1、Designation: D 5507 99Standard Test Method forDetermination of Trace Organic Impurities in MonomerGrade Vinyl Chloride by Capillary Column/MultidimensionalGas Chromatography1This standard is issued under the fixed designation D 5507; the number immediately following the designation indicates the yea
2、r 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.1. Scope1.1 This is a general-purpose capillary-based test methodf
3、or 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 chlorideimpurit
4、ies in a single 25-min run.NOTE 1There are no similar or equivalent ISO standards covering theprimary subject of this test method.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 establis
5、h 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:D 883 Terminology Relating to Plastics2D 1600 Terminology for Abbreviated Terms Relating toP
6、lastics2F 307 Practice for Sampling Pressurized Gas for GasAnaly-sis33. Terminology3.1 DefinitionsTerminology is in accordance with Termi-nologies D 883 and D 1600 unless otherwise indicated.4. Summary of Test Method4.1 The liquid vinyl chloride sample or calibration standardis injected either direc
7、tly 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. A preliminary GC separation isachieved on a 6-m pre-column, the purpose of which is toremove the bulk o
8、f 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 di
9、chloride 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 ob
10、tained 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
11、.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 5890A4(or equivalent), equipped as follows:6.1.1.1 Split/Splitless Injector SystemMust be demon-strated to be free of discriminati
12、on 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.6.1.1.3 Column Switching Device A pneumatics controlsystem, available from Scientific Glass Engineering, Inc.,5orequivalent.1Th
13、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 July 10, 1999. Published October 1999. Originallypublished as D 5507 94. Last previous edition D 5507 94.2Annual Book of AS
14、TM Standards, Vol 08.01.3Annual Book of ASTM Standards, Vol 15.03.4Available from Hewlett-Packard Co., 3495 Deer Creek Road, Palo Alto,California 94304.5Scientific Glass Engineering 2007 Kramer Lane, Austin, Texas 78758.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshoho
15、cken, PA 19428-2959, United States.6.1.1.4 Sub-Ambient Oven Temperature Control (optional).6.1.1.5 LPG Vaporizing Injector, available from Microana-lytics Instrumentation,6or equivalent (Fig. 1).6.2 Data SystemDual HP 3396A Integrators4(or equiva-lent) permit the acquisition, storage, and reduction
16、of theoutput signals from the two FIDs simultaneously. After theinitial method development, however, it is possible to consoli-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 restr
17、ictor coupled to the front ofa6mby0.53-mm inside diameter GSQTMavailable from J VCM impurities;vinyl chloride monomerTABLE 1 Single Laboratory and Single Operator Repeatability for Four Key Impurities Using Procedure B Vapor InjectionImpurityRetention Time (Short-Term)(1 day6 Sequential Runs)Quantit
18、ative (Short Term)(1 day6 Sequential Runs)Quantitative (Long Term)(9 day10 Sequential Runs)Mean,minSrArBMean,ppmSrrMean,ppmSrrMethyl 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 0.0
19、85 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 = 2.83 3 Sr.ASTM 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 expr
20、essly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, 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 revise
21、d, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may
22、attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM 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).D5507995
