Document po0yQ77Q3QdLr4NoRkNbdkpB

SUBJECT Consumer Product Safety Committee Thursday, October 13, 1977 Conference Room - Lower Level A 1:00 p.m. AGENDA 1. EPA -- Vinyl Chloride Standard 2. New Jersey, Skevln Bill 3. Bayport Update 4. Summary of EnvironmentalControl Projects '7%^ ,i ^ (1A-otccaJ W. C. Becker R. B. Downey M. Schmiederer R. B. Downey M. Schmiederer cc: W. C. Becker C. Blackfan R. B. Downey N. G. Duke D. L. Kent 7 74 UTHO UU BFG22208 <n c*> oo K L r*' CPSC Members Marie Schmiederer FlELO PO'NT CP DEPT. & BLDG. NO. D/5428 Consumer Product Safety Committee September, 16, 1977 f H i TT C OATE THIS LETTER 9/21/77 Present: W. C. Becker/R. B. Downey/D. L. Kent/F. E. Krause/ J. P. Morrill/R. D. Savage/M. E. Schmiederer Absent: C. Blackfan/N. G. Duke/R. L. Steller 1. Product Liability -- Approval has been granted for filling the position of "responsibility coordinator'1, in the External Affairs group. Coordina tion of testing for emissions in customer plants requires further refine ment. R. D. Savage will be again soliciting comments, from the marketing directors^on W. C. Becker's letter of August 8th on the topic. The basic measuring stick remains: Would we handle this testing in the same fashion for a BFG facility? 2. Vinyl Siding -- Polystyrene (PS) manufacturers are actively promoting PS for home insulation uses. Their flammability flat wall testing at Southwest Research Institute shows PVC siding over PS to perform poorly when subjected to ignition on the siding surface. Corner tests show all materials combinations perform poorly. What these results mean in terms of real life hazards is not clear, at this time. It is hoped that SPI will lay the ground rules in this new PS marketing campaign, so as not to have a deleterious result on other plastic materials. The topic will be discussed at SPI Siding Group meetings on September 20, 21. 3. EPA Vinyl Chloride Standard -- Rather than lose a year in court battles, SPI has decided to seriously evaluate the EDF and EPA newly proposed compromises. However a major stumbling block remains since EDF is insisting on "zero goals," SPI legal representatives will seek a meeting with EPA policy makers on this topic. The Steering Committee will evaluate* tBs. result* of that meeting on September 30. 22638001 4. TOSCA -- KHk held s public hearing last month on its re-proposal of procedures. The data confidentiality issue continues to be requested by Industry. I* 5. Hew Jersey -- BFG was planning to testify on the Cancer Control Bill (SB3035) on September 19. However the Senate Energy and Environment Committee postponed the meeting, late that same day. IfNEXT MEETING -- THURSDAY. OCTOBER 13, 1977, AT 1:00 P.M. IN CONFERENCE ROOM LLA (LOWER LEVEL A). Marie Schmiederer MS/tp IF6*435*C 7 74 liTHO u$A cc: W. C. Becker/R. B. Downey/D. L. Kent/F. E. Krause/ J. P. Morrill/R. D. Savage/M. E. Schmiederer/C. Blackfan/ N. G. IXike/R. L. Steller BFG22209 FOR REVIEW ONLY Do not cite or reprint. Beturn ns and review within 21 days. Du* r..*i.omf nation am Lonfi ration of > Polyvinyl Chloride Food Packaging ppb Residual Vinyl Chloride in J. LAURENCE DEKMISOfl, CHARLES V. BREOFR, TI?THV McNEAl, ROGER C. SNYDER, A. ROACH A.ND JAKES A. SPUON Division of Chemistry and Physics, 3ureau of Foods, Food and Drug Administration, Washington, DC 20204 ABSTRACT The ucten.-ination and confInnation of residual vinyl chloride (VC) In polyvinyl chloride (PVC) food packaging Materials 1$ described. PVC packaging materials are dissolved In dlaethylacetaiatde '(DhAC). VC is sparged froia solution with helium gas and collected In sealed vials of ethanol. Detection and quantitation of VC Is/perforwed using a headspace sampling technique and standard gas chromatography (GC) with fIan**-Ionization detection. GC peak heights of about 5S full scale deflection (FSO) are obtained for sables 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 91j ppb. Confirmation of VC was done by GC/KS using selected ion recording of n/z C2 and 64 In conjunction with full mass scans to loentlfy components eluting near VC. fm & e > z z '\h BFG22210 -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 e 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 GC Injection. decent work has shown that headspace sampling techniques can In crease sensitivities down to the low ppb range (4,5,o,7). PVC materials or PVC solutions were held In sealed vials and heated for fast equilibration between liquid or solid and vapor phases. A large aliquot of the headspace was withdrawn for GC or GC/MS injection. Further Increase In apparent sensitivity has been