Document kmjwdGEV9Qqwq4gN1Y8VkB0LO

SWIFT, SPEARS & HARPER, L.L.P. William b. swift KENNETH R. SPEARS'* CHARLES N. HARPER CLAUDIA H. GARY MIRCHANA S. EVERHART KEVIN POWELL `ALSO ADMITTED IN TEXAS VIA HAND DELIVERY ATTORNEYS AT LAW POST OFFICE BOX 1810 RECEIVED CC'.AVnl -j. /,\rt LAKE CHARLES, LOUISIANA 70602-1810 TELEPHONE (337) 433-0707 s4re9t>(W>ress: 4*ioSor FIRST FEDERAL BUILDING )RIVE 70601 TELEFAX (337) 433-0828 August 31, 2001 Mr. Charles B. Cappel BAGGETT, MCCALL, BURGESS Sc WATSON P.O. Box 7820 Lake Charles, LA 70606-7820 Re: Production of Documents by Monsanto Company in VCM Litigation Dear Bert: Enclosed are copies ofthe documents that you are missing out ofthe documents produced by Monsanto in the VCM litigation. It appears that the copier failed to copy both sides ofsome documents. The only document that I was unable to locate is RSV16576. I will make a note ofthis and ifI come across that particular page I will send it to you. However, it may have been another copier error. Sincerel' MKP/lsj Enclosure cc: Tom Bisdine (w/out enclosure) KEVIN POWELL Page 1 of 4 "April 12. T974 VINYL CHLORIDE DETERMINATION IN UiIR BY ADSORPTION ON ACTIVATED? CHARCOAL AND ANALYSIS BY GAS CHROMATOGRAPHY 1 PURPOSE AND LIMITATIONS This paper describes a procedure for measuring the exposure of personnel to vinyl chloride in the working environment. The method describe the preparation of standards which willdetermine .vinyl chloride i the ranee of 9 to 90 parts per million by volume m air, based on 10-minute sample at a flow rate of 100 ml.per minute. Lower or hi er ppm ranges can be determined by preparing additional _ standards cover the iange desired. (Vinyl chloride can be determined to at least Q.05 ppm by volume in air by this procedure, using more dilu standards.) PRINCIPLE The sample is collected by passing air through a gla tube containing activated charcoal which adsorbs any vinyl chloride vapors present. The vinyl chloride is then desorbe from the charcoal by carbon disulfide extraction and analyzed by g, chromatography. 3 INSTRUMENT PARAMETERS Chromat ogr aph Column Column temperature Injection temperature Detector Carrier Hydrogen flow rate Air flow rate Sample size Retention time AID (Analytical Instrument Davelopm Inc.) Portable Chromatograph* Mod' 511, or equivalent chromatograph* with flame ionization detector. Six-foot x 1/8-inch stainless steel packed with 10% di (2-ethylhexyl) sebacate on Chromasorb P, -80/100 mesh* MAW. 100C isothermal 100C flame ionization detector helium or nitrogen . 23 cc per minute 133 cc per minute 2 ul solvent flush technique 0.5 minute (adjust carrier flow until vinyl chloride elutes at this time) RSV 0011817 p 2 of 4 Alternate Column - Better Resolution Instrument Column Detector * Column temperature Detector temperature Injector temperature Carrier gas Air flow Hydrogen flow Sample size Approximate elution time .Hewlett-Packard 5750 gas chromato graph - dual column, or equivalent. 25-foot x 1/8 inch stainless steel packed with 25% by weight 75% C0880/25% Tergitol E-35 on 40/60 mesh rescreened Chromosorb P. / flame ionization 40 to 100C at 4C per minute 125C 125C helium, 30 ml per minute 350 ml per minute 30 ml per minute 10 U1 6.5 minutes 4 REAGENTS AND APPARATUS a) Personal sampling pump. MSA Model G or Bendix Micronair. Insert an in-line orifice made from a cut-off and restricted (pinched) hypodermic needle in the sampling line to the pump in order to obtain a lOOcc per minute flow on these pumps. b) Hypo-vials, 15-ml size. Cat. No. 12911;. Neoprene septa. Cat. No. 13233; alumina seals. Cat. No. 13214; and hand crimper. Cat. No. 13212, Pierce Chemical Company, Rockford, Illinois. c) Carbon disulfide, spectrophotometric grade d) Activated charcoal. Cat. No. 580-26, Barnebey-Cheney, Columbus, Ohio