ASTM D4443-19

Standard Test Method for Determining Residual Vinyl Chloride Monomer Content in PPB Range in Vinyl Chloride Homo- and Co-Polymers by Headspace Gas Chromatography

SIGNIFICANCE AND USE
5.1 Vinyl chloride-containing polymers are widely used to package a variety of materials, including foods.  
5.2 Vinyl chloride monomer has been shown to be a human carcinogen. Threshold toxicity value has not been established.  
5.3 Plastic manufacturers, food packagers, government agencies, etc. have a need to know the residual vinyl chloride monomer content of vinyl chloride-containing polymers.
SCOPE
1.1 This test method is suitable for determining the residual vinyl chloride monomer (RVM) content of homopolymer and copolymers of vinyl chloride down to a concentration of ∼5 µg/kg (ppb).  
1.2 This test method is applicable to any polymer form, such as resin, compound, film, bottle wall, etc. that can be dissolved in a suitable solvent.  
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 hazard statements are given in Section 9 and Note 10.  
Note 1: This standard is equivalent to ISO 6401.  
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: 31-Mar-2019
• ICS: 83.080.20 - Thermoplastic materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

Relations

• Referred By: ASTM D3749-19 - Standard Test Method for Residual Vinyl Chloride Monomer in Poly(Vinyl Chloride) Resins by Gas Chromatographic Headspace Technique
• Effective Date: 01-Apr-2019

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: D4443 − 19
Standard Test Method for
Determining Residual Vinyl Chloride Monomer Content in
PPB Range in Vinyl Chloride Homo- and Co-Polymers by
1
Headspace Gas Chromatography
This standard is issued under the fixed designation D4443; 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. Terminology
3.1 Abbreviations:
1.1 This test method is suitable for determining the residual
vinyl chloride monomer (RVM) content of homopolymer and
3.1.1 DMAc—N,N-dimethylacetamide.
copolymers of vinyl chloride down to a concentration of ;5
3.1.2 VCM—Vinyl chloride monomer.
µg/kg (ppb).
1.2 Thistestmethodisapplicabletoanypolymerform,such
4. Summary of Test Method
asresin,compound,film,bottlewall,etc.thatcanbedissolved
4.1 Samples of vinyl chloride-containing polymers are dis-
in a suitable solvent.
solved in a suitable solvent in a closed system.
1.3 This standard does not purport to address all of the
4.2 The polymer solution and headspace are equilibrated at
safety concerns, if any, associated with its use. It is the
an elevated temperature.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
4.3 Aliquots of headspace gas are injected into a gas
mine the applicability of regulatory limitations prior to use.
chromatograph and the vinyl chloride monomer is separated.
Specific hazard statements are given in Section 9 and Note 10.
The response of vinyl chloride monomer is determined by the
use of one of several suggested detectors.
NOTE 1—This standard is equivalent to ISO 6401.
1.4 This international standard was developed in accor-
4.4 Calibration is accomplished using either (a) vinyl chlo-
dance with internationally recognized principles on standard-
ride monomer in nitrogen gas standards, (b) standard solutions
ization established in the Decision on Principles for the
containingknownamountsofvinylchloridemonomer,or (c)a
Development of International Standards, Guides and Recom-
method of standard addition.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
5. Significance and Use
5.1 Vinyl chloride-containing polymers are widely used to
2. Referenced Documents
package a variety of materials, including foods.
2.1 ISO Standard:
5.2 Vinyl chloride monomer has been shown to be a human
ISO6401Plastics—Homopolymer and Copolymer Resins
carcinogen. Threshold toxicity value has not been established.
of Vinyl Chloride—Determination of Residual Vinyl
2
5.3 Plastic manufacturers, food packagers, government
Chloride Monomer—Gas Chromatographic Method
agencies, etc. have a need to know the residual vinyl chloride
2.2 OSHA Standard:
3 monomer content of vinyl chloride-containing polymers.
29 CFR 1919.1017Vinyl Chloride
6. Interferences
1 6.1 N,N-dimethylacetamideshouldbeanalyzedunderiden-
ThistestmethodisunderthejurisdictionofASTMCommitteeD20onPlastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods. ticalconditionstodeterminetheabsenceofinterferencesatthe
Current edition approved April 1, 2019. Published May 2019. Originally
vinyl chloride monomer gas chromatography (GC) retention
approved in 1984. Last previous edition approved in 2013 as D4443–13. DOI:
time.
10.1520/D4443-19.
2
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
6.2 Other solvents, monomers, or compounding aids may
4th Floor, New York, NY 10036, http://www.ansi.org.
3
cause interference at the vinyl chloride monomer GC retention
Available from Superintendent of Documents, US Government Printing Office,
Washington, DC 20402, https://bookstore.gpo.gov. time.
*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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D4443 − 19
7. Apparatus properly functioning hood and septum-sealed sample contain-
ers are recommended.
7.1 Gas Chromatography, equipped with either, a mass
9.1.2 Avoid all contact with heated parts of the gas
spectrometricdetector,flameionizationdetector(FID),aphoto
chromatograph, hot syringes, and sample bottles. Handle all
ionization detector (PID), or a Hall electroconductivity detec-
electrical connections with care.
tor (HED), backflushing valve, and either automatic capability
9.1.3 Once heated, sample vials are under pressure
...