achieved by concentration of VC from the polymer solution Into another solvent using a sparging technique. This was suggested by teller and llchtenberg (d) and has been used by Japanese scientists (9) for several years. We have modified the sparging and headspace sampling techniques to * ' aeaolw the described pruradames which permit the determination and confirmation of 1 ppb VC In PVC materials. Polymer samples of tubing, bottles, blood bags, food packaging films and unprocessed PVC resins were analyzed using f1ar<e Ionization detection (F10) and confirmed by GC/MS. 226390* BFG22211 C  j- TTfKX1 C<iut1on; Since vC Is a gas at room literature and has been designated a carcinogen (1,10,11) by Inhalation, special handling pre cautions must be taken to preserve the Integrity of the standards as well as to ensure the safely of the analyst. Only the $epta*$ealed vials describee under Apparatus were found satisfactory for handling VC. -.eagefit* U) vinyl chloride. -- (1) Three lb cylinder (99.9* pure), Matheson, or equivalent. (.) VC ,as standard (1.00 ppa) containing 2.6 ng VC/r.l In nitrogen, f G Scientific Gases, Kearny, hJ 07029 or equivalent. (b) Ethanol. -- Absolute, Publlcker Industries, Inc. or equivalent. Prior to use, test to show absence of co-eluting materials at the retention tine of VC unuer the conditions of analysis. (c) Dlinethylacetaialde. -- 3 k.j, Eastman Practical Grade 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 the retention time of VC under the conditions of analysis. Apparatus (a) Screw-capped bottles. -- One or narrow rwth, 35+0.5 rsl, Ace Scientific Supply Co., No. 10-4256, or equivalent. Similar bottles with 2 or capacity. Caps with Teflon-lined septe (Alltech Associates, 'o. 9522, or equivalent). BFG22212 S . f)S 9 2 2 -i- (L) Gas syringe. -- Two, 5, and lo ,1, Precision Sampling, Pressure-Lok, series A-;., or equlvalant. (c) Htul-vlals. -- 5 nl, with ceps and Teflon-lined septa. All tech Associates :*o. 9500, or equivalent. (a) Collection vials. -- P*rk1n-E1er F-42 headspace analyzer vials with gray septa and aluminum seals. Capper (P-C No. 105-C1G6) and decapper (P-F. :io. 105-0107) for vials, or equivalent. (c) Sparging apparatus. -- See descriptive drawings In Figs. 1 nd (f) Forced draft oven. -- Precision Scientific r<wpany, Thelco Model la, or equivalent. (?) Gas chromatograph. -- Hewlett-Packard Model 7620A. or equivalent, equipped with temperature programmer and flame Ionization detectors. Gpcratlng conditions: Temperature (C) -- Injection port 200, detector 250, column 110. After VC elution (% 7 rain) program column to ISO at fastest rate and hold for 20 rain; gas flows (r.l/nln) -- carrier (He), 35 (0.7 rotameter), makeup gas (He), 30, oxygen, 345, (3.35 rotameter), hydrogen, 35, (0.75 rotameter), electrometer setting, ixlO'1* afs, (!i) Chromatographic column. -- 6' x 1/3" 0.0. colled stainless steel (SS), filled with 80/100 mesh Porapak 18; retention time of VC approximately 7 win. BFG22213 CO 'Q ) O Ot % It) Gas chrpiuato ?raph-i .-ass spec trot c ter. -- Finnlgan 22'JOF electron lupact quaurupol* uass spectro;-*otor equipped with Finnlgan 'j5*ju gas chromatograph ana Flnnl^o 100 data system Full i-<dss scans and selected Ion recording of m/z 62 and 64 were obtained under computer control, iterating conditions: Temperature (C) -- Injector 170, colwan 153, separator 215, transfer line 210; after VC eluted, column vented and prograeried to 1G0C to clear solvent fron column; carrier gas hellu:< <-.5 .al/u.ln; sample size 2.00 t-1 headspace at w/V column listed under (h), (j) Pint bottles. -- Hint ' lass U* oi narrow routli, screw cap bottles, Flsner Scientific Ca.,.pany Catalog '.umber <-_c3rD ur equivalent, with foil line! caps. Preparation of Standards Accurately wei h a 2 oz narrow -outh bottle, '-inl-Vial cap, and septus.. A.id Vd ml absolute ethanol to weighed bottle. Tap and /! reweigh. In a hood, prepare 'K stock solution in this bottle by quickly uncapping bottle and adding C.5 - * 3 liquid VC from Inverted freezer-cooled cylinder of VC. Immediately cap bottle tightly and Mx well by shaking, reweigh and calculate VC concentration by weight (> 10,00*40,000 ppi;;). Gilute this stock solution by withdrawing aliquots through the septura with a syringe and Injecting Into a weighed, sealed container (1 oz bottle) cf ethanol. Reweigh and calculate VC concen tration either In weight/weight or In welght/volune units (*v CO ppm). This solution Is similarly diluted to yield a solution containing 1-5 ppo,. make final dilutions Into lo .1 of ethanol In a collection vial. Prepare working standards In the 1 - 50 ppb range. If refrigerated, this working standard Is stable for a period of up to one week.' Multiple septu.. punctures shorten the working life of the standards. .