e) Soap film flow meter, 10-ml size f) Stop watch 5 PREPARATION OF THE ACTIVATED JCARBON ADSORPTION TUBE a) Prepare the activated charcoal by placing the charcoal on a 40-mesh sieve and wash with demineralized water until no visible fines appear in the washings. b) Dry the carbon in a drying oven at 110C until dry and free flowing (overnight). Store in a screw-top, glass bottle until needed. c) Cut 8-mm O.D. x 6-mm I.D. Pyrex glass tubing into 6-inch lengths and fire polish the ends. d) Insert a Pyrex glass wool plug two-thirds of the distance into the glass tubes. The longer section of tubing will be designated as the primary end, while the shorter side of the tubing is the back-up end.' e) Pack the tubes with the activated carbon, using a length of 60 mm in the primary section and 35 mm in the back-up section. Retain the carbon with glass wool plugs. f) Seal the tubes with a red rubber septum or parafilm until ready for use. RSV 0011618 P 3 of A 6 SAMPLING PROCEDURE . a) Remove the seals from the charcoal tube and attached the back-up section to a portable pump by means of a length of 1/4-inch Tygon tubing. b) Set the flow rate at 100 ml per minute through the tube with a calibrated rotameter. (NOTE: The 10-ml soap bubble flow meter can be used to obtain a more precise reading of the air flow through the tube if desired) . c) Record the time the air sampling was started and the time when the sampling is completed. A 10-minute sample may be taken with this system. d) After sampling, recheck the flow rate and reseal the ends of the charcoal tube. Return the tube to the laboratory for analysis. e) Record the termperature and barometric pressure at the sampling site. 7 ANALYTICAL PROCEDURE a) Make a small hook at the end of a piece of wire and remove the glass wool plug from the primary end of the charcoal tube. Make sure that no charcoal particles adhere to the glass wool plug. b) Pour the charcoal into a 10-ml glass-stoppered volumetric flask, pipet 3 ml of carbon disulfide (CS2) into the flask and stopper securely. (CAUTION: Carbon disufide is toxic and should be handled under a hood.) c) Agitate the flask periodically for at least 30 minutes. d) Solvent Flush Injection Technique. This injection technique is designed to eliminate difficulties arising from blow- back or distillation with the needle of the microliter syringe. e) Flush a 10 yd syringe with CS2 several times to wet the barrel and plunger. f) Draw 2 ml of CS2 into the syringe and remove the tip of the needle from the solvent. Withdraw the plunger an additional 0.5 ml to separate the CS2 from the sample with a pocket of air. g) Dip the needle into the sample solution in. the volumetric flask and withdraw the plunger until the air bubble between the solvent and the sample has passed the 2 mark on the syringe. h) Remove the tip of the needle from the sample solution and adjust the volume in the syringe until the meniscus of the air bubble rests on the 2 il mark. .Remove the excess sample solution from the tip of the needle. i) Pull the plunger back an additional 0.5 jil to prevent the sample soluiton from evaporating from the tip of the needle. j) Inject the entire contents of the syringe into the chromato graph. k) Measure the peak height and determine the vinyl chloride content from a previously prepared calibration curve. RSV 0011819 p 4 of 4 8 CALIBRATION CURVE a) Pipet 10 ml of carbon disulfide (CS2) into each of five 15-ml hypo-vials. Cap the vials with the Neoprene septa and aluminum seals, using the hand crimper. b) Place the hypo-vials in wet ice to reduce the vapor pressure of CS2c) Cap one of the valves on a steel sample cylinder containing vinyl chloride with a 1/8-inch Swagelok tubing nut which has a chromatographic septum installed in the nut. d) Insert