ASTM D4526-20

Standard Practice for Determination of Volatiles in Polymers by Static Headspace Gas Chromatography

SIGNIFICANCE AND USE
4.1 There are various reasons why one would measure the level of unreacted or residual monomer, water, or other volatile components in a polymer sample.  
4.2 Volatiles of interest are often at trace concentrations. Headspace analysis is suited for determination of these trace components which often cannot be determined by conventional gas chromatography because of sample decomposition or interferences.  
4.3 For polymer analysis, sample treatment for headspace analysis is simpler than conventional gas chromatography, where additional precipitation steps are required to prevent polymer contamination of the chromatographic column.  
4.4 This headspace practice will be able to determine qualitatively any component with sufficient vapor pressure. It is capable of yielding semiquantitative results and can be used for relative comparisons between samples.
SCOPE
1.1 Headspace gas chromatography (GC) involves the determination of volatile components in a polymer solution by gas chromatography of a vapor phase in thermal equilibrium with the sample matrix. Volatiles in finely ground insoluble polymers can also be determined with and without an extracting solvent.  
1.2 This practice provides two procedures:  
1.2.1 Procedure A—Automatic headspace analysis.  
1.2.2 Procedure B—Manual injection headspace analysis.  
1.3 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 precautionary statements are given in Section 7.  
Note 1: There is no known ISO equivalent to this standard.  
1.4 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: 14-May-2020
• ICS: 83.080.01 - Plastics in general
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

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: D4526 − 20
Standard Practice for
Determination of Volatiles in Polymers by Static Headspace
1
Gas Chromatography
This standard is issued under the fixed designation D4526; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* E355PracticeforGasChromatographyTermsandRelation-
ships
1.1 Headspace gas chromatography (GC) involves the de-
E594Practice for Testing Flame Ionization Detectors Used
termination of volatile components in a polymer solution by
in Gas or Supercritical Fluid Chromatography
gas chromatography of a vapor phase in thermal equilibrium
with the sample matrix. Volatiles in finely ground insoluble
3. Terminology
polymers can also be determined with and without an extract-
3.1 General—Theunits,symbols,andabbreviationsusedin
ing solvent.
thistestmethodareinaccordancewithTerminologyD883and
1.2 This practice provides two procedures:
Practice IEEE/ASTMSI-10.
1.2.1 Procedure A—Automatic headspace analysis.
1.2.2 Procedure B—Manual injection headspace analysis.
4. Significance and Use
1.3 This standard does not purport to address all of the
4.1 There are various reasons why one would measure the
safety concerns, if any, associated with its use. It is the
levelofunreactedorresidualmonomer,water,orothervolatile
responsibility of the user of this standard to establish appro-
components in a polymer sample.
priate safety, health, and environmental practices and deter-
4.2 Volatiles of interest are often at trace concentrations.
mine the applicability of regulatory limitations prior to use.
Specific precautionary statements are given in Section 7. Headspace analysis is suited for determination of these trace
componentswhichoftencannotbedeterminedbyconventional
NOTE 1—There is no known ISO equivalent to this standard.
gas chromatography because of sample decomposition or
1.4 This international standard was developed in accor-
interferences.
dance with internationally recognized principles on standard-
4.3 For polymer analysis, sample treatment for headspace
ization established in the Decision on Principles for the
analysis is simpler than conventional gas chromatography,
Development of International Standards, Guides and Recom-
where additional precipitation steps are required to prevent
mendations issued by the World Trade Organization Technical
polymer contamination of the chromatographic column.
Barriers to Trade (TBT) Committee.
4.4 This headspace practice will be able to determine
2. Referenced Documents
qualitatively any component with sufficient vapor pressure. It
2
2.1 ASTM Standards: is capable of yielding semiquantitative results and can be used
D883Terminology Relating to Plastics for relative comparisons between samples.
D4322Test Method for Residual Acrylonitrile Monomer
Styrene-Acrylonitrile Copolymers and Nitrile Rubber by 5. Apparatus
3
Headspace Gas Chromatography (Withdrawn 2010)
5.1 Gas Chromatograph, equipped with an appropriate
E260Practice for Packed Column Gas Chromatography
detector and backflush valve.
5.1.1 For Procedure A, an Automated Headspace Sampler,
1 including backflush capability, thermostated sample tray, and
ThispracticeisunderthejurisdictionofASTMCommitteeD20onPlasticsand
is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
associated accessories fulfill these requirements while provid-
Current edition approved May 15, 2020. Published June 2020. Originally
ing for automatic sequential sampling of headspace vapors.
approved in 1985. Last previous edition approved in 2012 as D4526-12. DOI:
5.1.2 Procedure B requires the following additional equip-
10.1520/D4526-20.
2
ment:
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
5.1.2.1 Constant-Temperature Bath, capable of maintaining
Standards volume information, refer to the standard’s Document Summary page on
90 6 1°C.
the ASTM website.
3
5.1.2.2 Gas-Tight Gas Chromatographic Syringes, which
The last approved version of this historical standard is referenced on
www.astm.org. can be heated to 90°C for sampling and injection.
*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

