ASTM D5507-21a

Standard Test Method for Determination of Trace Organic Impurities in Monomer Grade Vinyl Chloride by Capillary Column/Multidimensional Gas Chromatography

SIGNIFICANCE AND USE
5.1 The multidimensional approach permits all of the trace impurities to be well separated from the main vinyl chloride peak, thereby improving quantitative accuracy over established packed column methods.  
5.2 The minimum detection limit (MDL) for all components of interest has been shown to be well below 500 ppb for this test method.
SCOPE
1.1 This is a general-purpose capillary-based test method for the determination of trace level impurities in high-purity vinyl chloride. This test method uses serially coupled capillary PLOT columns in conjunction with the multidimensional techniques of column switching and cryogenic trapping to permit the complete separation of the 11 key vinyl chloride impurities in a single 25-min run.  
Note 1: There is no known ISO equivalent to this standard.  
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 8.  
1.3 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 30-Apr-2021
• ICS: 83.080.20 - Thermoplastic materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

Relations

• Refers: ASTM F307-13(2020) - Standard Practice for Sampling Pressurized Gas for Gas Analysis
• Effective Date: 01-Apr-2020

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D5507 − 21a
Standard Test Method for
Determination of Trace Organic Impurities in Monomer
Grade Vinyl Chloride by Capillary Column/Multidimensional
1
Gas Chromatography
This standard is issued under the fixed designation D5507; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* 3. Terminology
1.1 This is a general-purpose capillary-based test method 3.1 Definitions—For definitions of terms in this test method
for the determination of trace level impurities in high-purity relating to plastics, refer to Terminology D883. For abbrevia-
vinyl chloride. This test method uses serially coupled capillary tions used in this test method, refer toTerminology D1600. For
PLOT columns in conjunction with the multidimensional definitions of terms that appear in this test method relating to
techniques of column switching and cryogenic trapping to quality and statistics, refer to Terminology E456.
permit the complete separation of the 11 key vinyl chloride
4. Summary of Test Method
impurities in a single 25-min run.
4.1 The liquid vinyl chloride sample or calibration standard
NOTE 1—There is no known ISO equivalent to this standard.
is injected either directly using a high-pressure liquid sampling
1.2 This standard does not purport to address all of the
valveoralternatelyasanexpandedgas.Anappropriatevolume
safety concerns, if any, associated with its use. It is the
of the liquid or gas sample is injected to enable the required
responsibility of the user of this standard to establish appro-
detection limits to be achieved.Apreliminary GC separation is
priate safety, health, and environmental practices and deter-
achieved on a 6-m pre-column, the purpose of which is to
mine the applicability of regulatory limitations prior to use.
removethebulkofthevinylchloridepeakfromthetracepeaks
Specific hazards statements are given in Section 8.
of interest. Two heart-cut transfers are made from this pre-
1.3 This international standard was developed in accor-
column separation, which sends selected portions to a second
dance with internationally recognized principles on standard-
column for additional separation. These two cuts incorporate
ization established in the Decision on Principles for the
10 of the 11 trace impurities of interest, but they exclude 1,2
Development of International Standards, Guides and Recom-
ethylenedichlorideandthebulkofthevinylchloridepeak.The
mendations issued by the World Trade Organization Technical
1,2 EDC peak is eluted from the 6-m pre-column and detected
Barriers to Trade (TBT) Committee.
at the first FID after the two cuts are made.
2. Referenced Documents
4.2 The components eluting to the two FID detectors are
2
identified and quantitated by comparing their retention times
2.1 ASTM Standards:
and area counts to those obtained previously from a calibration
D883 Terminology Relating to Plastics
standard run under identical conditions.
D1600 Terminology forAbbreviatedTerms Relating to Plas-
tics
5. Significance and Use
E456 Terminology Relating to Quality and Statistics
E2935 Practice for Conducting Equivalence Tests for Com- 5.1 The multidimensional approach permits all of the trace
paring Testing Processes
impurities to be well separated from the main vinyl chloride
F307 Practice for Sampling Pressurized Gas for Gas Analy-
peak,therebyimprovingquantitativeaccuracyoverestablished
sis packed column methods.
5.2 Theminimumdetectionlimit(MDL)forallcomponents
1
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
of interest has been shown to be well below 500 ppb for this
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
test method.
Current edition approved May 1, 2021. Published May 2021. Originally
approved in 1994. Last previous edition approved in 2021 as D5507 – 21. DOI:
6. Apparatus
10.1520/D5507-21A.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.1 Instrumentation:
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
6.1.1 Capillary Column/Multidirectional Gas
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Chromatograph, equipped as follows:
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5507 − 21 D5507 − 21a
Standard Test Method for
Determination of Trace Organic Impurities in Monomer
Grade Vinyl Chloride by Capillary Column/Multidimensional
1
Gas Chromatography
This standard is issued under the fixed designation D5507; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope*
1.1 This is a general-purpose capillary-based test method for the determination of trace level impurities in high-purity vinyl
chloride. This test method uses serially coupled capillary PLOT columns in conjunction with the multidimensional techniques of
column switching and cryogenic trapping to permit the complete separation of the 11 key vinyl chloride impurities in a single
25-min run.
NOTE 1—There is no known ISO equivalent to this standard.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of
regulatory limitations prior to use. Specific hazards statements are given in Section 8.
1.3 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D1600 Terminology for Abbreviated Terms Relating to Plastics
E456 Terminology Relating to Quality and Statistics
E2935 Practice for Conducting Equivalence Tests for Comparing Testing Processes
F307 Practice for Sampling Pressurized Gas for Gas Analysis
3. Terminology
3.1 Definitions—Terminology is in accordance with Terminologies For definitions of terms in this test method relating to plastics,
refer to Terminology D883 and . For abbreviations used in this test method, refer to Terminology D1600 unless otherwise
indicated. For definitions of terms that appear in this test method relating to quality and statistics, refer to Terminology E456.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved Jan. 15, 2021May 1, 2021. Published January 2021May 2021. Originally approved in 1994. Last previous edition approved in 20122021 as
D5507 – 99D5507 – 21.(2012). DOI: 10.1520/D5507-21.10.1520/D5507-21A.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D5507 − 21a
4. Summary of Test Method
4.1 The liquid vinyl chloride sample or calibration standard is injected either directly using a high-pressure liquid sampling valve
or alternately as an expanded gas. An appropriate volume of the liquid or gas sample is injected to enable the required detection
limits to be achieved. A preliminary GC separation is achieved on a 6-m pre-column, the purpose of which is to remove the bulk
of the vinyl chloride peak from the trace peaks of interest. Two heart-cut transfers are made from this pre-column separation, which
sends selected portions to a second column for additional separation. These two cuts incorporate 10 of the 11 trace impurities of
interest, but they exclude 1,2 ethylene dichloride and the bulk of the vinyl chloride peak. The 1,2 EDC peak is eluted from the
6-m pre-column and detected at the first FID after the two cuts are made.
4.2 The components eluting to the two FID detectors are identified and quantitated by comparing their retention times and area
counts to those obtained previously from a calibration standard run under identical conditions.
5. Significance and Use
5.1 The multidimensional approach permits all of the trace impurities to be well separated from the main vinyl chloride peak,
...