 5 METHOD * RT 107 197 293 AREA p 6484 318 398621 405423 Vf 1 l........... L 16. 1 - soisXiM-ejpadc; VAB.0001115736  * * m *T * t 9^ 1. ' A t ROL VCM 198 2 JUN 10 15: : 28 CHANNEL 1 INDEX 33 RUN 121 a FILE 5 method NOME CQNC RT RREA vp 1 2 VCM TOTALS 25440 25440 - 56 197 293 5615 411492 417429 L IS. 18 pecira- ri i i VAB.0001115737 h ^ V -** ' I * ' - *--- i>r* ".* c ^ ^ V- S' * < r- ,J 4 * ikJ*. -.,* I. " H X - %' I *,- * . 'i i Tu s > -"?* * V-1 ". * ji x. -# A * Sample _ Pressure Loop Temp. Column Temp. Flow Rate Attenuator , Chart Speed * ROL MOM CHANNEL 1 INDEX 36 NAME VCM TOTALS + RUN 134 1?-1 8! FILE ttjk! hi ' -H.r * 3 MERIT'D 5 CALIBRATION CONC 4052 4052 FT 290 MV ;*' ill* Lt 4 * 68018 62022 -** ;* * 16. ~*2 NEW FILE NOME VCM % P P.T 286 d Y 0 Spectra-Physics VAB.000111i>/3 Sample Pressure Loop Temp. Column Temp. Flow Rate Attenuator , Chart Speed A i S' ROL VCM CHANNEL i INDEX 37 NAME * VCM TOTALS -4 ap;0 JTJN 11 29 : 49 : *3 RUN 135 FIL.E r . MET'-'TiO 5 CALIBRATION rnviiTCv 4052 P.T 290 All * 1 ^ ---- & - -* (/r* * * tr 4052 - hew file HOME VCM ?DQ * . L1> \ Q *D 01 VAB.000111573B01* 1 f Sample _ Pressure Loop Temp. . Column Temp Flow Rate _ . Attenuator . Chart Speed *7 6 O .b I 1 154 * ROL VCM CHANNEL 1 INDEX NAME VCM 38 TOTALS RUN 125 CAL IBRATION CONC *\ I 4052 290 4052 NEW FILE NAME VCM RT 239 \.r 4 * Spectra-Phys VAB.OOOlllS^gtt Sample Pressure 9(a6+(a Loop Temp. Column Temp. Flow Rate Attenuator /, Chart Speed ROL VCF1 CHANNEL 1 INDEX 29 NAME VCM TOTALS RUN 129 CONC 47. 46 47. 46 1982 thm 11 1G. 1448 FILE 5 METI-'CT* *** RT 290 i PEA 767 rTM 1W Kf'sfT f *r 1 is- wLm wmm Spectra-Physlest VAB.0001115 * Sample __ Pressure Loop Temp. Column Temp. Plow Rate Attenuator Chart Speed j y 4 a 157 i ROL VCM CHANNEL 1 INDEX 40 NAME *^ 1 VCM TOTALS - RUN 140 CONC - 47. 95 47. 95 i9s:l JUM 11 10.51:45 FILE - RT 47 237 pwTrt w* 775 e 14 *.'1r IS. IS % Spectra-Physic VAB.0001115^2 % * O OO Ty 1 Sample Pressure Loop Temp. Column Temp. Flow Rate Attenuator Chart Speed A 158 J POL VCM CHANNEL 1 INDEX . NAME 41 1 VCM TOTALS 1S3Z2 JUM 11 11 1C .Z2 RUN 141 FILE 3 >t * CGNC RT Qi 1p1 ^i Twtrai!* !*r- ... 50. 27 50. 37 50 i .* n ** O *4 ,4 o *r ^ -f -- ** </> o n a) i Ui If VAB.00011157w33 * i Sample Pressurc Loop Temp. Column Temp Flow Rate Attenuator Chart Speed 1 j ROL VCM CHANNEL 1 IN5>EX 42 NAME VCM TOTALS RUN 142 CQNC 470 469, 9 1982 *T1JU*-ti .44.a~L a--a . ji- ;? .. nj.. nJ p FILE 5 1F T ! C' 0 ^ RT 287 opcrp i *i\ tt tr n ss* * . " * -*--* 7 i^ir ' .i ^ -w * j^ * *zZ7 i_ .. \ \ Spectra-Physic VAB.0001115^4  4 + ' T,` 1 ' 4 ?' * " - - -r - J \ 1 . Sample Pressure Loop Temp. Column Temp. Flow Rate Attenuator Chart Speed h 160 / ROL VCM CHANNEL INDEX NAME VCM TOTALS RUN 142 CONC 1382 T! fM W4 t CTT IT 1 Imm 4 ! i 4 *A I Tn<C3DA (A VAB.000111745 * 1 3 Sample __ Pressure ~?6 Q. (t Loop Temp. Column Temp. Plow Rate ______ Attenuator - Chart Speed :/sw7A 4 ROL VCM CHANNEL 1 INDEX 44 NAME VCM TOTALS w RUN 144 CONC 500. 2 500. 