ASTM D4526-12
(Practice)Standard Practice for Determination of Volatiles in Polymers by Static Headspace Gas Chromatography
Standard Practice for Determination of Volatiles in Polymers by Static Headspace Gas Chromatography
SIGNIFICANCE AND USE
3.1 For various reasons, one may want to measure the level of unreacted or residual monomer, water, or other volatile components in a polymer sample.
3.2 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.
3.3 For polymer analysis, sample treatment for headspace analysis is simpler than conventional gas chromatography, where precipitation steps may be required to prevent polymer contamination of the chromatographic column.
3.4 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 and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 6. Note 1—There is no known ISO equivalent to this standard.
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Designation: D4526 − 12
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* 3. Significance and Use
3.1 For various reasons, one may want to measure the level
1.1 Headspace gas chromatography (GC) involves the de-
of unreacted or residual monomer, water, or other volatile
termination of volatile components in a polymer solution by
components in a polymer sample.
gas chromatography of a vapor phase in thermal equilibrium
with the sample matrix. Volatiles in finely ground insoluble
3.2 Volatiles of interest are often at trace concentrations.
polymers can also be determined with and without an extract- Headspace analysis is suited for determination of these trace
ing solvent. componentswhichoftencannotbedeterminedbyconventional
gas chromatography because of sample decomposition or
1.2 This practice provides two procedures:
interferences.
1.2.1 Procedure A—Automatic headspace analysis.
3.3 For polymer analysis, sample treatment for headspace
1.2.2 Procedure B—Manual injection headspace analysis.
analysis is simpler than conventional gas chromatography,
where precipitation steps may be required to prevent polymer
1.3 This standard does not purport to address all of the
contamination of the chromatographic column.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3.4 This headspace practice will be able to determine
priate safety and health practices and determine the applica-
qualitatively any component with sufficient vapor pressure. It
bility of regulatory limitations prior to use. Specific precau-
is capable of yielding semiquantitative results and can be used
tionary statements are given in Section 6.
for relative comparisons between samples.
NOTE 1—There is no known ISO equivalent to this standard.
4. Apparatus
4.1 Gas Chromatograph, equipped with an appropriate
2. Referenced Documents
detector and backflush valve.
2
2.1 ASTM Standards:
4.1.1 For Procedure A, an Automated Headspace Sampler,
4,5
D4322Test Method for Residual Acrylonitrile Monomer
including backflush capability, thermostated sample tray,
Styrene-Acrylonitrile Copolymers and Nitrile Rubber by
and associated accessories fulfill these requirements while
3
Headspace Gas Chromatography (Withdrawn 2010) providing for automatic sequential sampling of headspace
E260Practice for Packed Column Gas Chromatography
vapors.
E355PracticeforGasChromatographyTermsandRelation- 4.1.2 Procedure B requires the following additional equip-
ment:
ships
4.1.2.1 Constant-Temperature Bath, capable of maintaining
E594Practice for Testing Flame Ionization Detectors Used
90 6 1°C.
in Gas or Supercritical Fluid Chromatography
4.1.2.2 Gas-Tight Gas Chromatographic Syringes, which
can be heated to 90°C for sampling and injection.
4.1.2.3 Valve, 6-port for backflush assembly.
1
ThispracticeisunderthejurisdictionofASTMCommitteeD20onPlasticsand
is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
NOTE 2—Appropriate detectors could include the following:
Current edition approved Dec. 15, 2012. Published December 2012. Originally
(a) Flame ionization (FID) for general organic volatiles,
approved in 1985. Last previous edition approved in 2007 as D4526-97(2007).
DOI: 10.1520/D4526-12.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Thesolesourceofsupplyoftheapparatusknowntothecommitteeatthistime
Standards volume information, refer to the standard’s Document Summary page on is Perkin-Elmer Corp., Main Ave., Norwalk, CT 06856.
5
the ASTM website. If you are aware of alternative suppliers, please provide this information to
3
The last approved version of this historical standard is referenced on ASTM International Headquarters. Your comments will receive careful consider-
1
www.astm.org. ation at a meeting of the responsible technical committee, which you may attend.
*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 − 12
(b) Electron capture (EC) for halogenated species,
6. Safety Precautions
(c) Nitrogen-phosphorous (NPD) for acrylonitrile,
6.1 Volatiles such as vinyl chloride and acrylonitrile should
(d) Thermal conductivity (TC)
...
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 − 96 (Reapproved 2007) D4526 − 12
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 and health practices and determine the applicability of regulatory
limitations prior to use. Specific precautionary statements are given in Section 6.
NOTE 1—There is no equivalent ISO known ISO equivalent to this standard.
2. Referenced Documents
2
2.1 ASTM Standards:
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. Significance and Use
3.1 For various reasons, one may want to measure the level of unreacted or residual monomer, water, or other volatile
components in a polymer sample.
3.2 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.
3.3 For polymer analysis, sample treatment for headspace analysis is simpler than conventional gas chromatography, where
precipitation steps may be required to prevent polymer contamination of the chromatographic column.
3.4 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.
4. Apparatus
4.1 Gas Chromatograph, equipped with an appropriate detector and backflush valve.
4,5
4.1.1 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.
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 Sept. 1, 2007Dec. 15, 2012. Published November 2007December 2012. Originally approved in 1985. Last previous edition approved in 20012007
ε1
as D4526 - 97(2001)(2007). . DOI: 10.1520/D4526-96R07.10.1520/D4526-12.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. 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.
4
The sole source of supply of the apparatus known to the committee at this time is Perkin-Elmer Corp., Main Ave., Norwalk, CT 06856.
*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 − 12
4.1.2 Procedure B requires the following additional equipment:
4.1.2.1 Constant-Temperature Bath, capable of maintaining 90 6 1°C.
4.1.2.2 Gas-Tight Gas Chromatographic Syringes, which can be heated to 90°C for sampling and injection.
4.1.2.3 Valve, 6-port for backflush assembly.
NOTE 2—Appropriate detectors could include the following:
(a) Flame ionization (FID) for general organic volatiles,
(b) Electron capture (EC) for halogen
...
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