ASTM D3749-08

Standard Test Method for Residual Vinyl Chloride Monomer in Poly(Vinyl Chloride) Resins by Gas Chromatographic Headspace Technique

SIGNIFICANCE AND USE
Poly(vinyl chloride) resins must contain a minimum possible amount of unreacted, or free, VCM.
This test method provides a measure of RVCM which is suitable for manufacturing control or specification acceptance purposes.
Under optimum conditions, a lower level of detection of 2 ppm by volume VCM can be detected in the headspace vapor. Using a 4-g sample, this is equivalent to about 0.02 ppm by mass RVCM in the PVC resin.
SCOPE
1.1 This test method is suitable for determining the residual vinyl chloride monomer (RVCM) content of poly(vinyl chloride) (PVC) homopolymer and copolymer resins for uses other than food contact. The range for this test, based on interlaboratory evaluation, is from 0.1 to 400 ppm RVCM.
1.2 This test method can be adapted to determinations of RVCM in a PVC copolymer resin if the Henry's Law constant at 90°C for that copolymer is known.
1.3 This test method cannot be used for polymer in fused forms, such as cubes or sheets. Refer to Test Method D 4443 or Test Method D 3680 for these materials.
1.4 This test method is proposed as an alternative to EPA Method 107 for determination of vinyl chloride monomers in dry-resin samples.
1.5 The values stated SI units are to be regarded as the standard.
1.6 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.
Note 1—This standard and ISO 6401:2008 address the same subject matter, but differ in technical content.

General Information

• Status: Historical
• Publication Date: 30-Nov-2008
• ICS: 83.080.20 - Thermoplastic materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

Relations

• Replaces: ASTM D3749-95(2002) - Standard Test Method for Residual Vinyl Chloride Monomer in Poly(Vinyl Chloride) Resins by Gas Chromatographic Headspace Technique
• Effective Date: 01-Dec-2008
• Replaced By: ASTM D3749-12 - Standard Test Method for Residual Vinyl Chloride Monomer in Poly(Vinyl Chloride) Resins by Gas Chromatographic Headspace Technique
• Effective Date: 01-Oct-2012

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D3749 − 08
StandardTest Method for
Residual Vinyl Chloride Monomer in Poly(Vinyl Chloride)
1
Resins by Gas Chromatographic Headspace Technique
This standard is issued under the fixed designation D3749; 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* Copolymers by Solution Injection Technique (Withdrawn
3
2005)
1.1 This test method is suitable for determining the residual
D4443Test Method for Determining Residual Vinyl Chlo-
vinyl chloride monomer (RVCM) content of poly(vinyl chlo-
ride Monomer Content in PPB Range in Vinyl Chloride
ride)(PVC)homopolymerandcopolymerresinsforusesother
Homo- and Co-Polymers by Headspace Gas Chromatog-
than food contact. The range for this test, based on interlabo-
raphy
ratory evaluation, is from 0.1 to 400 ppm RVCM.
D4526Practice for Determination of Volatiles in Polymers
1.2 This test method can be adapted to determinations of
by Static Headspace Gas Chromatography
RVCM in a PVC copolymer resin if the Henry’s Law constant
E691Practice for Conducting an Interlaboratory Study to
at 90°C for that copolymer is known.
Determine the Precision of a Test Method
1.3 This test method cannot be used for polymer in fused 2.2 Federal Standards:
forms,suchascubesorsheets.RefertoTestMethodD4443or EnvironmentalProtectionAgencyMethod107 Determina-
Test Method D3680 for these materials. tion ofVinyl Chloride Content of In-ProcessWaste-Water
Samples,andVinylChlorideContentofPoly(VinylChlo-
1.4 This test method is proposed as an alternative to EPA
4
ride) Resin, Slurry, Wet Cake, and Latex Samples
Method107 for determination of vinyl chloride monomers in
29CFR 1919.1017 Vinyl Chloride for Regulated Levels of
dry-resin samples.
5
Exposure
1.5 The values stated SI units are to be regarded as the
2.3 ISO Standard:
standard.
ISO6401:2008 Determination of Residual Vinyl Chloride
1.6 This standard does not purport to address all of the
Monomer in Homopolymers and Copolymers by Gas
6
safety concerns, if any, associated with its use. It is the
Chromatography
responsibility of the user of this standard to establish appro-
3. Terminology
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
3.1 Acronyms:
3.1.1 VCM—Vinyl chloride monomer.
NOTE 1—This standard and ISO6401:2008 address the same subject
matter, but differ in technical content.
3.1.2 RVCM—Residual vinyl chloride monomer.
3.1.3 PVC—Poly(vinyl chloride).
2. Referenced Documents
2
3.1.4 OSHA—Occupational Safety and Health Agency.
2.1 ASTM Standards:
D3680Test Method for Residual Vinyl Chloride Monomer
3.1.5 FID—Flame ionization detector.
Content of Poly(Vinyl Chloride) Resins, Compounds, and
3
The last approved version of this historical standard is referenced on
1
ThistestmethodisunderthejurisdictionofASTMCommitteeD20onPlastics www.astm.org.
4
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods. Available from United States Environmental Protection Agency (EPA), Ariel
Current edition approved Dec. 1, 2008. Published December 2008. Originally Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460, http://
approved in 1978. Last previous edition approved in 2002 as D3749-95(2002). www.epa.gov.
5
DOI: 10.1520/D3749-08. AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM www.access.gpo.gov.
6
Standards volume information, refer to the standard’s Document Summary page on Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.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

