ASTM_D_3680_-_89_1996e1.pdf

Designation:D 3680 89(Reapproved 1996)e1An American National StandardStandard Test Method forResidual Vinyl Chloride Monomer Content of Poly(VinylChloride)Resins,Compounds,and Copolymers by SolutionInjection Technique1This standard is issued under the fixed designation D 3680;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(e)indicates an editorial change since the last revision or reapproval.e1NOTEEditorial changes were made throughout in November 1996.1.Scope1.1 This test method can be used to determine smallamounts of residual vinyl chloride monomer(VCM)in poly-(vinyl chloride)(PVC)resins.It may be possible to use it forother resins or compounds containing vinyl chloride providedthere are no other volatile components present with the sameretention time as vinyl chloride monomer.1.2 The values stated in inch-pound units are to be regardedas the standard.The values given in parentheses are forinformation only.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.For a specifichazard statement,see Section 9.2.Referenced Documents2.1 ASTM Standards:E 260 Practice for Packed Column Gas Chromatography2E 355 Practice for Gas Chromatography Terms and Rela-tionships23.Terminology3.1 Abbreviations:3.1.1 VCMvinyl chloride monomer.3.1.2 PVCpoly(vinyl chloride)resin.3.1.3 RVCMresidual vinyl chloride monomer.3.1.4 DMACdimethyl acetamide.3.1.5 THFtetrahydrofuran.4.Summary of Test Method4.1 The resin,compound,or copolymer specimen is dis-solved in a suitable solvent and is then analyzed by conven-tional gas chromatographic(GC)techniques.Analysis time canbe decreased by utilizing a backflush mode to eliminate thesolvent.5.Significance and Use5.1 Poly(vinyl chloride)(PVC)resins must contain a mini-mum possible amount of unreacted,or free vinyl chloridemonomer.5.2 Under optimum conditions approximately 1 ppm VCMcan be detected in PVC resins.6.Interferences6.1 Any material that elutes at approximately the sameretention time as VCM will cause erroneously high RVCMresults.6.2 Special care must be exercised in interpreting theRVCM results obtained from the analyses of PVC copolymersor compounds.Many ingredients are added to PVC resins toobtain compounds with desired properties for each particularend use.These additives,or components in them,couldpossibly have the same retention time as VCM.In general,if aPVC compound apparently has a much larger VCM contentthan the starting resin,then the presence of some interferingcomponent can be suspected as the probable cause of the largerthan expected amount in the compound.7.Apparatus7.1 Gas Chromatograph,with dual flame ionization detec-tor,and heated injection port with removable glass inserts.Forfurther information see Practice E 355.7.2 Recorder,0 to 1-mV full scale.NOTE1Electronic integrators,or computer systems can be used toobtain peak areas and make the required calculations.7.3 Analytical Balance,capable of weighing to 60.0001 g.7.4 Soap Film Flowmeter.7.5 Stopwatch.7.6 Pressure Regulators,for all the required gas cylinders.7.7 Filter Dryer Assemblies,for each of the GC gas cylin-ders.7.8 Vials,6-dram,with polyethylene-lined screw caps.1This test method is under the jurisdiction of ASTM Committee D-1 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.33 on Polymers and Resins.Current edition approved April 28,1989.Published June 1989.Originallypublished as D 3680 78.Last previous edition D 3680 78.2Annual Book of ASTM Standards,Vol 14.02.1AMERICAN SOCIETY FOR TESTING AND MATERIALS100 Barr Harbor Dr.,West Conshohocken,PA 19428Reprinted from the Annual Book of ASTM Standards.Copyright ASTMNOTE2Caps with wax liners should not be used for sample dissolu-tion.NOTE3Vials and caps should be used only once and discarded.7.9 Serum Bottles,60-mL,and Stoppers.7.10 Liquid Sampling Syringes,10 and 50-L.GC LiquidSampling Syringes,10 and 50-L.7.11 Gas Syringes,0.1 and 1-mL,equipped with valvelocks.7.12 Ball Valve,two-way,stainless steel.37.13 Flow Controller.47.14 Screw Cap,6-dram,with Needle Seal Septa.7.15 Reciprocating or Wrist-Action-Type Shaker.7.16 Column and PackingsAny of the following may beused:For further information see Practice E 260.7.16.118in.outside diameter by 1 ft plus18in.outsidediameter by 6 ft stainless steel packed with 80/100 meshcopolymerized divinyl benzene/4 vinyl pyridine porous poly-mer beads(UPS code S8);or silanized divinyl benzene porouspolymer beads.57.16.218in.outside diameter by 20 ft stainless steel packedwith 20%nonyl phenyl poly(ethylene glycol)on 60/80-meshacid washed,white flux-calcined diatomite(USP co