Document mBDg7n49Qz5Q1Nb55jBg1rb5J

April 19, 1978 croduct SAFF r APR 211978 TO: J. B. Charm 3. B. Charm RE: CROSS-INDEX OF VARIOUS CHEMICALS Enclosed for your information is a cross-index of various chemicals and the activities that have taken place by the EPA, CPSC, FDA and OSHA. JWA:ck Enclosure cc: A. E. K. A. W. S. w. M. Baker Bodden Ferguson Reiter Original: Acrylonitrile cc: Arsenic Asbestos Benzene Beryllium Cadmium Trichloroethylene (TCE) Perchloroethylene (PCE) Methyl Chloroform Chloroform Dibromochloropropane Ethylene Dibromide Ethylene Oxide Lead Mercury Chlorofluorocarbons Chromates Coke Oven Emissions DES (Diethylstilbestrol) Methyl Alcohol Nitrosamines Noise Ozone PBB' s PCB's Radiation Sludge Sulflir Dioxide yl Chloride ASI 00009045 center for regulatory services March 6, 1978 Mr. J. W. Anderson Manager, Material Safety Corporate Environmental Services Allied Chemical Corporation P. 0. Box 1057-R Morristown, NJ 07960 Dear Jim: SUBJECT: Completed Paper, Vinyl Chloride Analysis in Food Packaging Enclosed is a copy of the completed paper entitled, The Determination and Confirmation of Less Than One PPB Vinyl Chloride Residues in Polyvinyl Chloride Food Packaging as published by a group of chemists at FDA. Previously I have sent you a copy of an unofficial draft methodology. Sincerely WA0:vb Enclosure Paper WILLIAM A. OLSON, Ph.D. Consultant 2347 Paddock Lane Reston, Virginia 22091 703-620-9175 * 703-860-0078 ASI 00009046 The Determination and Confirmation of _>/cpb Vinyl Chloride Resits 'n Polyvinyl Chloride Food Packaging ,w MAR 9 1976 J. LAWRENCE DENNISON, CHARLES V. SREQER, TIMOTHY McHEAL, ROGER C. ShCER, JOHN A. ROACH, and JAMES A. SPHON Food and Drug Administration, Division of Chemistry and Physics Washington, DC 20204 ABSTRACT The determination and confirmation of residual vinyl chloride (VC) in polyvinyl chloride (PVC) food packaging materials are described. PVC packaging materials are dissolved in dimethyl acetamide (DMA.C). VC is sparged from solution with helium gas and collected in sealed vials of ethanol. Detection and quantitation of VC is performed using a headspace sampling technique and standard gas chromatography (GC) with flame-ionization detection, GC peak heights of about full scale deflection (FSD) are obtained for samples of PVC containing 1 ppb VC. Polymer samples taken from tubing, blood bags, food packaging films bottles, and unprocessed resin were analyzed. Residual VC levels ranged from 0.3 to 913 ppb. Confirmation of VC was done by GC/mass spectrometry (GC/MS) using selected ion recording of m/z 62 and 64 in conjunction with full mass scans to identify components eluting near VC. ASI 00009047 -2- The detection and quantitation of vinyl chloride (VC) in various matrices have been continuing problems for the past several years. Since the implication of VC as a cause of angiosarcoma of the liver (1) and several other diseases (2), there has existed a need for a highly sensitive and specific analytical method for the determination and confirmation of residual VC in PVC food packaging materials. Previous work in this laboratory (3) was limited to quantitative determination of VC from PVC solutions at the 1 ppm level by direct gas-solid chromatographic (GC) injection. Recent work has shown that headspace sampling techniques can in crease sensitivities down to the low ppb range (4-7). PVC materials or PVC solutions were held in sealed vials and heated for fast equili bration between liquid or solid and vapor phases. A large aliquot of the headspace was withdrawn for GC or GC/mass spectrometric injection. Further increases in apparent sensitivity have been achieved by con centration of VC from the polymer solution into another solvent using a sparging technique. This was suggested by Bel 1 ar and Lichtanberg (8) and has been used by Japanese scientists* for several years. Vootnota: Anal, method attached to Dec. 13, 1375 letter from Sumitomo Bakelite Company, Ltd., 345 Park Avenue, New York, NY 10022, to Hearing Clerk, FDA, 5600 Fishe^ Lane, Rockville, NO 20852 ASI 00009048 'f -3- We have modified the sparging and headspace sampling techniques to obtain the described procedures which permit the determination and con firmation of _> 1 ppb VC in PVC materials. Polymer samples of tubing, bottles, blood bags, food packaging films, and unprocessed PVC resins were analyzed using flame ionization detection (FID) and