a hypodermic needle through the septum on the cylinder, open the valve and allow the vinyl chloride to vent through the needle for about 10 seconds to purge the air from the system. Remove the needle. e) Using the appropriate gas-tight syringe fitted with a number 27 gauge hypodermic needle, insert the needle through the septum on the cylinder and allow the pressure of the vinyl chloride to displace the volume of the syringe, flush the syringe two times to remove any air which may have been trapped in the needle. f) Into the respecitve hypo-vials, inject 0.2, 0.3, 0.5, 1.0, and 2.0 cc of vinyl chloride from the syringe. g) Shake the hypo-vials for one minute to put the vinyl chloride in solution. These standards will contain 56, 82, 133, .260, 515 mgra of vinyl chloride per ml. (NOTE: These calcula tions are corrected for the dead space in the gas syringe needle. The cold CS2 solutions in the hypo-vials are under slight negative pressure. Measurements have shown that the dead space in the syringe needle amounts to 0.04 cc, and 0.02 cc of this volume is pulled into the hypo-vial by the negative pressure.) h) Allow the standards to warm up to. room temperature, then inject these standards into the chromatograph using the procedure described in Section 7, paragraphs d through j. Shake the hypo-vials each time just prior to withdrawing a sample. i) Plot peak height versus micrograms of vinyl chloride per ml. 9 CALCUHATION A x 3 x 24.5 L x 62.5 " vinyl chloride, ppm by volume at 25C and 760 mm A mgm per ml of vinyl chloride read from'calibration curve L - total liters of air sample (flow rate x time) RSV 0011820 VINYL CHLORIDE DETE RMINATION IN AIR BY GAS CHROMATOGRAPHY PURPOSE AND LIMITATION This method was developed to detenn: vinyl chloride in air by grab sample taken with a 50-ml hypodermic syringe. Air samples are intro duced directly into the gas chromatograph by means ox a 5-cc gas sampling valve. The minimum detectable concentration of vinyl chloride is about 0.1 part per million (ppm) by volume in air using this procedure. The method- has been written for use with an Analytical Instrument Development portable chroma tograph but can be used with other suitably equipped gas chromatographs. INSTRUMENT PARAMETERS Chromatograph Column Column temperature Injection temperature Detector Carrier, flow rate Hydrogen flow rate Air flow rate Sample size Retention time AID (Analytical Instrument Development, Inc.) Portable Chromatograph, Model 511, or equivalent chromatograph, with flame ionization detector, eight foot x 1/8-inch stainless steel packed with Poropak Q, 50/80 mesh. 100C,.isothermal 100C flame ionization detector nitrogen, 40 cc per minute 26 cc per minute 120 cc per minute 5-cc gas sampling loop approximately 2.8 min. SAMPLING AND ANALYTICAL PROCEDURE a) Grab samples are taken with a 50-ml hypodermic syringe without needle. After taking samples, cap the opening of the syringe with parafilm or a 7/32 Caplug to prevent diffusion of the vinyl chloride from the syringe. Sampl must be analyzed within 30 minutes after taking,as losse of vinyl chloride will occur in the syringe. Samples ma also be taken with pre-conditioned Saran plastic bag if desired. . . ----- b) Turn the gas sampling valve to the load position and connect the 50-ml hypodermic syringe to the inlet. Allow the weight of the plunger to force the contents of the syringe through the 5-cc loop. RSV 0011021 DETERMINATION OF RESIDUAL VINYL CHLORIDE MONOMER IK VINYL RESINS 1 PURPOSE A procedure for determining the amount of residual vinyl chloride present in vinyl resins is described* The resin is dissolved in a solvent and the vinyl chloride analyzed using a gas chroma tographic technique. The method is applicable for use with poly (vinyl chloride), vinyl chloride-vinyl acetate copolymers and other vinyl resins in which there are no volatiles which interfere in the determination. 