( BFG22214 tO O B S ^Z -6- Determin$ the actual VC concentration in the headspace of the above working standard under condition* or an1yl By pari son to the standard gas (1 ppm in N2) cental MR0 M R8 Calculate an average partition coefficient using tjie following equation: Equation #1: Partition Coefficient * ^ " -2?14.rn.l q.29 CL .71/10 ml where Cv - Concentration in vapor (headspace) CL = Concentration in liquid .29 * 29% determined to be In headspace 14 ml = Volume of headspace (13 ml) plus volume of syringe (1 ml) .71 = 71% determined by difference to remain In liquid 10 ml b Volume of ethanol standard Preparation of Solvents and Samples Chick the absolute ethanol to be used In the collection vials for materials cb-eluting with VC by carefully pipetting 10.00 ml Into one of the vials and sealing the vial with a hand capper. Analyze as described under "Analysis." Drill two holes Into the cap of the 3 kg reagent bottle of dimethyl acetamide (DMAC) and run a 1/16" Teflon0 or stainless steel tube to the bottom.of the bottle through one of the holes. Sparge the DMAC using a slow flow of helium (5-15 ml/min) for several days at room temperature prior to use. After DMAC has been obtained which Is free of materials co-eluting at retention time for VC (determined by running a reagent blank), add 200 ml to a 1 pint bottle along with a 2" Teflon0 coated magnetic stirring bar. * * BFG22215 V '0 B S 9 Z -7- Cut thick PVC samples such as tubing And bottles Into small pieces which will fit through the neck of tho narrow &outh pint bottles. Prepare film by rolling tho sample Into a long narrow tube which can ba cut Into short sections to fit Into th bottla. Accurately weigh 2C.G0 y of PVC material and Add to the bottle containing 200 ! of OHAC and the stirring bar. Tightly cap the bottle using e cap with a foil liner, and stir contents until the PVC Is coepletely dissolved. Complete solution requires stirring froa two hours to overnight, depending ou the PVC formulation Involved. Highly plasticized samples dissolve wore readily than do the wore rigid samples, (iioti - Opaque solutions are generally obtained when the PVC composition contains Inpact modifiers or pigments.) Analysis After the PVC sample Is dissolved In the pre-sparged (MAC, add 10.00 1 of absolute ethanol to each of two collection vials. Interconnect the vials with short lengths of 1/16' SS tubing as shown In Fig. 2, and cool In a thick Dry Ice0 - ethanol slurry for 30 sin before use* Fit tho bottle containing the PVC solution with e tight cep equipped with a 1/16" SS sparge tube extending to the bottos of the bottle. The apparatus Is shown In Fig. 1. Ionerse the pint bottle containing the PVC solution In a steas bath and Add hellun sparge gas via a needle valve through the 1/16 SS sparge tube at a rate of v 35 1/iih. Oulckly leak cl||Ck the apparatus by applying Snoop* to all Joints end briefly plug the final outlet tube In order to build up pressure. After leak checking, allow the sparge qas to freely pass through the PVC solution, through the bulkhead fitting, into the effluent tube and Into the collection ft vials lonersed In the Dry Ice - ethanol slurry- Sparging apparatus Is shown In Fig. 2. BFG22216 ** CO CD O O CO -8- After sparging for 2 to 2 1/2 hours, disconnect the collection , vials while still cold, decap using the deeapper and ?-&! ySlUfl & fresh unpunctured septum. Analyze vials Immediately or stgfp Hn^r refrigeration for no longer than 2 days. For analysis, hep$ vials to 90C in either a water bath or a forced graft pyep and allow to equilibrate at this temperature for a minimum of 1 hour. Heat a gas-tljjht syringe having an Integral valve to 90C in the forced-draft oven. Wear gloves to use the preheated gas-tight syringe and withdraw 1.00 ml of headspace. Close the l.vringe valve and return syringe containing the sample to the oven for 5 min to vaporjze any condensed solvent. Remove the hot syringe and immediately ihject the sample Into the gas chromatograph. Make standard VC gas Injections (1.00 ml, 2.6 ng) both before and after each headspace sample injection. Quantitate the unknown using the following equation (#2) where ppb VC in PVC = Total nq VC in sample _ (nq/ml In HS)14 ml (ng/rol In L1q)10 ml 20 g 20 g combined with equation #1 where -- = 0.29 CL CL - Cv 0.29 Equation # 2 giving Cv ppb VC 1n pvc a (Cv) 14 ml + TP^9TlOT_ml 20 g - E4 ' rar] 20 g = 2.42 Cv The remainder of the sample