1、Designation:D782314Standard Test Method forDetermination of Low Level,Regulated Phthalates in Poly(Vinyl Chloride)Plastics by Thermal DesorptionGasChromatography/Mass Spectrometry1This standard is issued under the fixed designation D7823;the number immediately following the designation indicates the
2、 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 provides a procedure to identify andquan
3、tify six phthalates by thermal desorption(TD)gas chro-matography(GC)mass spectrometry(MS).The phthalates areBBP,DBP,DEHP,DNOP,DINP and DIDP.NOTE1The method can be extended to include other phthalates.1.2 Within the context of this method,“low level”is definedas 1000 ppm.1.3 The values in SI units ar
4、e to be regarded as standard.1.4 This test method includes references,notes and foot-notes that provide explanatory material.These notes andfootnotes(excluding those in the tables and figures)shall notbe considered as requirements of this method.1.5 This standard does not purport to address all of t
5、hesafety 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.NOTE2There is no known ISO equivalent to this test method.2.Referenced D
6、ocuments2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD1600 Terminology forAbbreviated Terms Relating to Plas-ticsD3465 Test Method for Purity of Monomeric Plasticizers byGas ChromatographyD7083 Practice for Determination of Monomeric Plasticiz-ers in Poly(Vinyl Chloride)(PVC)by Gas Chrom
7、atogra-phyE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE355 Practice for Gas Chromatography Terms and Relation-shipsE594 Practice for Testing Flame Ionization Detectors Usedin Gas or Supercritical Fluid ChromatographyE691 Practice for Conducting an Interlaboratory Study t
8、oDetermine the Precision of a Test MethodIEEE/ASTM SI10 Practice for Use of the InternationalSystem of Units(SI),the Modernized Metric System3.Terminology3.1 DefinitionsFor definition of plastic terms used in thistest method,see Terminologies D883 and D1600.3.2 For units,symbols,and abbreviations us
9、ed in this testmethod refer to Practices E594,E355,or SI10.3.3 Compounds and Instrumentation:3.3.1(DOA)Hexanedioic acid,1,6bis(2ethylhexyl)esterCAS#1032313.3.2(DINCH)1,2Cyclohexanedicarboxylic acid,dinonylester,branched and linear CAS#4749195903.3.3(DBP)1,2Benzenedicarboxylicacid,1,2dinbutylester CA
10、S#847423.3.4(BBP)Benzyl butyl phthalate CAS#856873.3.5(DEHP)Bis(2Ethyhexyl)Phthalate CAS#1178173.3.6(DNOP)Di(noctyl)phthalate CAS#1178403.3.7(DINP)1,2Benzenedicarboxylicacid,diC810branched alkyl esters,C9rich(Jayflex)CAS#685154803.3.8(DINP)1,2Benzenedicarboxylicacid,1,2diisononyl(Palatinol)CAS#28553
11、1203.3.9(DIDP)1,2Benzenedicarboxylicacid,diC911branched alkyl esters,C10rich(Jayflex)CAS#685154913.3.10(DIDP)1,2Benzenedicarboxylicacid,1,2diisodecylCAS#267614003.3.11 TD Thermal Desorption3.3.12 GC Gas Chromatography3.3.13 GC/MS Gas Chromatography/Mass Spectrometry3.3.14 PVC Poly(Vinyl Chloride)1Th
12、is 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 Aug.1,2014.Published September 2013.Originallyapproved in 2013.Last previous edition approved in 2013 as D7823-13.DOI:10.15
13、20/D7823-14.2For 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.*A Summary of Changes section appears at the end of th
14、is standardCopyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 3.3.15 THF GC grade or higher“Tetrahydrofuran”3.3.16 DCM GC grade or higher Methylene Chloride”3.3.17 EGAMS Evolved Gas Analysismass spectrometry3.3.18 FTIR Fourier Transform Infr
15、ared Spectroscopy3.3.19 TIC Total ion chromatogram3.3.20 DQO Data quality objectivesNOTE3DINP and DIDP,when used in various PVC formulations aretechnical mixtures.Take care,when preparing the phthalate calibrationstandard to use the technical grade.Here is specific information on DINPand DIDP.For mo
16、re information,please refer to Appendix X3.Jayflex DIDP:1,2Benzenedicarboxylicacid,diC911branched alkylesters,C10rich:CAS#68515491.Jayflex DINP:1,2Benzenedicarboxylicacid,diC810branched alkylesters,C9rich:CAS#68515 480.4.Summary of Test Method4.1 200 mg of the PVC sample are dissolved in 10 mL ofTHF.10 L of the THF solution are analyzed using TD-GC/MS.Phthalates are identified by their retention times and theirmass spectra.Quantification is based on the area of a desig-nated quant ion(SIM or ful