ASTM D4443-12
(Test Method)Standard Test Method for Determining Residual Vinyl Chloride Monomer Content in PPB Range in Vinyl Chloride Homo- and Co-Polymers by Headspace Gas Chromatography
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 level of ∼5 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.
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Designation: D4443 − 12
StandardTest 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* 4.2 The polymer solution and headspace are equilibrated at
an elevated temperature.
1.1 This test method is suitable for determining the residual
vinyl chloride monomer (RVM) content of homopolymer and 4.3 Aliquots of headspace gas are injected into a gas
copolymers of vinyl chloride down to a level of ;5 ppb. chromatograph and the vinyl chloride monomer is separated.
The response of vinyl chloride monomer is determined by the
1.2 Thistestmethodisapplicabletoanypolymerform,such
use of one of several suggested detectors.
asresin,compound,film,bottlewall,etc.thatcanbedissolved
in a suitable solvent. 4.4 Calibration is accomplished using either (a) vinyl chlo-
ride monomer in nitrogen gas standards, (b) standard solutions
1.3 This standard does not purport to address all of the
containingknownamountsofvinylchloridemonomer,or (c)a
safety concerns, if any, associated with its use. It is the
method of standard addition.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Significance and Use
bility of regulatory limitations prior to use. Specific hazard
5.1 Vinyl chloride-containing polymers are widely used to
statements are given in Section 9 and Note 13.
package a variety of materials, including foods.
NOTE 1—This standard is equivalent to ISO 6401.
5.2 Vinyl chloride monomer has been shown to be a human
2. Referenced Documents
carcinogen. Threshold toxicity value has not been established.
2.1 ISO Standard:
5.3 Plastic manufacturers, food packagers, government
ISO6401Plastics—Homopolymer and Copolymer Resins
agencies, etc. have a need to know the residual vinyl chloride
of Vinyl Chloride—Determination of Residual Vinyl
monomer content of vinyl chloride-containing polymers.
2
Chloride Monomer—Gas Chromatographic Method
2.2 OSHA Standard:
6. Interferences
3
29 CFR 1919.1017Vinyl Chloride
6.1 N,N-dimethylacetamideshouldbeanalyzedunderiden-
ticalconditionstodeterminetheabsenceofinterferencesatthe
3. Terminology
vinyl chloride monomer gas chromatography (GC) retention
3.1 Abbreviations:
time.
3.1.1 DMAc—N,N-dimethylacetamide.
6.2 Other solvents, monomers, or compounding aids may
3.1.2 VCM—Vinyl chloride monomer.
cause interference at the vinyl chloride monomer GC retention
time.
4. Summary of Test Method
4.1 Samples of vinyl chloride-containing polymers are dis-
7. Apparatus
solved in a suitable solvent in a closed system.
7.1 Gas Chromatography, equipped with either a flame
ionization detector (FID), a photo ionization detector (PID), or
1
ThistestmethodisunderthejurisdictionofASTMCommitteeD20onPlastics
a Hall electroconductivity detector (HED), backflushing valve,
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
and either automatic capability or manual sampling (Note 2)
Current edition approved Oct. 1, 2012. Published November 2012. Originally
and ability to analyze the headspace vapors contained in a
approved in 1984. Last previous edition approved in 2007 as D4443–07. DOI:
10.1520/D4443-12.
sealed vial.
2
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
NOTE 2—If the analyses are to be performed manually (that is, by
4th Floor, New York, NY 10036, http://www.ansi.org.
3
Available from Superintendent of Documents, US Government Printing Office, syringe injection), then the following equipment will also be needed:
Washington, DC 20402. (1) Constant-temperature bath or oven capable of maintaining a
*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 − 12
temperature of 90 6 1°C.
8.5 Air, breathing or water-pumped.
(2) Gas-tight GC syringes for sampling and injection.
8.6 N,N-Dimethylacetamide (DMAc), sparged with nitrogen
(3) Sample bottles with fluoropolymer faces septa and caps (size
gas for up to a week at room temperature to remove chromato-
optional).
(4) Gloves for handling hot syringes.
graphic interferences.
4,5
7.2 Chromatographic Column, 3% OV-101 on 80/100
4,5
9. Hazards
1
mesh Chromosorb WHP , ⁄8-in. (3.2-mm) outside diameter
1
by2ft(0.6m),stainlesssteelconnectedthrough ⁄8-in.“tee
...
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 − 07 D4443 − 12
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 level of ;5 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 and health practices and determine the applicability of regulatory
limitations prior to use. Specific hazard statements are given in Section 9 and Note 13.
NOTE 1—This standard is equivalent to ISO 6401.
NOTE 1—This test method is similar to ISO 6401.
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.
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.
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, 2007Oct. 1, 2012. Published November 2007November 2012. Originally approved in 1984. Last previous edition approved in 20022007
as D4443 – 95D4443 – 07.(2002). DOI: 10.1520/D4443-07.10.1520/D4443-12.
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.
*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 − 12
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 flame ionization detector (FID), a photo ionization detector (PID), or a Hall
electroconductivity detector (HED), backflushing valve, and either automatic capability or manual sampling (Note 2) and ability
to analyze the headspace vapors contained in a sealed vial.
NOTE 2—If the analyses are to be performed manually (that is, by syringe injection), then the following equipment will also be needed:
(1) Constant-temperature bath or oven capable of maintaining a temperature of 90 6 1°C.
(2) Gas-tight GC syringes for sampling and injection.
(3) Sample bo
...
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