in the collection vials after GC deter jnlhation of residual VC is used to confirm the presence of VC by GC/MS. Equilibrate samples at 90C for 1 hour In a constant temperature *bath and withdraw a 2.00 ml aliquot of headspace with a preheated gas-tight syringe having an Integral valve. Inject the sample quickly Into the GC/MS to minimize cooling of the syringe and condensation of vapor. BFG22217  :> Calculate the raspeuisa areas of V- 6<: jrt-J ^4 uslr.'j Flnnlnan Ppvlsion l! software. Calculate the relative abundance of f-:/z f*l and rl from the response areas at the retention t1re of vinyl chloride and compare to theoretical 3.1 ratio. F.usults and discussion Previous work In this laboratory Indicated that quantitative jfetfcralnatlons of VC In PVC at very low levels would require a combination of headspace sampling and sparging. Headspace techniques nave the advantage of allowing larger portions of the VC present In the sample to be Injected Into the ,as chromatograph than could oe done by direct Injection of solutions. Undesirable components can often be reduced or eliminated, i ^fortunately, 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 free sample to sample, direct headspace sampling has been shewn to reliably detect low levels of VC in several food sluilatlny solvents (f). If the polymer Is dissolved in a suitable solvent a favorable partition* ing of VC Into the headspace raay be obtained, f'ur desire to use a relatively dilute polymer solution to Insure rapid equilibration resulted In a low total VC concentration in the heedspace for samples containing VC at the ppb level. Therefore, an additional concentration step was needed. Sparging provided a ireans of transferlng VC from a solution of low concentration to one of higher concentration. The combination of sparging and headspace sampling techniques produced the oeslred sensitivity. BFG22218 8 CD O h* h* t'fvU' was chosen to Mssolvo the PVC because of Its excellent solvent properties and Its low volatility. >.J.$clute ethanol was chosen as and Is an excellent solvent for vc. hello.; was chosen as the sparge gas because of Us 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 of PVC In 200 il uf 'WAC without entrainment of the *KAC Into the -ias 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 trass used in the cap construction. A larger bottle (1 c,t) could be used for the determination ,f VC Jt lower levels where a largor saiple would be required. Figure 1 shows the details of the cap and Figure 2 shows the assembled sparging apparatus. (iC analysis of the headspaces of several PVC sarnies following sparging denonstrated that VC could not be adequately resolved fro* other coaiponants using Carbowax 0 ;t or Slier 10 C liquid phases In conventional packed columns, Chrowosorti 10), Chrooosorb 109, Porapak T, Porapak ft. and Tenax r.C also provided Inadequate resolution. Chranosorb 104 was marginally useful but Is not recouuended. The Porapak M column was selected for Us excellent resolution of VC from all encountered Interferences except one component eluting after VC which soiaetlkies precluded baseline resolution. GCA'S analysis showed that this coq>onent was Isobutane. When using the porous pol/rvor coli#..ns, from 4C rln to 1 hour was required before the FIf baseline was considered adequate for the next analysis. BFG22219 ET00S92 -II- *e were unable to obtain syringes capable of sustained use at yOC. Syringe leakage problems were occasionally encountered due to sustained usea<je at '*0C. Syringes were tested by pulling back the plunger, closing the integral valve, and pushing on the plunger while holding the syringe under water, A strata of bubbles indicated leakage and the syringe was discarded. Pre-sparging of the CKAC satisfactorily removed possible interferences contained therein, bo attempts to clean up the absolute ethanol were wade. If materials co-eluting with VC were present la the chromatograms of the blank ethanol, a new container was opened and checked. In general. Interferences were not a problem. Sefore attempting tlie analysis of unknown PVC materials, e complete analysis of a reagent blank should be obtained using the sparging apparatus described. A known amount of VC should then 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 (C*29) was made by analyzing VC-ethanol solutions ranging In concentration from 2.5 to 40 ppb. These solutions (10.00 ml) were prepared In collection vials and analyzed under the conditions of the analysis. An average of 37 determinations showed that 29* of the VC partitioned lute the headspace. This was