confirmed by GC/mass spectrometry (MS). METHOD Caution Since VC is a gas at room temperature and has been designated a carcinogen (1,9,10) by inhalation, special handling pre cautions must be taken to preserve the integrity of the standards as well as to ensure the safety of the analyst. Only the septa-sealed vials described under Apparatus were found satisfactory for handling VC. Reagents (a) Vinyl chloride. -- (1) Three lb cylinder (99.9" pure), Matheson Gas Products, 6655 Ambertcn Drive, Dorsey, MD. 21227, or equivalent. (2) VC gas standard (0.43 ppm v/v) containing 1.25 ng VC/ml in nitrogen, MG Scientific Gases, Kearny, NJ 07029, or equivalent. (b) Ethanol. --Absolute, Publicker Industries, Inc., 1429 Walnut St., Philadelphia, PA. 19102, or equivalent. Prior to use, test to show absence of co-eluting materials at retention time of VC under conditions of analysis. ASI 00009049 -4- (c) Dimethyl acetamide (DMAC). -- Three Kg bottle, Eastman Practical Grade, Eastman Chemical Products, ?,0. Box 431, Kingsport, VI 37652, or equivalent. Pre-sparge the entire reagent bottle with helium for 2*3 days before use. Prior to use, test to show absence of co eluting materials at retention time of VC under conditions of analysis. \ Apparatus (a) Screw-capoed bottles. -- One oz narrow mouth, 350.5 ml, Ace Scientific Supply Co., 1420 East Linden Ave., Linden, HO 07036, No. 10-4256, or equivalent. Similar bottles with 2 oz capacity. Caps with Teflon-lined septa (Alltech Associates, 202 Campus Drive, Arlington Heights, IL 60004, No. 9522, or equivalent). (b) Gas svririce. -- Two, 5, and 10 ml, Precision sampling Corp., P.0. Box 15119, Baton Rouge, LA 70815, Pressure-Lck, series A-2, or equivalent (c) Mini-Vials. *~ 5 ml, with caps and Teflon-lined septa, Alltech Associates No. 9500, or equivalent. (d) Col lection vials. -- Perkin-Elmer F-42 headspace analyzer vials with gray septa and aluminum seals. Capper (P-E Mo. 105-0iG6) and decapper (P-E No. 105-0107) for vials, or equivalent. (e) Sparging apparatus. -- See descriptive drawings in rigs. 1 and 2. ASI 00009050 -5- (0 Forced draft oven. -- Precision Scientific Co., 3737 '.;est Cortland St., Chicago, IL 60747, Thelco Model 18, or epuivalent. (g) Gas chromatograph. -- Hewlett-Packard Model 752CA, or equivalent, equipped with temperature programmer and flame ionization detectors (using 0.01 in ID flame jets). Operating conditions: Temperature (C) -- injection port 200, detector 130, column 110. After VC elution (t 7 min) program column to 130 at fastest rate and hold for 20 min; gas flows (ml/min) -- helium carrier 35 (0.7 rotameter), helium makeup gas 30, oxygen 345 (3.35 rotameter), hydrogen 35 (0.75 rotameter), electrometer setting, 2 x 10'12 amps full scale (APS). (h) Chromatographic column. -- 6' x 1/8" 0D coiled stainless steel, filled with 30/100 mesh Porapak N; retention time of VC ca 7 min. (i) Gas chromatograph-mass spectrometer. -- Finnigan 330CF electron impact quadrupole mass spectrometer equipped with Finnigan S500 gas chroma tograph and Finnigan 6100 data system. Full mass scans and selected icn recording of m/z 62 and 64 were obtained under computer control. Operat ing conditions: Temperature (C) -- injector 170, column 155, separator 215, transfer line 210; after VC eluted, column vented and programmed to 180C to clear solvent from column; carrier gas helium. 25 ml/min; sample size 2.00 ml headspace at S0C; column listed under (h). (j) Pint bottles. -- Flint glass 16 oz narrow mouth, screw-cao, Fisher Scientific Co., 7722 Fenton Street, Silver Soring, MD 209:2. * Mo 2-833DD, or equivalent, with foil lined caps. ASI 00009051 rlteS. `} -6- Preparation of Standards Accurately weigh 2 oz narrow mouth bottle, Mini-Vial cap, and septum. Add 50 ml absolute ethanol to weighed bottle. Cap and reweigh. In hood, prepare VC stock solution in this bottle by quickly uncapping bottle and adding 0.5-2 g liquid VC from inverted freezer-cooled cylinder of VC. Immediately cap bottle tightly and mix well by shaking. Reweigh and calculate VC concentration by weight (v 10,C00-40,0C0 ppm). Dilute this stock solution by withdrawing aliquots through septum with syringe and injecting into weighed, sealed container (1 cz bottle) of ethanol. Reweigh and calculate VC concen tration either in weight/weight or in weight/volume units (r. 50 ppm). This solution is similarly diluted to yield solution containing 1-5 ppm. Make