ASTM_D_4443_-_13.pdf

Designation:D444313Standard Test Method forDetermining Residual Vinyl Chloride Monomer Content inPPB Range in Vinyl Chloride Homo-and Co-Polymers byHeadspace Gas Chromatography1This standard is issued under the fixed designation D4443;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope*1.1 This test method is suitable for determining the residualvinyl chloride monomer(RVM)content of homopolymer andcopolymers of vinyl chloride down to a level of;5 ppb.1.2 This test method is applicable to any polymer form,suchas resin,compound,film,bottle wall,etc.that can be dissolvedin a suitable solvent.1.3 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.Specific hazardstatements are given in Section 9 and Note 10.NOTE1This standard is equivalent to ISO 6401.2.Referenced Documents2.1 ISO Standard:ISO 6401 PlasticsHomopolymer and Copolymer Resinsof Vinyl ChlorideDetermination of Residual VinylChloride MonomerGas Chromatographic Method22.2 OSHA Standard:29 CFR 1919.1017 Vinyl Chloride33.Terminology3.1 Abbreviations:3.1.1 DMAcN,N-dimethylacetamide.3.1.2 VCMVinyl chloride monomer.4.Summary of Test Method4.1 Samples of vinyl chloride-containing polymers are dis-solved in a suitable solvent in a closed system.4.2 The polymer solution and headspace are equilibrated atan elevated temperature.4.3 Aliquots of headspace gas are injected into a gaschromatograph and the vinyl chloride monomer is separated.The response of vinyl chloride monomer is determined by theuse of one of several suggested detectors.4.4 Calibration is accomplished using either(a)vinyl chlo-ride monomer in nitrogen gas standards,(b)standard solutionscontaining known amounts of vinyl chloride monomer,or(c)amethod of standard addition.5.Significance and Use5.1 Vinyl chloride-containing polymers are widely used topackage a variety of materials,including foods.5.2 Vinyl chloride monomer has been shown to be a humancarcinogen.Threshold toxicity value has not been established.5.3 Plastic manufacturers,food packagers,governmentagencies,etc.have a need to know the residual vinyl chloridemonomer content of vinyl chloride-containing polymers.6.Interferences6.1 N,N-dimethylacetamide should be analyzed under iden-tical conditions to determine the absence of interferences at thevinyl chloride monomer gas chromatography(GC)retentiontime.6.2 Other solvents,monomers,or compounding aids maycause interference at the vinyl chloride monomer GC retentiontime.7.Apparatus7.1 Gas Chromatography,equipped with either a flameionization detector(FID),a photo ionization detector(PID),ora Hall electroconductivity detector(HED),backflushing valve,and either automatic capability or manual sampling(Note 2)and ability to analyze the headspace vapors contained in asealed vial.NOTE2If the analyses are to be performed manually(that is,bysyringe injection),then the following equipment will also be needed:(1)Constant-temperature bath or oven capable of maintaining a1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.70 on Analytical Methods.Current edition approved Nov.1,2013.Published November 2013.Originallyapproved in 1984.Last previous edition approved in 2012 as D4443 12.DOI:10.1520/D4443-13.2Available from American National Standards Institute(ANSI),25 W.43rd St.,4th Floor,New York,NY 10036,http:/www.ansi.org.3Available from Superintendent of Documents,US Government Printing Office,Washington,DC 20402.*A Summary of Changes section appears at the end of this standardCopyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 temperature of 90 6 1C.(2)Gas-tight GC syringes for sampling and injection.(3)Sample bottles with fluoropolymer faces septa and caps(sizeoptional).(4)Gloves for handling hot syringes.7.2 Chromatographic Column,3%OV-101 on 80/100mesh Chromosorb WHP,18-in.(3.2-mm)outside diameter by2 ft(0.6 m),stainless steel connected through18-in.“tee”to0.19%picric acid on 80/100 mesh Carbopack C,18-in.outsidediameter by 8 ft(2.4 m),stainless steel.NOTE3Any column packing that will resolve VCM from interfer-ences and elute VCM in a reasonable length of time(1 to 5 min)issatisfactory.For example,a 3-ft(0.9-m)by18-in.(3.2-mm)outsidediameter column containing 0.19%picric acid on 80/100 mesh Car-bopack C can replace the recommended 3%OV 101 column.Settingsrecommended in 11.3.1 may have to be modified to suit the packingmaterial being used.7.3 Detector Output Filter/AmplifierThe extreme sensitiv-ity of