demonstrated by direct comparison to the standard gas (1 ppm In N,) which contained 2.6 ng VC/ml. Equation (1) was used for calculation of the partition coefficient. Standard deviation of all determinations was 0.075. Spiking and recovery studies at levels of 7 to 26 ppb VC in DKAC and lot PVC polyner solutions in PHAC were carried out for the entire procedure. The average recovery for 6 analyses of DMAC containing no PVC was S3 *. The average recovery for 21 polymer solutions was 93?. The PVC for the recovery studies was free of residual VC. (iiote: PVC containing no VC was obtained by several precipitations from BFG22220 22639013 tetrahydrofuran (TiiF) Into . .wthanul. n.oul 50 y of PVC fror. tubing cr film was -HssolvvJ In a ..iuluar amount of THF. TMs solution was slowly poured 1 ito a vigorously stirred beaker containing ethanol. The ratio of the TI'F solution to ethanol was about I K. Tie pre cipitated PVC was filtered onto a large Buchner funnel anJ air dried. For processing larger quantities of PVC. a Urge size blender was used for the precipitation. Generally two to three precipitations provided clean PVC if the starting PVC contained no ore than about 1 ppm VC.) A variety of PVC materials were analyzed using the -.'fethod described and are tabulated In Table 1. A typical FIT1 chromatogram Is shown In Fig 2 along with the chromatugran* of the reagent blank. Thirteen sables were analyzed Uui found to contain VC at levels ranging from 0.3 to 912 ppb In these PVC formulations. ;-ss spectrometry was the confirmation step In the method. It proved Invaluable In the uevelopiaent of the method by Identifying components eluting near the retention tine 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 CCA'S scans (: f i 16-200) of U* of the samples chromatographed on Porapak a were obtaineJ to Identify the components eluting near vinyl chloride. Figure ' Is the total Ion current profile of a typical sample recorded fron. the elution of carbon dioxide until the elution of ethanol. The reagent blank, and the sables were found to contain carbonyl sulfi Is, propenc, water and acetaldehyde. Chlorousthane Isobutanc and butene were identified in frost of the samples. The retention ttn,es of the corponeHts Identified In each of the saroples relative to vinyl chloride are listed In Table 2. Identification of all co.vuM>nts was based on spectral interpretation and comparison with reference cc pounds analyzed under the Identical CC/MS conditions. The sample represented by Fly 4 contained 2 ppb VC. At this level, a VC response was not evident in the total Ion current profile but was readily apparent In Fig ; which Is the selected ion current profile of this Ssmpl:. BFG22221 -lj- Stfkttsi-J io recording of Qi and (< was used to confirm the presence of VC. Tie characteristic 3:1 ratio of these Ions at the retention tl.^e of VC produced ty tr.e natural abundance of 35 Cl and ' Cl In the molecular Ion of \'C Increased the specificity of the ye time'. This ratio was reproducible to within 2t of the theoretical value when the level of resloual monooor In the poly mr was 1 ppb. cnftorlnj this n/i CZ and U ratio Insured that only compounds containlnj one chlorine atoi.i anJ thus the ele-.ental composition of vinyl chloride as a '.-olecular ion or fragment are possible Interferences to the mass spectrometry confirmation. Chlcrobutenes. eplchlorohydrln and dlchloroethant: are low molecular weight compounds that produce a frovj. ?nt at t/t 52 containing one chlorine atom and are. potential Interferences to the <>ass spectro:netry conf inr.atlon. Analysis of samples of eplchlorohydrln and dir.Moroethane datonstrated that they elute after VC. The chlorobutenes being heavier than butene would also .rlute later than VC (Id). Tfie lack of cu-e1ut1n<; materials that would have Interfenred with the FID results made It unnecessary to quantitate the samples by :<C/i'S. Cood quantitation by CC/,*S requires strict control of the analytical conditions and the construction of an analytical curve from standards analyzed simultaneously with the studies. Such an effort was considered redundant in this case. BFG22222 2639015 '>.f<;rer.ces (>) (?) (3) (-) (S) (') (7) () (9) (10) (11) (12) '''tiltool, C., 4 tffersine, . (1974) Fnyiron. Pas. 7, 357-405 Thorns, L.5., Popper, Perk, P.">., 5ol1koff, 1., ! Falk, . (1975) >v-w frig. 3. **4.. 292(1), 17-22 li racer, C.V., Oennison, 3.1., t Srown, M.f, (1975) JAOAC V3, 1214-l?i''> Piien, .'vrina, Pareles, S.?.., Clacln, J.P., t Gilbert, 5.C. {1975) JAOAC ,3. 700-70? Van Lierop, i. Stei., W. (1976) J. Chroa. 