final dilutions into 10 ml ethanol in collection vial. Prepare working standards in 1-50 ppb range. If refrigerated, these working standards are stable for 1 week. Multiple septum punctures shorten working life of standards. Determine actual VC concentration in headspace of above working standards under conditions of analysis by direct comparison to standard gas (.48 ppm in nitrogen) containing 1.25 ng VC/ml. Calculate average partition coefficient using the following equation: ASI 00009052 n -7- IJ (1) Partition coefficient = Cv/Cl * (0.12/14 ml)/(0.87/10 ml) = 0.11 where Cv concentration in vapor (headspace); Cl = concentration in liquid; 0.13 = 13% determined to be in headspace; 14 ml = volume of headscace (13 ml) plus volume of syringe (1 ml); 0.37 = 37% determined by differ ence to remain in liquid; 10 ml = volume of ethanol standard. Preparation of Solvents and Samples Check absolute ethanol to be used in collection vials for materials co-eluting with VC by carefully pipetting 10.00 ml into one of the vials and sealing the vial with a vial capper. Analyze as described under Analysis. Drill 2 holes in cap of 3 kg reagent bottle of dimethyl acetamide (DMAC) and run 1/16" Teflon or stainless steel tube to bottom of bottle through 1 of the holes. Sparge DMAC using slow flow of helium (5-15 ml/min) for several days at room temperature prior to use. After DMAC free of materials co-eluting at retention time for VC has been obtained (determined by running reagent blank), add 200 ml to 1 pt bottle along with 2" Teflon-coated magnetic stirring bar. Cut thick PVC samples such as tubing and bottles into small pieces which will fit through neck of narrow mouth pint bottles. Prepare film by rolling sample into long narrow tube which can be cut into short ASI 00009053 -8- sections to fit into bottle. Accurately weigh 20.00 g PVC material and add to bottle containing 200 ml DMAC and stirring bar. Tightly cap bottle using cap with foil liner, and stir contents until PVC is com pletely dissolved. Complete solution requires stirring from 2 hr to overnight, depending on PVC formulation involved. Highly plasticized samples dissolve more readily than do more rigid samples. (Mote: Opaque solutions are generally obtained when the PVC composition con tains impact modifiers or pigments.) Analysi s After PVC sample is dissolved in pre-sparged DMAC, add 10.00 ml abso lute ethanol to each of 2 collection vials. Interconnect vials with short lengths of 1/16" stainless steel tubing as shown in Fig. 2, and cool in thick Dry Ice-ethanol slurry for 30 min before use. Fit bottle containing PVC solution with tight cap equipped with 1/16" stainless steel sparge tube extending to bottom of bottle. The apparatus is shown in Fig. 1. Immerse pint bottle containing PVC solution in steam bath and add helium sparge gas via needle valve through 1/16" stainless steel sparge tube at rate of v 85 ml/min. Quickly leak check apparatus by apDlying Snoop (Potomac Valve and Fitting, Inc., 15QQ East Jefferson St., Rockville, KD 20852) to all joints and briefly plug final outlet tube to build up pressure. After leak checking, allow sparge gas to freely pass through PVC solution, through bulkhead fitting, into effluent tube and -into collection vials immersed in Dry Ice-ethancl slurry. Sparging apparatus is shown in Fig. 2. ASI 000090S4 -9- After sparging for 2 to 2 1/2 hr, disconnect collection vials ,,nile still cold, decap using decapper and re-seal using fresh unpunctured septum. Analyze vials immediately or store under refrigeration for < 2 days. For analysis, heat vials to 90C in either water bath or forced draft oven and allow to equilibrate at this temperature for > 1 hr. Heat gas-tight syringe having integral valve to 90C in forced-draft oven. Wear gloves to use preheated gas-tight syringe and withdraw 1.00 ml headspace. Close syringe valve and return syringe containing sample to oven for 5 min to vaporize any condensed solvent. Remove hot syringe and immediately inject sample into gas chromatograph. Make standard VC gas injection (1.00 ml, 1.25 ng) both before and after each headspace sample injection. Quantitate unknown using the following equation. (2) ppb VC in PVC = Total ng VC in sample/20 g = [(ng/ml in HS) 14 ml + (ng/ml in Liq) 10 ml3/20 g combined with equation (1) Cv/Cl = 0.11 where Cl = Cv/0.11 giving ppb VC in PVC = [Cvxl4 ml + (Cv/0.11)10 ml]/20 g = CCv(14 ml + 10 