2 EQUIPMENT AND REAGENTS Gas Chromatograph, Hewlett-Packard (F and M) Model 5750 or equivalent, equipped with a hydrogen flame ionization detector* Tetrahydrofuran, reagent grade. Balance with accuracy to 0.10 gram. 3 SAMPLE PREPARATION Prepare the sample for chromatograph injection by dissolving the test resin in tetrahydrofuran (THF). Weigh 9 grams of TKF into a suitable vial. Add 1 gram of the resin to be tested to the THF. Resin addition should be made as quickly as possible. Cap the bottle and place it on a can-roller to attain complete solution. When complete solution has occurred, the sample is ready for injection into the chromatograph. 4 INSTRUMENT PARAMETERS ' Instrument Hewlett-Packard(F/M) Model 5750 (or equivalent) equipped with hydrogen flame ionization detector. Column 6-ft by 1/8-in. stainless steel tubing' packed with Chromosorb 102, 60/80 mesh. Temperatures: Column Injector Detector 100C for 4 minutes, manually to 250C ' 100C (maximum) 300C (flame ionization) increased Sample Size Flows; Helium Carrier Gas Hydrogen Air 4 microliters RSV 25 cc/minute 20 psi at cylinder head 40 nsi at cylinder head 0011622 -2- Elution Times Vinyl Chloride Tetrahydrofuran 2,8 minutes 6.3 minutes 5 calibration Prepare solution mixtures of varying amounts of vinyl chloride in tetrahydrofuran to cover the expected range of concentration. Obtain from the chromatograph scan the area per cent of vinyl chloride for each sample of known monomer content. Prepare a chart plotting the area per cent vinyl chloride versus the known weight per cent vinyl chloride to establish the relative detector response of the vinyl chloride with respect to tetrahydrofuran. 6 CALCULATION ~ . Determine the area per cent vinyl chloride from the chromatograph scan for the resin solution to be characterized. Multiply this figure by 10, which converts the data to area per cent vinyl chloride based on resin weight. Using the chart developed with the calibration samples, read off the corresponding weight per cent of vinyl chloride. RSV 0011823 TYPICAL CALIBRATION- CURVE Residual Vinyl Chloride Monomer in Vinyl Resin. ' Area- Percent Conversion to Weight -Percent.,.* ,, ... t o in WIGHT PERCENT RSV 0011824 s syKTHETIC SAMPLE OF 1 PPM VINYL CHLORIDE, IN THE SOLVENT (Sawp\a volume ~ 2 Microlitors) * i Tetrahydrofuran > i .104x32 ** SYNTHETIC SAMPLE OF 10 PPM VINYL CHLORIDE IN THE SOLVENT .(Sanple Volume - 2 Microliters) vo u *H <D *H U 6 >* O O *Ch mHfoi >03 xS c tS u 3 *ouH A tte n u a tio n RSV 0011826 TYPICAL PVC RESTK IK THE SOLVENT SCAN 2 44 .A tte n u a tio n Retention Time, Minutes rsv 0011827 SAMPLING GUIDELINES WORKPLACE AIR MONITORING Sampling procedures should meet the following general requirements: 1. Samples collected shall be representative of the individual worker's exposur or of the concentration in a particular work area. 2. Sample records shall include; a) The date and time of the sample collection. b) Duration of the sample collection. c) Volumetric flow rate of sample collection. d) Description of the sampling location. e) Other pertinent information. 3. Breathing zone samples shall be collected as near as practicable to the worker's face without interfering with his freedom of movement. These samples shall characterize the exposure from each job or operation. *4. Work area samples shall be collected at the normal breathing zone level of an average worker. These samples may be used to characterize the exposure from each job or operation, if the time a worker spends in this area is identifiable. 5. Sampling methods and analytical procedures shall be calibrated at least weekly to ensure accuracy. RNWheelerJr/ra May 8, 1974 RSV 0011826