ASTM_D_3749_-_13.pdf

Designation:D374913Standard Test Method forResidual Vinyl Chloride Monomer in Poly(Vinyl Chloride)Resins by Gas Chromatographic Headspace Technique1This standard is issued under the fixed designation D3749;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(RVCM)content of poly(vinyl chlo-ride)(PVC)homopolymer and copolymer resins for uses otherthan food contact.The range for this test,based on interlabo-ratory evaluation,is from 0.1 to 400 ppm RVCM.1.2 This test method can be adapted to determinations ofRVCM in a PVC copolymer resin if the Henrys Law constantat 90C for that copolymer is known.1.3 This test method cannot be used for polymer in fusedforms,such as cubes or sheets.Refer to Test Method D4443 orTest Method D3680 for these materials.1.4 This test method is proposed as an alternative to EPAMethod 107 for determination of vinyl chloride monomers indry-resin samples.1.5 The values stated SI units are to be regarded as thestandard.1.6 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.NOTE1This standard and ISO 6401 address the same subject matter,but differ in technical content.2.Referenced Documents2.1 ASTM Standards:2D3680 Test Method for Residual Vinyl Chloride MonomerContent of Poly(Vinyl Chloride)Resins,Compounds,andCopolymers by Solution Injection Technique(Withdrawn2005)3D4443 Test Method for Determining Residual Vinyl Chlo-ride Monomer Content in PPB Range in Vinyl ChlorideHomo-and Co-Polymers by Headspace Gas Chromatog-raphyD4526 Practice for Determination of Volatiles in Polymersby Static Headspace Gas ChromatographyE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 Federal Standards:Environmental Protection Agency Method 107Determina-tion of Vinyl Chloride Content of In-Process Waste-WaterSamples,and Vinyl Chloride Content of Poly(Vinyl Chlo-ride)Resin,Slurry,Wet Cake,and Latex Samples429 CFR 1919.1017 Vinyl Chloride for Regulated Levels ofExposure52.3 ISO Standard:ISO 6401 Determination of Residual Vinyl Chloride Mono-mer in Homopolymers and Copolymers by Gas Chroma-tography63.Terminology3.1 Acronyms:3.1.1 VCMVinyl chloride monomer.3.1.2 RVCMResidual vinyl chloride monomer.3.1.3 PVCPoly(vinyl chloride).3.1.4 OSHAOccupational Safety and Health Agency.3.1.5 FIDFlame ionization detector.1This 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 1978.Last previous edition approved in 2012 as D3749-12.DOI:10.1520/D3749-13.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from United States Environmental Protection Agency(EPA),ArielRios Bldg.,1200 Pennsylvania Ave.,NW,Washington,DC 20460,http:/www.epa.gov.5Available from U.S.Government Printing Office Superintendent of Documents,732 N.Capitol St.,NW,Mail Stop:SDE,Washington,DC 20401,http:/www.access.gpo.gov.6Available from American National Standards Institute(ANSI),25 W.43rd St.,4th Floor,New York,NY 10036,http:/www.ansi.org.*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 3.1.6 PIDPhotoionization detector.3.1.7 HEDHall electroconductivity detector.3.1.8 MHEMultiple headspace extraction.4.Summary of Test Method4.1 The basis for this test method relates to the vaporequilibrium that is established between RVCM,PVC resin,andair in a closed system.The RVCM in a PVC resin willequilibrate in a closed vessel quite rapidly,provided that thetemperature of the PVC resin is maintained above the glasstransition temperature of that specific resin type.4.2 After sample equilibration,conventional gas chromato-graphic(GC)techniques are used.A constant amount ofsample headspace vapor is injected into a GC column that ispacked with a liquid-coated solid support or porous polymerbeads.Sample injection is accomplished by available commer-cial automatic equipment.Passing through the column in astream of carrier gas,the vinyl chloride monomer(VCM)isseparated from other components which may be pr