ml/0.ll)]/20 g = 5.25 Cv The remainder of the sample in the collection vials after GC deter mination of residual VC is used to confirm the presence of VC by GC/MS. Equilibrate samples at 90C for 1 hr in a constant temperature bath and withdraw a 2.00 ml aliquot of headspace with a preheated gastight syringe having an integral valve. Inject the sample quickly into the*GC/MS to minimize coding of the syringe and condensation of vapor. ASI 00009055 -10- Calcut ate response areas of m/z 62 and 64 using Finniyan Revision H software. Calculate relative abundance of m/z 62 and 64 fran response areas at retention time of VC and compare to theoretical 3:1 ratio. Results and Discussion Previous unpublished work in this laboratory indicated that quanti tative determinations of VC in PVC at very low levels would require a combination of headspace sampling and sparging. Headspace techniques have the advantage of allowing larger portions of the VC present in the sample to be injected into the gas chromatograph than could be done by direct injection of solutions. Undesirable components can often be reduced or eliminated. Unfortunately, the accurate determination of low ppb levels of VC in solid food packaging materials could not be achieved using headspace sampling alone. This is due to differing and unknown equilibration times from sample to sample. Direct headspace sampling has been shown to reliably detect low levels of VC in several food simulating solvents (6). If the polymer is dissolved in a suitable solvent a favorable partitioning of VC into the headspace may be obtained. Our desire to use a relatively dilute polymer solution to insure rapid equilibration resulted in a low total VC concentration in the headspace for samples containing VC at the ppb level. Therefore, an additional concentration step was needed. Sparging provided a means of transfering VC from a solution of low concentration to one of higher' concentration. The combination of sparging and headspace sampling techniques produced the desired sensitivity. ASI 00009056 1 -u- DMAC was chosen to dissolve the PVC because of its excellent solvent properties and its low volatility. Absolute ethanol was chosen as collection solvent because it remains a liquid at Dry Ice temperatures and is an excellent solvent for VC. Helium was chosen as the sparge gas because of its low solubility in ethanol. The sparge train was designed to use readily available components, the pint bottle being chosen for its convenience in holding 20 g PVC in 200 ml DMAC without entrainment of the DMAC into the gas stream. Some breakage of bottles occurred at the threads, possibly due to overtightening, machining mismatch, or,differences in co efficient of expansion between the glass and brass used in the cap construction. A larger bottle (1 qt) could be used for the determination of VC at lower levels where a larger sample would be required. Figure 1 shows the details of the cap and Fig. 2 shows the assembled sparging apparatus. GC analysis of the headspaces of several PVC samples following sparg ing demonstrated that VC could not be adequately resolved from other components using Carbowax 2QM or Silar 10C liquid phases in con ventional packed columns. Chromosorb 101, Chrcmosorb 103, Pcrapak T, Porapak R, and Tenax GC also provided inadequate resolution. Chro mosorb 104 was marginally useful but is not recommended. The Porapak N column was selected for its excellent resolution of VC from ail en countered interferences except one component eluting after VC which ASI 00009057 -12- n o sometimes precluded baseline resolution. GC/MS analysis showed that this component was isobutane. When using the porous polymer columns, from 45 min to 1 hr was required before the FID baseline was considered adequate for the next analysis. Attempts to shorten these turn-around times by backflushing were unsuccessful. The Hall electrolytic conductivity detector and the Dohrmann microcoulometric detector were evaluated in an attempt to provide interference free detection of VC. These detectors were difficult to use and suffered from a lack of repro ducibility on a day to day basis. Since vinyl chloride interferences were not eliminated by the use of these detectors, the FID remained the detector of choice. We were unable to obtain syringes capable of continued use at 90c. Syringe leakage problems were occasionally encountered due to sustained useage