2 V t \* *161 j w Spectra- Phys VAB.0001115^6 Sample Pressure Loop Temp. Column Temp. Flow Rate Attenuator Chart Speed ROL VCM CHANNEL 1 INDEX i. t NAME 45 VCM TOTALS 9 RUN 14 CONC 2040 2040 19 $ FILE RT 287 AREA 32968 1I *i i f i\ tih i 1 f t J \J 1 *4 i h 4 I Spectra-P 4 Sample Pressure Loop Temp. Column Temp. Flow Rate Attenuator . Chart Speed ROL VCM CHANNEL * INDEX 46 * NAME 1 VCM TOTALS RUN 146 FILE CONC 2092 2092 RT 287 JUT! 11 1: * r "! f\ f % t% Spectra-Physics VAB.OOOim; Sample Pressure Loop Temp. Column Temp. Flow Rate Attenuator Chart Speed k, V ROL VCM CHANNEL ' t INDEX '' ' ^NRNE 47 VCM 'j ** TOTALS RUM 147 199 FILE JUN 11 11:*TM:27 Mr i V. .1 * p CQNC 2169 RT AREA 061 i i * * * tT Spectra-Physi VAB.0001115^4-9 IAM*iO/77>A A DIVISION or WUL ROSS, INC Minted in u.s.a. FORM AAA-03-2-80 GAS ANALYSIS -CYU" no. > --INVOICE NO. /2?no CONTROL _____________ VOLUME PERCENT GAS REQUESTED ANALYSIS * CARBON DIOXIDE b OXYGEN ____ SuuKMC*.PR00UCTSUSA.INC. GAS ANALYSIS Ati'O&floINVNOOIC/Eo y - 4sf3. CONTROL ft ---- VOLUME PERCENT ? HYDROGEN CARBON MONOXIDE 0 GAS CARBON REQUESTED ANALYSIS i.'. WTROGEN DIOXIDE OXYGEN METHANE HYDROGEN CARBON MONOXIDEV *.* i i om oate NITROGEN * ARGON- ^ ------------------ COMPONENITT MMAAYV 1 l/M'*-"* -- ANALYZED BY _____ AIR METHANE PRESSURE i CONTENTS CUBIC FEET r . READ OTHER SIDE BEFORE USE, *-+-71 F V * # COMPONENT MAY UQUEFY AT. ANALYZED BY " PRESSURE CONTENTS 1 -------------- nJUBIC FEET READ OTHER SIDE BEFORE USE. / f/ CONFIDENTIAL 4 VAB.0001115750 MA<OF3O<R10MJ77<A MBathesori A DIVISION Of WILL ROSS. INC 4 } gas analysis ,o- SS:J7os/ y?i72-,nvho'.ce CONTROL NO. SL VOLUME PERCENT GAS REQUESTED CARBON '= r*.-! - . -, . D,0X,|Ofiis of iinvted shelt oxygEiiife. Use is recommenaed HYDRogothin one ye CARBON^ MONOXf0Eu,a " NITROGEN ARGON * AIR METHANE ^ELIU 'I'CoO^ COMPONENT MAY LIQUEFY AT X/tp*y "f ANALYZED BY PRESSURE CONTENTS CUBIC FEET READ OTHER SIOE BEFORE USE VAB.0001115751 REACTOR OPENING LOSS CALCULATION Data Volume of Reactor, V = 4,487 ft. 3 Barometric Pressure, P = 29.95 in. Hg Reactor Temperature, T - 650R Molecular Weight of VCM, M * 62.5 lb. lb. -mole Gas Constant, R 21.9 (in. Hg) (ft.3) (lb.-mole (R) Density of VCM at reactor conditions, D D = PM = (29.95) (62.5) = 0,131 lb. RT (21.9) (650) ft.3 Fraction of water vapor in reactor gas, W = 0.635 PVC Production, Z = 61,924 lbs. for 5385 resin Z = 57,357 lbs. for 5305 resin Concentration of vinyl chloride in reactor, dry basis, C C = 9210ppm for batch 700 - 223 8955ppm for batch 700 - 224 r . * 25,650 ppm for batch 700-1229 Reactor Opening Loss Calculations ROL (C) (1-W) (V) (D) (Z) (ft.^ VCM) (MM ft.3 dry gas) X __ (ft.3 dry gas) (ft.J reactor gas) X (ft 3 reactor gas) X (lb. VCM) (ft. VCM) X L^l lbs. PVC lbs. VCM MM Lbs, PVC Batch No. 700-223 ROL = (9210) (1-0.635) (4,487) (0.131) 61,924 32 lbs. VCM MM Lbs. PVC Batch No. 700-224 ROL (8955) (1-0.635) (4,487) (0.131) (61,924) = 31 lbs. VCM MM Lbs. PVC A VAB.0001115752 * * Conoco Chemicals Company Conoco Inc. P. O. Box 91, New Highway 25 Aberdeen, Mississippi 39730 (601) 369-8111 A April 7, 1982 =V n % Mr. Jerry B. Banks Mississippi Department of Natural Resources Bureau of Pollution Control P. 0. Box 10385 Jackson, MS 39204 Dear Mr. Banks: In accordance with Section 61.67 of the National Emission Standards for Hazardous Air Pollutants, Conoco Chemicals Company, a division of Conoco Inc. is submitting the attached Emission Test Report for the newly constructed polymerization reactor D-745, at its PVC production facility located in Aberdeen, Mississippi. The new reactor was brought on-line on December 18, 1981. The emission test was conducted on March 9 and 10 at which time you observed one of the test runs. Please note that we regard all information contained in this report confidential. If you have any questions concerning this report, please contact me or Dave Mahler at (601) 369-8111. + Frohreich Chief Process Engineer tap Attachments bcc: JF, , SJV, PEM, DLM, DSC, JCL VAB.0001115753