ASTM D4443-95

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

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 [simalar]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-There is no similar or equivalent ISO standard.

General Information

• Status: Historical
• Publication Date: 31-Dec-1994
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

Relations

• Replaced By: ASTM D4443-95(2002) - Standard Test Method for Determining Residual Vinyl Chloride Monomer Content in PPB Range in Vinyl Chloride Homo- and Co-Polymers by Headspace Gas Chromatography
• Effective Date: 10-Oct-1995

Standards Content (Sample)

Designation: D 4443 – 95
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
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 D 4443; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope ride monomer in nitrogen gas standards, (b) standard solutions
containing known amounts of vinyl chloride monomer, or (c) a
1.1 This test method is suitable for determining the residual
method of standard addition.
vinyl chloride monomer (RVM) content of homopolymer and
copolymers of vinyl chloride down to a level of ;5 ppb.
5. Significance and Use
1.2 This test method is applicable to any polymer form, such
5.1 Vinyl chloride-containing polymers are widely used to
as resin, compound, film, bottle wall, etc. that can be dissolved
package a variety of materials, including foods.
in a suitable solvent.
5.2 Vinyl chloride monomer has been shown to be a human
1.3 This standard does not purport to address all of the
carcinogen. Threshold toxicity value has not been established.
safety concerns, if any, associated with its use. It is the
5.3 Plastic manufacturers, food packagers, government
responsibility of the user of this standard to establish appro-
agencies, etc. have a need to know the residual vinyl chloride
priate safety and health practices and determine the applica-
monomer content of vinyl chloride-containing polymers.
bility of regulatory limitations prior to use. Specific hazard
statements are given in Section 9 and Note 13.
6. Interferences
NOTE 1—There is no similar or equivalent ISO standard.
6.1 N,N- dimethylacetamide should be analyzed under iden-
tical conditions to determine the absence of interferences at the
2. Referenced Document
vinyl chloride monomer gas chromatography (GC) retention
2.1 OSHA Standard:
time.
2
29 CFR 1919.1017—Vinyl Chloride
6.2 Other solvents, monomers, or compounding aids may
cause interference at the vinyl chloride monomer GC retention
3. Terminology
time.
3.1 Abbreviations:
3.1.1 DMAc—N,N-dimethylacetamide. 7. Apparatus
3.1.2 VCM—Vinyl chloride monomer.
7.1 Gas Chromatography, equipped with either a flame
ionization detector (FID), a photo ionization detector (PID), or
4. Summary of Test Method
a Hall electroconductivity detector (HED), backflushing valve,
4.1 Samples of vinyl chloride-containing polymers are dis-
and either automatic capability or manual sampling (Note 2)
solved in a suitable solvent in a closed system.
and ability to analyze the headspace vapors contained in a
4.2 The polymer solution and headspace are equilibrated at
sealed vial.
an elevated temperature.
NOTE 2—If the analyses are to be performed manually (that is, by
4.3 Aliquots of headspace gas are injected into a gas
syringe injection), then the following equipment will also be needed:
chromatograph and the vinyl chloride monomer is separated.
(1) Constant-temperature bath or oven capable of maintaining a
The response of vinyl chloride monomer is determined by the
temperature of 90 6 1°C.
use of one of several suggested detectors.
(2) Gas-tight GC syringes for sampling and injection.
4.4 Calibration is accomplished using either (a) vinyl chlo-
(3) Sample bottles with fluoropolymer faces septa and caps (size
optional).
(4) Gloves for handling hot syringes.
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This test method is under the jurisdiction of ASTM Committee D-20 on Plastics
3
7.2 Chromatographic Column, 3 % OV-101 on 80/100
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods
3
1
(Section D20.70.03).
mesh Chromosorb WHP , ⁄8-in. (3.2-mm) outside diameter by
Current edition approved Oct. 10, 1995. Published December 1995. Originally
1
2 ft (0.6 m), stainless steel connected through ⁄8-in. “tee” to
e1
published as D4443 – 84. Last previous edition D 4443 – 84 (1989) .
This revision includes the addition of an ISO equivalency statement and a
keywords section.
2 3
Available from Superintendent of Documents, US Government Printing Office, Column packing is available from Supelco, Inc., P.O. Box 628, 146 S. Water
Washington, DC 20402. St., Bellefonte, PA 16823.
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D 4443
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0.19 % picric acid on 80/100 mesh Carbopack C , ⁄8-in. properly functioning hood and septum-sealed sample contain-
outside diameter by 8 ft (2.4 m), stainless steel. ers are recommended.
9.1.2 Avoid all contact with heated parts of the gas chro-
NOTE 3—Any column packing that will resolve VCM from interfer-
matograph, hot syringes, and sample bottles. Handle all elec-
ences and elute VCM in
...