125, 123-137 L-lachenko, (.?., Cre-Jer, ".V., Croen, H.F. A Dennison, J.l. (1977) JAOAC AC. J70-575 Stolcheu, :..I. (1C7C-) Aral. Chen. , 13St-140! Sellar, T.A., Licfctenberg, J.J. (1974) JAWWA ?t<.. 739-744 A<<al. -..rethod attached to t cc. 19, 1970 letter fron Sun1tO:> Bakellte Coiapany, Lti., 340 Park Avenue, "ew York, kY 10022, to Hearing Clerk, FOA. Oi-GC fisher lane, *ock*111e, .'?> ?C052 Viola, P.l. (1970) 7*mth I<tt. Cancer tJonf., Houston, TX, Session 55, p. 742 (Abstract ;-y) Viola, P.L., iil^otti, A., - Caputo, A. (1571) Cancer ses. 31, 5U-522 The Packed ColuuM in ^as Ohroisatography (1974) Supine. W.A., SupeUo. Inc., vellefonte, PA BFG22223 Table 1. PVC Sai.iple Sjr.ruary Sample ic. 1 2 7 i 9 1C 11 1? n 14 Smple description Rigid calendared food grade sheet Thin plasticized food film Thin plasticized food film Plasticized blood bag T<)1n plasticized copolymer food film Thin plasticized food flln Plasticized food and Ilk tubing Plasticized beverage tubing Rigid vegetable oil bottle Rigid French water bottle French bottle avoiding compound Thick plasticized canning sheet Plasticized blood bag eagent blank VC found* (ppb) 1.2 2.5 2.1 1.2 2.1 0.6* 0.7fc 0.7* 120 913 0.6* 0.4* 0.3* NDC Quantitated ;>y tangent skimping VC peak and measuring peak height Estimated value - below > ethod's quantitation Unit '* chone detected f BFG22224 & CO CD o >1 Table 2. - R etention tim e o f Id e n tifie d components r e la tiv e to VC 0 touem: auaip -nna-E* l auaVH! -2-sp aue^ng coe apXq -dpin^ov NOiN i-i-O XCMCMr~-0r-00 CM f-- CM CM CM CMCMCMr--CMCJJCMCM ............................................................... < r( S aua^ng O CM I-- <-- CM 0000X0000 CMCMCMCM-- CVJCMCMCM aue^nqosj o Uo1 o rO*. aPMLM3 oo oo oo oo OO OO OO OO (I <"o8o 8 oo l*uu -WM rr-^C|SVJ|^NrN^(O\JNOCf^VhJlrt^CNNNiNfOSO^lNO ro-. or^. ausMtaui -oao 143 r0si>pcxninorovcNvNi0i)o0s4*' o im auedojd auadojd act ouiui OU)U)tf) rlO- CtOM CVM UCM* fUO> CM O IT) ^ apUins N^NvON^M'N^dCfOO VAiL^upqjeo apixo*p -uoqjso ro d * * diuai limOninumi vniAui3nut>oconj uu>)mu)ivnr>uvo)uu>) com o o 0> (Csi/IL v-- CM at at X) <o i P-CNifO^ vovovotsco cm m co 2 ml Blank (sp ike d ) 155 .49 2 ml Blank (tu b e 2 155 2 ml Blank (spiked) D lc h lo ro e th a n e 1 ,3 -B u ta d ie n e 10lijuglh tBeurtane c ls -2 -B u te n e Acetaldehyde CM 0d0 s S CSJ oo tVoO ttoo eCM rVOCI4*DJ* iI--f) 'U rCO- 45<-o dM- .10 - elutes ow^-- i^vn> it^oo ^ocm1iv--ooiv0o--o BFG22225 ?0 <r> co *D D QO ,r1`iy> Caption** FI9. 1 - Cap Patalls FIs. 2 - Tb Fin. 3 - fa* Oro*witioraMi tf 1.0 1 tttaritpac* Fig. 4 - Total Icn cotrr^ni orofll* *f tM>U #3 coot*taint *.1 ppfe VC Fit. * - Solectao Ion rocortfliw profiles of m/t i? ittf M pf saapta #'J costal Pirn; ?.1 pvt VC BFG22226 ?0 N> & <0 o hCD Inside bored to 1/4" Fig. #1 - CAP DETAILS A. 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 soldering In a bulk head fitting with the sparge tube attached. The sparge tube is attached to the bulkhead fitting by drilling a hole slightly larger than 1/16 inch downward at an angle Into the bore of the filling (See diagram). The flats of the nut portion and the upper major part of the threads should be avoided. After Insertion of the sparge tube to the proper length (enough to reach the bottom of the bottle), the tube Is silver soldered in place. A thick teflon or polyethylene gasket is then cut to fit the inside of the cap. The threads on standard metal caps are not sturdy enough for continual use and often strip off after a short time. Plastic caps were found to be unsatisfactory for even temporary usage. B. A more permanent cap for continual use has been designed. Machined from solid brass, the sparging cap consists of a hex-shaped cap (1 1/4 inch flats) threaded to the same configuration as the bottle and drilled and tapped in the top to accommodate a Swage!ok 1/4 inch bulkhead fitting. J BFG22227 226390' A second c o lle c tio n v ia l is required since as much as 10% o f the VC may pass through the f i r s t v ia l. At le ve ls above 100 ppb a th ir d v ia l is recommended. 