1、Designation: D5507 99 (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 i
2、ndicates 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-bas
3、ed 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
4、chlorideimpurities in a single 25-min run.NOTE 1There 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
5、 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
6、 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 samp
7、lingvalve or alternately as an expanded gas.An appropriate volumeof the liquid or gas sample is injected to enable the requireddetection limits to be achieved. A preliminary GC separation isachieved on a 6-m pre-column, the purpose of which is toremove the bulk of the vinyl chloride peak from the tr
8、ace 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 ch
9、loride 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 calibrations
10、tandard 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
11、) 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 vaporviscosit
12、y 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
13、 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 An
14、nual 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 sup
15、pliers, 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 Ba
16、rr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.1.1.3 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, availab
17、le 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, however, it is possible to consoli-
18、date the output to a single integrator using the instrumentssignal switching capability.6.3 Columns:6.3.1 Pre-Column100 cm of 0.20-mm inside diameterfused silica fixed restrictor coupled to the front ofa6mby0.53-mm inside diameter GSQTMavailable from J VCM impurities;vinyl chloride monomerTABLE 1 Si
19、ngle Laboratory and Single Operator Repeatability for Four Key Impurities Using Procedure B Vapor InjectionImpurityRetention Time (Short-Term)(1 day6 Sequential Runs)Quantitative (Short Term)(1 day6 Sequential Runs)Quantitative (Long Term)(9 day10 Sequential Runs)Mean,minSrArBMean,ppmSrrMean,ppmSrrM
20、ethyl chloride 11.02 0.02 0.057 29.50 0.12 0.340 34.48 0.60 1.6981,3 butadiene 17.48 0.01 0.028 2.75 0.02 0.057 3.27 0.06 0.170Vinyl acetylene 17.86 0.01 0.028 5.23 0.03 0.085 10.09 0.14 0.396Ethyl chloride 18.14 0.01 0.028 17.44 0.09 0.255 19.23 0.29 0.821ASr= standard deviation.Br =2.83Sr.D5507 99
21、 (2012)5ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rig
22、hts, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
23、 standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM
24、 Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D5507 99 (2012)6
