ASTM D3749-95(2002)
(Test Method)Standard Test Method for Residual Vinyl Chloride Monomer in Poly(Vinyl Chloride) Resins by Gas Chromatographic Headspace Technique
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 90C 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 test method is similar to ISO 6401-1985 in title only. The technical content is significantly different.
General Information
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D3749–95 (Reapproved 2002)
Standard Test Method for
Residual Vinyl Chloride Monomer in Poly(Vinyl Chloride)
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope by Headspace Gas Chromatography
E691 Practice for Conducting an Interlaboratory Study to
1.1 This test method is suitable for determining the residual
Determine the Precision of a Test Method
vinyl chloride monomer (RVCM) content of poly(vinyl chlo-
2.2 Federal Standards:
ride)(PVC)homopolymerandcopolymerresinsforusesother
EnvironmentalProtectionAgencyMethod107 Determination
than food contact. The range for this test, based on interlabo-
of Vinyl Chloride Content of In-Process Waste-Water
ratory evaluation, is from 0.1 to 400 ppm RVCM.
Samples, andVinyl Chloride Content of Poly(Vinyl Chlo-
1.2 This test method can be adapted to determinations of
ride) Resin, Slurry, Wet Cake, and Latex Samples
RVCM in a PVC copolymer resin if the Henry’s Law constant
29 CFR 1919.1017 Vinyl Chloride for Regulated Levels of
at 90°C for that copolymer is known.
Exposure
1.3 This test method cannot be used for polymer in fused
2.3 ISO Standard:
forms,suchascubesorsheets.RefertoTestMethodD4443or
ISO 6401-1985 Determination of Residual Vinyl Chloride
Test Method D3680 for these materials.
Monomer in Homopolymers and Copolymers by Gas
1.4 This test method is proposed as an alternative to EPA
Chromatography
Method107 for determination of vinyl chloride monomers in
dry-resin samples.
3. Terminology
1.5 The values stated SI units are to be regarded as the
3.1 Acronyms:Acronyms:
standard.
3.1.1 VCM—Vinyl chloride monomer.
1.6 This standard does not purport to address all of the
3.1.2 RVCM—Residual vinyl chloride monomer.
safety concerns, if any, associated with its use. It is the
3.1.3 PVC—Poly(vinyl chloride).
responsibility of the user of this standard to establish appro-
3.1.4 OSHA—Occupational Safety and Health Agency.
priate safety and health practices and determine the applica-
3.1.5 FID—Flame ionization detector.
bility of regulatory limitations prior to use.
3.1.6 PID—Photoionization detector.
NOTE 1—ThistestmethodissimilartoISO6401-1985intitleonly.The
3.1.7 HED—Hall electroconductivity detector.
technical content is significantly different.
3.1.8 MHE—Multiple headspace extraction.
2. Referenced Documents
4. Summary of Test Method
2.1 ASTM Standards:
4.1 The basis for this test method relates to the vapor
D3680 Test Method for ResidualVinyl Chloride Monomer
equilibriumthatisestablishedbetweenRVCM,PVCresin,and
Content of Poly(Vinyl Chloride) Resins, Compounds, and
air in a closed system. The RVCM in a PVC resin will
Copolymers by Solution Injection Technique
equilibrate in a closed vessel quite rapidly, provided that the
D4443 Test Method forAnalysis for Determining Residual
temperature of the PVC resin is maintained above the glass
Vinyl Chloride Monomer Content in PPB Range in Vinyl
transition temperature of that specific resin type.
Chloride Homo- and Co-Polymers by Headspace Gas
4.2 After sample equilibration, conventional gas chromato-
Chromatography
graphic (GC) techniques are used. A constant amount of
D4526 Practice for Determination of Volatiles in Polymers
sample headspace vapor is injected into a GC column that is
1 4
ThistestmethodisunderthejurisdictionofASTMCommitteeD20onPlastics Annual Book of ASTM Standards, Vol 14.02.