50 CO -O c 0I/9I o cr o en --1 ~-j mro oo -- o-a* o3 =n>r O-tt TUI <-* o --1 O -h --* --* **00 o3 -* -* O O3* 3 3 Oo 3* 3 3* I/* O0 (09.0f1t o C-* -0 0 3 r-t9> (--3O 0--I/I' (t M cc 73 M<-t 3 00 <0 3 0 rt c cr <o co (i) o N h* BFG22228 BFG22229 is s to to -1 BFG22230 s fa o w cu BFG22231 o 5 Page 18 October 17, 1977 FOOD CHEMICAL NEWS FDA has been compiling data on sodium Intake through its marketbasket studies, Vanderveen said, forecasting an assessment of salt intake. He predicted it will show that most people are consuming an adequate amount of salt, but that some consumers with unusual eating patterns may consume more than 20 grams a day. If so, Vanderveen continued, there may be a "great debate" on whether FDA should take any action. Noting that FDA's enrichment-restoration-fortification regulations are on the "verge" of being finalized, Vanderveen said fortification "will become more and more impor tant." The new regulations, which he said spell out fortification practices, will take a balanced nutrient approach. Such an across-the-board policy is needed rather than consideration of fortification on an item-by-ltem basis, he said. The FDA-er predicted that new foods "will receive the brunt" of FDA's regulatory effort in the future, because it is an area in which "we can make changes." Amendment of Law Placed Emphasis on Nutrient Toxicity. FDA-er Savs A "big concern" of FDA will be nutrient toxicitles, Vanderveen said, explaining that the amendment to FDA's law sponsored by Sen. Proxmire (D-Wls.), which limited FDA's authority to regulate vitamins and minerals, puts pressure on the agency to regulate on the basis of toxicity rather than need. The protein quality standard is a "matter of concern," Vanderveen said, noting that FDA recognizes the weaknesses in use of the Protein Efficiency Ratio but has found no good alternative. He said the agency is also Interested in quality assessment of other nutrients. The FDA-er indicated that his agency is seeking new terms to use in place of the term "fiber," using this as an example of definition problems in nutrition. FDA's efforts in the field of nutrition were summarized by Vanderveen as dealing with: nutritional needs, especially regarding disease; application of dietary management of diseases; nutritional Interactions between nutrients and other substances, such as food additives; nutritional toxicitles; bloavailability; and nutritional information and how to communicate it. University of Florida's Dr. Howard Appledorf, who presented nutrient data on various "fast foods," attacked Assistant Agriculture Secretary Carol Tucker Foreman for stating that "fast foods are junk foods." He predicted a USDA "blitz" against fast foods, but predicted that fast foods will prevail. He stressed the possibilities of fast food items being used in school lunch programs to assure that students eat the food and receive the nutrition, and to reduce waste. SZ06S9Z FDA PREFERS REGULATING ONLY WATER USED AS A FOOD INGREDIENT The Food and Drug Administration would prefer regulating water only as it is used as an ingredient in commercial food products, Food and Drugs Commissioner Dr. Donald Kennedy told the Environmental Protection Agency recently (See FOOD CHEMICAL NEWS, Sept. 5, Page 33). BFG22232 October 17, 1977 Page 19 FOOD CHEMICAL NEWS In an Oct. 4 letter to EPA Administrator Douglas M. Costle, the Commissioner said discussions between FDA and EPA seem to lead to a choice between two options: -- "FDA's role in regulating water could be limited to water used as an ingredient in com mercial food products (e.g. in bread, canned punch, bottled water). EPA would assume plenary responsibility for safety of tap water provided by public water systems. This option would generally result in our agencies having mutually exclusive areas of respon sibility with respect to water. -- "FDA could assume an active role in regulating water provided by public water systems in addition to water used in commercial food products. This option might require FDA to promulgate food additive regulations for water treatment chemicals and would probably result in FDA establishment of poisonous or deleterious substance tolerance regulations for unavoidable contaminants in drinking water provided by public water systems. This option would probably result in substantial overlap of our agencies' programs for regula tion of water." On balance, the first option appears to FDA to be the preferable choice, Kennedy said, explaining that FDA believes Congress intended EPA to have full authority over public water systems when it passed the Safe Drinking Water Act. In recognition of the Congressional intent, he continued, FDA would defer to EPA to regulate drinking water, and would not regard water meeting FPA, State and local standards as "actionable" when used as a food ingredient, poin.ng out that FDA has deferred in the past to the drinking water program of the Public Health Service. Concerns with this approach are, the Commissioner observed: "(1) It is uncertain whether EPA has sufficient statutory authority to bring about adequate control; and (2) there may be a lack of resources to undertake all the