at 90C. Syringes were tested by pulling back the plunger, closing the integral valve, and pushing on the plunger while holding the syringe under water. A stream of bubbles indicated leakage and the syringe was discarded. Pre-sparging of the DMAC satisfactorily removed possible interferences contained therein. No attempts to clean up the absolute ethanol were made. If materials co-eluting with VC were present in the chromatograms of the blank ethanol, a new container was opened and checked. In general, interferences were not a problem. ASI 00009058 -13- Before attempting the analysis of unknown PVC materials, a complete analysis of a reagent blank should be obtained using the sparging apparatus described. A known amount of VC should be sparged from the apparatus to check for recovery, leakage, and the GC retention time of VC under operating conditions. The determination of the partition coefficient was made by analyzing 17 VC-ethanol solutions ranging in concentration from 1.8 to 12 ppb (polymer basis). These solutions (10.00 ml) were prepared in collection vials and analyzed under the conditions of the analysis. Quantitation was effected by direct comparison to the standard gas (0.48 ppm in ) which contained 1.25 ng VC/ml. By using equation 1, the partition coefficient was calculated to be 0.11 with a standard deviation of 0.015. Spiking and recovery studies at levels of 0.7-26 ppb VC in DMAC and in 10% PVC polymer solutions in DMAC were carried out for the entire procedure. The average recovery for 6 analyses of DMAC containing no PVC was 91% with a standard deviation of 3.7. The average recovery for 21 polymer solutions containing 10% PVC was 93% with a standard devi ation of 11.7. The PVC for the recovery studies was free of residual VC. (Note: PVC containing no VC was obtained by several precipitations ASI 00009059 v3 "14- from tetrahydrofuran (THF) into methanol. About 50 g PVC from tubing or film was dissolved in a minimum amount of THF. This solution was slowly poured into a vigorously stirred beaker containing methanol. The ratio of the THF solution to methanol was about 1:10. The pre cipitated PVC was filtered onto a large Buchner furnel and air dried. For processing larger quantities of PVC, a large size blender was used for the precipitation. Generally 2-3 precipitations provided clean PVC if the starting PVC contained no more than about 1 ppm VC. A variety of PVC materials were analyzed using the method described and are tabulated in Table 1. A typical FID chromatogram is shown in Fig 3 along with the chromatogram of the reagent blank. Thirteen samples were analyzed and found to contain VC at levels ranging from 0.3 to 913 ppb. MS was the confirmation step in the method. It proved invaluable in the development of the method by identifying components eluting near the retention time of vinyl chloride. This insured in the final procedure that there were no components co-eluting with the vinyl chloride that would have invalidated the GC quantitation. Full GC/MS scans (m/z 162C0) of 12 of the samples chromatographed on Pcrapak N were obtained to identify the components eluting near vinyl chloride. Figure 4 is the total ion current profile of a typical sample recorded from the elution of carbon dioxide until the elution of ethanol. The reagent blank, and the samples 'were found to contain carbonyl sulfide, procene, water and ace*taldehyde. Chioromethane, isobutane, and butene were identified in most of the samples. Identification of all components was based on ASI 00009060 -15- ff<*lk {* spectral interpretation and comparison with reference compounds analyzed under the identical GC/MS conditions. The sample represented by Fig. 4 contained 2.1 ppb VC. At this level, a VC response was not evident in the total ion current profile but was readily apparent in Fig. 5 which is the selected ion current profile of this sample. Selected ion recording of m/z 62 and 64 was used to confirm the presence of VC. The characteristic 3:1 ratio of these ions at the retention time of VC produced by the natural abundance of 35Cl and 37 Cl in the molecular ion of VC increased the specificity of the method. This ratio was reproducible to within 2% of the theoretical value when the level of residual monomer in the polymer was 1 ppb. Monitoring the m/z 62 and 64 ratio insured that only compounds con taining one chlorine atom and thus the elemental composition of