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods. Available from the U.S. Environmental Protection Agency, Research Triangle
Current edition approved June 15, 1995. Published August 1995. Originally Park, NC27711.
published as D3749–78. Last previous edition D3749–93. This edition includes Available from the Superintendent of Documents, Government Printing Office,
revisions to Section 14. Washington, DC20402.
2 7
Annual Book of ASTM Standards, Vol 06.03. Available from American National Standards Institute, 25 W. 43rd St., 4th
Annual Book of ASTM Standards, Vol 08.03. Floor, New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3749–95 (2002)
packed with a liquid-coated solid support or porous polymer 8. Reagents and Materials
beads.Sampleinjectionisaccomplishedbyavailablecommer-
8.1 Standards—Cylinders of known concentrations of vinyl
cial automatic equipment. Passing through the column in a
chloride in nitrogen gas. Nominal concentrations of 5, 50, and
stream of carrier gas, the vinyl chloride monomer (VCM) is
500 ppm by volume (vppm) are needed, unless multiple
separated from other components which may be present and is
headspace extraction (MHE) is used. Lower concentration
detectedbyastandardsensingdevice.Thesignalisrecordedto
standards may be desirable for a detection limit less than 2
indicatetherelativeconcentrationoftheVCManditsretention
ppm.
time.
8.2 Nitrogen, or helium, oxygen-free, carrier gas for chro-
4.3 Refer to Practice D4526 for additional information on
matograph.
headspace gas chromatography.
8.3 Hydrogen, prepurified for FID detector.
8.4 Air, breathing grade, for FID detector.
5. Significance and Use
5.1 Poly(vinyl chloride) resins must contain a minimum
9. Hazards
possible amount of unreacted, or free, VCM.
9.1 Vinyl chloride monomer is a cancer-suspect agent and
5.2 ThistestmethodprovidesameasureofRVCMwhichis
must never be released to the laboratory atmosphere, even at
suitable for manufacturing control or specification acceptance
low ppm levels. Venting or purging of VCM mixtures must be
purposes.
held to a minimum and should be vented into a properly
5.3 Underoptimumconditions,alowerlevelofdetectionof
functioning fume hood. Refer to 29 CFR 1919.1017 for
2ppmbyvolumeVCMcanbedetectedintheheadspacevapor.
regulated levels of exposure.
Using a 4-g sample, this is equivalent to about 0.02 ppm by
9.2 Be careful not to come into contact with heated parts of
mass RVCM in the PVC resin.
thechromatograph,suchasthedetector,column,hotvials,etc.
Handle all electrical connections with care.
6. Interferences
9.3 Vials should be vented to atmospheric pressure after
6.1 Normally, the vapor above PVC resin will contain only
analysis and prior to removal from the thermostatted turntable.
air, VCM, water, small amounts of catalyst breakdown prod-
A hypodermic needle connected to a syringe containing a
ucts, and any solvents or comonomers used in polymerization.
freshly activated charcoal is suitable for this operation.
Impuritiesinthe0to1000-ppmrangewillgenerallyhaveonly
a very small influence on this equilibrium relationship.
10. Sampling and Storage
6.2 Any material that elutes from the chromatographic
10.1 Weigh and seal resin samples in the headspace vials in
column at approximately the same time as vinyl chloride will
accordance with 12.1 as soon as possible, not to exceed 24 h.
cause high RVCM results.
10.2 Resins may be stored in the sealed headspace vials for
7. Apparatus up to four weeks without loss of VCM if they are analyzed
without being reopened.
7.1 Gas Chromatograph, equipped with a flame ionization
detector (FID), photoionization detector (PID), or a Hall
11. Preparation of Gas Chromatograph
electroconductivity detector (HED) and capable of heating,
sampling, and analyzing the headspace vapors contained in 11.1 Connect carrier gas and detector gas cylinders to the
sealed vials.
chromatograph with the recommended filters and regulators as
required by the manufacturer.
NOTE 2—Automatic backflushing capability may be a desirable option
11.2 Es
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