evaluations that apparently would be required." Kennedy said he believed the new Toxic Substances Control Act (TSCA) would probably give EPA the necessary authority to "pre-clear" the application of new chemicals to production of water, but he added there would still be doubt as to the extent of EPA's authority to require submissions for evaluating substances that have been in use for some time. The Commissioner said he recognized that control of a new substance under TSCA may present some difficulties because of the need first to issue a regulation requiring that the substance be tested. To regulate substances already in use, he continued, "EPA would need to conduct an inventory and Itself undertake the burden of testing, which leads to resource questions." He pointed out, however, that a need for additional resources to carry out an effective program of safety assurance for water treatment substances is a common problem under either option and probably should not be the primary factor in reaching a decision. He acknowledged that the second option offers greater ability under the Food, L and Cosmetic Act to exercise control over substances used in public water supplies, but he noted that FDA could only use the 406 approach for unavoidable contaminants. BFG22233 Page 20 October 17, 1977 FOOD CHEMICAL NEWS "This approach would also carry with it a commitment to undertake a comprehensive review program in order to establish permanent tolerances for water treatment sub stances," he wrote. Kennedy said the second option appears to prevent "a substantial prospect of waste ful duplication of effort by our agencies and of confusion arising out of overlapping regulation by two government agencies." If the first option is adopted, the Commissioner said steps would be needed to co ordinate responsibilities in an effort to avoid regulatory gaps, pointing out, for example, food and food additives are exempt from TSCA. In cases of uncertainty as to which agency has responsibility, Kennedy advocated joint action, saying, however, it would be preferable to work under the Safe Drinking Water Act. He added that a review of authority under this act would be helpful in determining a strategy that would minimize the workload of this option and increase the likeli hood of its success. Meanwhile, Resources for the Future announced that it had begun planning a Safe Drinking Water Conference for Feb. 15-17 in Washington as proposed by Foremost Foods (See FOOD CHEMICAL NEWS, Aug. 8, Page 53; and Aug. 22, Page 2). FDA TO PUBLISH TETRACYCLINE PROPOSAL OCT. 18 The Food and Drug Administration will publish its proposal to ban some feed uses of tetracyclines in the Oct. 18 Federal Register, the agency informed Congressional Committees in an Oct. 3 letter. The House Appropriations Committee had directed FDA to inform interested groups on Capitol Hill at least 15 days in advance of proposals to ban uses of low-level antibiotics in feed (See FOOD CHEMICAL NEWS, Sept. 19, Page 7). In his letters to Appropriations subcommittee chairman Whitten (D-Miss.) and other members of Congress, FDA Commissioner Donald Kennedy also revealed that a proposal on "distribution controls" for antibiotics "will be published shortly after the tetracycline proposal." The Commissioner previewed the tetracycline proposal, as follows: " ... The subtherapeutic uses of tetracyclines intended to be eliminated are those uses for which there are effec tive alternative drugs. Nontherapeutlc uses of tetracy clines for which there are no alternative drugs available will be retained for use by the livestock industry. "Examples of effective alternative drugs available for the uses of penicillin and the tetracyclines Include bacitracin (zinc and methylene disalicylate), erythromycin. eo o BFG22234 ilPGoodrich INTER-ORGANIZATION CORRESPONDENCE TO FROM SUBJECT CPSC Members Marie Schmiederer FIELD POINT OR DEPT. & BLDG. NO. FIELD POINT OR DEPT. & BLDG. NO. D/5428 DATE YOUR LETTER DATE THIS liTTER 10/28/77____ Consumer Product Safety Committee Monday, October 31, 1977 1:00 p.m., Lower Level A Conference Rm. 1. Virginia Toxic Substances Act 2. Michigan Critical Materials List 3. Canadian Brith Defects Study 4. SP1 Board Meeting (OSHA Cancer Policy, Fire Safety Policy, Acrylo bottles) 5. Combustibility -- BFG Efforts Marie Schmiederer Marie Schmiederer Robert B. Downey Jean F. Malone CPSC members Villiam C. Becker discussion leader cc: W. C. Becker C. Blackfan R. B. Downey N. G. Duke D. L. Kent F. E. Krause J. F. Malone J. F. Morrill R. D. Savage R. L. Steller G. Alberts QFG-4956*D 2/77 LITHO JSA BFG22235 N) S o