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: D4443 − 13 D4443 − 19
Standard Test Method for
Determining Residual Vinyl Chloride Monomer Content in
PPB Range in Vinyl Chloride Homo- and Co-Polymers by
1
Headspace Gas Chromatography
This standard is issued under the fixed designation D4443; 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 test method is suitable for determining the residual vinyl chloride monomer (RVM) content of homopolymer and
copolymers of vinyl chloride down to a levelconcentration of ;5 ppb.μg/kg (ppb).
1.2 This test method is applicable to any polymer form, such as resin, compound, film, bottle wall, etc. that can be dissolved
in a suitable solvent.
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 hazard statements are given in Section 9 and Note 10.
NOTE 1—This standard is equivalent to ISO 6401.
NOTE 1—This standard is equivalent to ISO 6401.
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
2.1 ISO Standard:
ISO 6401 Plastics—Homopolymer and Copolymer Resins of Vinyl Chloride—Determination of Residual Vinyl Chloride
2
Monomer—Gas Chromatographic Method
2.2 OSHA Standard:
3
29 CFR 1919.1017 Vinyl Chloride
3. Terminology
3.1 Abbreviations:
3.1.1 DMAc—N,N-dimethylacetamide.
3.1.2 VCM—Vinyl chloride monomer.
4. Summary of Test Method
4.1 Samples of vinyl chloride-containing polymers are dissolved in a suitable solvent in a closed system.
4.2 The polymer solution and headspace are equilibrated at an elevated temperature.
4.3 Aliquots of headspace gas are injected into a gas chromatograph and the vinyl chloride monomer is separated. The response
of vinyl chloride monomer is determined by the use of one of several suggested detectors.
4.4 Calibration is accomplished using either (a) vinyl chloride monomer in nitrogen gas standards, (b) standard solutions
containing known amounts of vinyl chloride monomer, or (c) a method of standard addition.
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 Nov. 1, 2013April 1, 2019. Published November 2013May 2019. Originally approved in 1984. Last previous edition approved in 20122013 as
D4443 – 12.D4443 – 13. DOI: 10.1520/D4443-13.10.1520/D4443-19.
2
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
3
Available from Superintendent of Documents, US Government Printing Office, Washington, DC 20402.20402, https://bookstore.gpo.gov.
*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 ----------------------
D4443 − 19
5. Significance and Use
5.1 Vinyl chloride-containing polymers are widely used to package a variety of materials, including foods.
5.2 Vinyl chloride monomer has been shown to be a human carcinogen. Threshold toxicity value has not been established.
5.3 Plastic manufacturers, food packagers, government agencies, etc. have a need to know the residual vinyl chloride monomer
content of vinyl chloride-containing polymers.
6. Interferences
6.1 N,N- dimethylacetamide should be analyzed under identical conditions to determine the absence of interferences at the vinyl
chloride monomer gas chromatography (GC) retention time.
6.2 Other solvents, monomers, or compounding aids may cause interference at the vinyl chloride monomer GC retention time.
7. Apparatus
7.1 Gas Chromatography, equipped with either a either, a mass spectrometric detector, flame ionization detector (FID), a photo
ionization detector (PID), or a Hall electroconductivity detector (HED), ba
...