---------------------- Page: 1 ----------------------
D4526 − 20
5.1.2.3 Valve, 6-port for backflush assembly. 6.5 Standards, best a
...

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: D4526 − 12 D4526 − 20
Standard Practice for
Determination of Volatiles in Polymers by Static Headspace
1
Gas Chromatography
This standard is issued under the fixed designation D4526; 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 Headspace gas chromatography (GC) involves the determination of volatile components in a polymer solution by gas
chromatography of a vapor phase in thermal equilibrium with the sample matrix. Volatiles in finely ground insoluble polymers can
also be determined with and without an extracting solvent.
1.2 This practice provides two procedures:
1.2.1 Procedure A—Automatic headspace analysis.
1.2.2 Procedure B—Manual injection headspace analysis.
1.3 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 67.
NOTE 1—There is no known ISO equivalent to this standard.
1.4 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
D4322 Test Method for Residual Acrylonitrile Monomer Styrene-Acrylonitrile Copolymers and Nitrile Rubber by Headspace
3
Gas Chromatography (Withdrawn 2010)
E260 Practice for Packed Column Gas Chromatography
E355 Practice for Gas Chromatography Terms and Relationships
E594 Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid Chromatography
3. Terminology
3.1 General—The units, symbols, and abbreviations used in this test method are in accordance with Terminology D883 and
Practice IEEE/ASTM SI-10.
4. Significance and Use
4.1 For various reasons, one may want to There are various reasons why one would measure the level of unreacted or residual
monomer, water, or other volatile components in a polymer sample.
4.2 Volatiles of interest are often at trace concentrations. Headspace analysis is suited for determination of these trace
components which often cannot be determined by conventional gas chromatography because of sample decomposition or
interferences.
1
This practice 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 Dec. 15, 2012May 15, 2020. Published December 2012June 2020. Originally approved in 1985. Last previous edition approved in 20072012
as D4526 - 97D4526 - 12.(2007). DOI: 10.1520/D4526-12.10.1520/D4526-20.
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.
3
The last approved version of this historical standard is referenced on www.astm.org.
*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

---------------------- Page: 1 ----------------------
D4526 − 20
4.3 For polymer analysis, sample treatment for headspace analysis is simpler than conventional gas chromatography, where
additional precipitation steps may be are required to prevent polymer contamination of the chromatographic column.
4.4 This headspace practice will be able to determine qualitatively any component with sufficient vapor pressure. It is capable
of yielding semiquantitative results and can be used for relative comparisons between samples.
5. Apparatus
5.1 Gas Chromatograph, equipped with an appropriate detector and backflush valve.
,
5.1.1 For Procedure A, an Automated Headspace Sampler, including backflush capability, thermostated sample tray, and
associated accessories fulfill these requirements while providing for automatic sequential sampling of headspace vapors.
5.1.
...