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ASTM D4747-02

(Test Method)

Standard Test Method for Determining Unreacted Monomer Content of Latexes Using Gas-Liquid Chromatography

Standard Test Method for Determining Unreacted Monomer Content of Latexes Using Gas-Liquid Chromatography

SIGNIFICANCE AND USE
Excessive amounts of unreacted monomer may cause concerns relating to toxicity and odor. This test method is designed to measure the unreacted monomer content of latexes. The results may be used to monitor the extent of polymerization during manufacture, as well as to establish maximum unreacted monomer content for regulatory purposes.
SCOPE
1.1 This test method covers the determination of free monomer content of acrylic latexes. Monomers that have been successfully determined by this procedure include n-butyl methacrylate, n-butyl acrylate, styrene, and methyl methacrylate. The determination of other monomers has not been evaluated, but this test method is believed to be applicable. The established working range of this test method is from 100 to 1000 μg/g, but there is no reason to believe it will not work outside of this range, provided that appropriate dilutions and adjustments in specimen size are made.
1.2 The volatile composition of acrylic latexes is expected to change with time and environmental factors. This time dependence of the determination may be seen as an artificially large deviation of results, making the method mostly applicable for in-house quality control, where sampling and analysis conditions can be better controlled.
1.3 The values stated in inch-pound units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 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. See Section 7 for specific hazard statements.

General Information

Status
Historical
Publication Date
09-Jan-2002
ICS
83.040.10 - Latex and raw rubber
Technical Committee
D01 - Paint and Related Coatings, Materials, and Applications
Drafting Committee
D01.21 - Chemical Analysis of Paints and Paint Materials
Current Stage
Ref Project

Relations

Replaces
ASTM D4747-87(1996)e1 - Standard Test Method for Determining Unreacted Monomer Content of Latexes Using Gas-Liquid Chromatography
Effective Date
10-Jan-2002
Replaced By
ASTM D4747-02(2008) - Standard Test Method for Determining Unreacted Monomer Content of Latexes Using Gas-Liquid Chromatography
Effective Date
01-Feb-2008

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ASTM D4747-02 - Standard Test Method for Determining Unreacted Monomer Content of Latexes Using Gas-Liquid Chromatography
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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:D4747–02
Standard Test Method for
Determining Unreacted Monomer Content of Latexes Using
1
Gas-Liquid Chromatography
This standard is issued under the fixed designation D 4747; 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 into a gas chromatographic column containing a packing
material coated with a stationary phase that separates the
1.1 This test method covers the determination of free
internal standard and monomers in question from each other
monomer content of acrylic latexes. Monomers that have been
and from other volatile compounds.
successfully determined by this procedure include n-butyl
methacrylate, n-butyl acrylate, styrene, and methyl methacry-
4. Significance and Use
late. The determination of other monomers has not been
4.1 Excessive amounts of unreacted monomer may cause
evaluated,butthistestmethodisbelievedtobeapplicable.The
concerns relating to toxicity and odor. This test method is
established working range of this test method is from 100 to
designedtomeasuretheunreactedmonomercontentoflatexes.
1000 µg/g, but there is no reason to believe it will not work
The results may be used to monitor the extent of polymeriza-
outside of this range, provided that appropriate dilutions and
tion during manufacture, as well as to establish maximum
adjustments in specimen size are made.
unreacted monomer content for regulatory purposes.
1.2 The volatile composition of acrylic latexes is expected
to change with time and environmental factors. This time
5. Apparatus
dependence of the determination may be seen as an artificially
5.1 Gas Chromatograph, any gas-liquid chromatographic
large deviation of results, making the method mostly appli-
instrument having a flame ionization detector and linear
cableforin-housequalitycontrol,wheresamplingandanalysis
temperature programming. An injection port using replacable
conditions can be better controlled.
glass liners to facilitate periodic removal of accumulated
1.3 The values stated in inch-pound units are to be regarded
residues is recommended.
as the standard. The values given in parentheses are for
5.2 Column, 2 by 2-mm inside diameter glass or 6 ft by
information only.
1
⁄8-in. outside diameter steel tubing, packed with 10 % by
1.4 This standard does not purport to address all of the
weight of a 2-nitroterephthalic acid derivative of a synthetic
safety concerns, if any, associated with its use. It is the
polyester wax on 100/120 mesh acid washed, silane treated
responsibility of the user of this standard to establish appro-
4
diatomaceous earth. A column of equivalent or superior
priate safety and health practices and determine the applica-
performance may also be used.
bility of regulatory limitations prior to use. See Section 7 for
5.3 Recorder—A recording potentiometer with a full-scale
specific hazard statements.
deflection of 10 mV, a full-scale response time of 2 s or less,
and a maximum noise level of 60.03 % of full scale (see
2. Referenced Documents
Practice E 260).
2.1 ASTM Standards:
5.4 Liquid Charging Devices, microsyringe, 10-µL capacity
D 3980 Practice for Interlaboratory Testing of Paint and
2 or an automatic liquid sampling device.
Related Materials
3 5.5 Dropper Pipets, glass, disposable.
E 260 Practice for Packed Column Gas Chromatography
5.6 Vials,approximately7-mLcapacity,withcaps.Opentop
3. Summary of Test Method screw cap vials fitted with polytetrafluoroethylene/silicone
septa are preferred.
3.1 A suitable aliquot of the latex is internally standardized
5.7 Autosampler Vials, 2-mL capacity (optional).
with isobutyl acrylate, diluted with water, and then injected
5.8 Analytical Balance, accurate to 0.1 mg.
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved Jan. 10, 2002. Published March 2002.Originally
{1
published as D 4747 - 87. Last previous edition D 4747 - 87 (1996) .
2 4
Discontinued—See1999 Annual Book of ASTM Standards. Columns prepared from the stationary phases and supports have been found
3
Annual Book of ASTM Standards, Vol 03.06. suitable for this purpose and are available from scientific supply houses.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D4747
TABLE 1 Instrument Conditions
and maintain at 220°C overnight. In no case should the
Detector flame ionization temperat
...

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