vinyl chloride as a molecular ion or fragment are possible interferences to the GC/MS confirmation. Chiorobutenes, epichlorohydrin and dichloroethane are low molecular weight compounds that produce a fragment at m/z 62 containing one chlorine atom and are potential interferences. Analysis of samples of epichlorohydrin and dichloroethane demonstrated that they elute after VC. The chiorobutenes being heavier than butene would also elute later than VC (11). The lack of co-eluting materials that would have interferred with the FID results made it unnecessary to quantitate the samples by GC/MS, Good quantitation by GC/MS requires strict control of the analytical conditions and the construction of an analytical curve from * standards analyzed simultaneously with the samples. Such an effort was considered redundant in this case. ASI 00009061 1 References (1) Maltoni, C., & Lefemine, G. (1974) Environ. Res. 7, 387-405 (2) Thomas, L.B., Popper, H., Berk, P.D., Selfkoff, I., & Falk, H. (1975) New Eng. J. Med. 292, 17-22 (3) Breder, C.V., Dennison, J.L., & Brown, M.E. (1975) JAOAC 58, 1214-1220 (4) Rosen, J.D., Morano, J.R., Pareles, S.R., Giacin, J.R., 4 Gilbert, S.G. (1975) JAOAC 58, 700-702 (5) Van Lierop, & Stek, W. (1976) J. Chromatoor. 123, 133-137 (6) Diachenko, G.W., Breder, C.V., Brown, M.E,, and Dennison, J.l, (1977) JAOAC 60, 570-575 (7) Steichen, R.I. (1976) Anal. Chem. 48, 1398-1402 (8) Bellar, T.A., Lichtenberg, J.J. (1974) J. Amer. Water Works Assoc. Dec., 739-744 (9) Viola, P.L. (1970) Tenth Int. Cancer Conf., Houston, TX, Session 56, p. 742 (Abstract 29) (10) Viola, P.L., Bigotti, A., & Caputo, A. (1971) Cancer Res. 31, 515-522 (11) Supina, W.A. (1974) The Packed Column in Gas Chromatography, Supelco, Inc., Bellefonte, PA ASX 00009062 Figure Captions: Fig. 1 - Cap details; 1. Hexagonal cap machined from solid brass (1-1/4" flat to flat), threaded to same configuration as glass bottle, drilled and tapped in the top to accommodate a 1/4" Swage!ok bulkhead fitting, 2. For temporary use and preliminary tests a standard metal cap may be used by removing the liner, drilling a hole through the top, removing the surface paint with acetone, and soft solder ing in a bulkhead fitting with the sparge tube attached. The sparge tube is attached to the bulkhead fitting by drilling a hole slightly larger than 1/16" downward at an angle into the bore of the fitting (see Fig. 1). The flats of the nut portion and the upper major part ,of the threads should be avoided. After the insertion c the sparge tube to the proper length (enough to reach the bottom of the bottle), the tube is silver soldered in place. A thick gasket is then cut to fit the inside of the cap. The threads on standard metal caps are not sturdy enough for con tinual use and often strip off after a short time Plastic caps were found to be unsatisfactory for even temporary usage. ASI 00009063 Fig. 2 - Sparge train details; Requires 7" X 1/8" stainless steel tubing, 1/4" to 1/8" reducing union, 5' X 1/8" copper . tubing, and brass cap as shown in Fig. 1. Fig. 3 - Typical gas chromatograms; A, 1 ml headspace of reagent blank B, 1 ml headspace of Sample 3 contain ing 2.1 ppb VC polymer basis (0.4 ng VC injected) Fig. 4 - Total ion current profile of Sample 3 containing 2.1 ppp polymer basis (0.8 ng VC injected) Retention time of VC indicated by arrow. Fig. 5 - Selected ion recording profiles of m/z 62 and 64 of Sample 3 containing 2.1 ppb VC polymer basis (0.8 ng VC injected) ASI 00009064 Table 1. Residual VC found in various PVC samples Sample No. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 Sample descriDtion rigid calendared food grade sheet thin plasticized food film thin plasticized food film plasticized blood bag thin plasticized copolymer food film thin plasticized food film plasticized food and milk tubing plasticized beverage tubing rigid vegetable oil bottle rigid French water bottle French bottle molding compound thick plasticized canning sheet plasticized blood bag reagent blank VC found3, pob 1.2 2.5 2.1 1.2 2.1 0.6b 0.7b 0.7b 120 913 0.6b 0.4b 0.3b fJDc aQuantitated by tangent skimming VC peak and measuring peak height -single determination ^Estimated value - below method1s quantitation limit cNone detected ASI 00009065 i, .4 I.'IS IDE 3CRED TO l/k" ASI 00009066 1/8" STEEL Effluent tube details ASX 00009067 Time (min) ASX 00009068 100 ( RESPONSE response ASI 00009069 64 62