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D3749 − 08
7
3.1.6 PID—Photoionization detector. 7.2 Chromatographic Column, 80/100-mesh in 1-m by
3.2-mm stainless steel tubing.
3.1.7 HED—Hall electroconductivity detector.
NOTE 3—Any column that will resolve VCM from any interferences
3.1.8 MHE—Multiple headspace extraction.
and will elute VCM between 1 and 4 min using a system pressure of 100
to 150 kPa is satisfactory. If an alternate column is used, the chromato-
4. Summary of Test Method
graphic conditions may need to be modified.
4.1 The basis for this test method relates to the vapor
7.3 Integrator,
...

This document is not anASTM standard and is intended only to provide the user of anASTM 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:D3749–95 (Reapproved 2002) Designation:D3749–08
Standard Test Method for
Residual Vinyl Chloride Monomer in Poly(Vinyl Chloride)
1
Resins by Gas Chromatographic Headspace Technique
This standard is issued under the fixed designation D3749; 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*
1.1 This test method is suitable for determining the residual vinyl chloride monomer (RVCM) content of poly(vinyl chloride)
(PVC) homopolymer and copolymer resins for uses other than food contact. The range for this test, based on interlaboratory
evaluation, is from 0.1 to 400 ppm RVCM.
1.2 ThistestmethodcanbeadaptedtodeterminationsofRVCMinaPVCcopolymerresiniftheHenry’sLawconstantat90°C
for that copolymer is known.
1.3 This test method cannot be used for polymer in fused forms, such as cubes or sheets. Refer toTest Method D4443 orTest
Method D3680 for these materials.
1.4 ThistestmethodisproposedasanalternativetoEPAMethod107fordeterminationofvinylchloridemonomersindry-resin
samples.
1.5 The values stated SI units are to be regarded as the standard.
1.6 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.
NOTE1—This test method is similar to ISO 6401-1985 in title only. The technical content is significantly different. 1—This standard and
ISO6401:2008 address the same subject matter, but differ in technical content.
2. Referenced Documents
2
2.1 ASTM Standards:
D3680 Test Method for Residual Vinyl Chloride Monomer Content of Poly(Vinyl Chloride) Resins, Compounds, and
Copolymers by Solution Injection Technique
D4443 TestMethodforAnalysisforDeterminingResidualVinylChlorideMonomerContentinPPBRangeinVinylChloride
Homo- and Co-Polymers by Headspace Gas Chromatography
D4526 Practice for Determination of Volatiles in Polymers by Static Headspace Gas Chromatography
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 Federal Standards:
EnvironmentalProtectionAgencyMethod107 Determination of Vinyl Chloride Content of In-Process Waste-Water Samples,
3
and Vinyl Chloride Content of Poly(Vinyl Chloride) Resin, Slurry, Wet Cake, and Latex Samples
4
29 CFR 1919.1017 Vinyl Chloride for Regulated Levels of Exposure
2.3 ISO Standard:
ISO6401-1985ISO6401:2008 DeterminationofResidualVinylChlorideMonomerinHomopolymersandCopolymersbyGas
5
Chromatography
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 June 15, 1995. PublishedAugust 1995. Originally published as D3749–78. Last previous edition D3749–93. This edition includes revisions to
Section 14.
Current edition approved Dec. 1, 2008. Published December 2008. Originally approved in 1978. Last previous edition approved in 2002 as D3749-95(2002).
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,[e-mail] Annual Book of ASTM Standards
, Vol 06.03.volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Annual Book of ASTM Standards, Vol 08.03.
3
Available from United States Environmental Protection Agency (EPA), Ariel Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460, http://www.epa.gov.
4
Annual Book of ASTM Standards, Vol 14.02.
4
Available from U.S. Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
www.access.gpo.gov.
5
Available from the U.S. Environmental Protection Agency, Research Triangle Park, NC27711.
5
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.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

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D3749–08
3. Terminology
3.1 Acronyms: Acronyms:
3.1.1 VCM—Vinyl chloride monomer.
3.1.2 RVCM—Residual vinyl chloride monomer.
3.1.3 PVC—Poly(vinyl ch
...