ASTM_D_5507_-_99_2012.pdf

Designation:D550799(Reapproved 2012)Standard Test Method forDetermination of Trace Organic Impurities in MonomerGrade Vinyl Chloride by Capillary Column/MultidimensionalGas Chromatography1This standard is issued under the fixed designation D5507;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.Scope1.1 This is a general-purpose capillary-based test methodfor the determination of trace level impurities in high-purityvinyl chloride.This test method uses serially coupled capillaryPLOT columns in conjunction with the multidimensionaltechniques of column switching and cryogenic trapping topermit the complete separation of the 11 key vinyl chlorideimpurities in a single 25-min run.NOTE1There is no known ISO equivalent to this standard.1.2 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 hazardsstatements are given in Section 8.2.Referenced Documents2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD1600 Terminology forAbbreviated Terms Relating to Plas-ticsF307 Practice for Sampling Pressurized Gas for Gas Analy-sis3.Terminology3.1 DefinitionsTerminology is in accordance with Termi-nologies D883 and D1600 unless otherwise indicated.4.Summary of Test Method4.1 The liquid vinyl chloride sample or calibration standardis injected either directly using a high-pressure liquid samplingvalve or alternately as an expanded gas.An appropriate volumeof the liquid or gas sample is injected to enable the requireddetection limits to be achieved.Apreliminary GC separation isachieved on a 6-m pre-column,the purpose of which is toremove the bulk of the vinyl chloride peak from the trace peaksof interest.Two heart-cut transfers are made from this pre-column separation,which sends selected portions to a secondcolumn for additional separation.These two cuts incorporate10 of the 11 trace impurities of interest,but they exclude 1,2ethylene dichloride and the bulk of the vinyl chloride peak.The1,2 EDC peak is eluted from the 6-m pre-column and detectedat the first FID after the two cuts are made.4.2 The components eluting to the two FID detectors areidentified and quantitated by comparing their retention timesand area counts to those obtained previously from a calibrationstandard run under identical conditions.5.Significance and Use5.1 The multidimensional approach permits all of the traceimpurities to be well separated from the main vinyl chloridepeak,thereby improving quantitative accuracy over establishedpacked column methods.5.2 The minimum detection limit(MDL)for all componentsof interest has been shown to be well below 500 ppb for thistest method.6.Apparatus6.1 Instrumentation:6.1.1 HP 5890A3,4(or equivalent),equipped as follows:6.1.1.1 Split/Splitless Injector SystemMust be demon-strated to be free of discrimination effects induced by vaporviscosity differences if helium-or nitrogen-based gas standardsare to be used for instrument calibration.6.1.1.2 Dual Flame-Ionization Detectors.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 Oct.10,2012.Published November 2012.Originallyapproved in 1994.Last previous edition approved in 2008 as D5507-99(2008)1.DOI:10.1520/D5507-99R12.2For 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 sole source of supply of the apparatus known to the committee at this timeis Hewlett-Packard Co.,3495 Deer Creek Road,Palo Alto,California 94304.4If you are aware of alternative suppliers,please provide this information toASTM International Headquarters.Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.*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 6.1.1.3 Column Switching Device A pneumatics controlsystem,available from Scientific Glass Engineering,Inc.,4,5orequivalent.6.1.1.4 Sub-Ambient Oven Temperature Control(optional).6.1.1.5 LPG Vaporizing Injector,available from Microana-lytics Instrumentation,4,6or equivalent(Fig.1).6.2 Data SystemDual HP 3396A Integrators3,4(or equiva-lent)permit the acquisition,storage,and reduction of theoutput signals from the two FIDs simultaneously.After theinitial method development,howe