ASTM D4827-03

Standard Test Method for Determining the Unreacted Monomer Content of Latexes Using Capillary Column Gas 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 is for the determination of the unreacted 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 g/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 unreacted monomer in 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 test method mostly applicable for in-house quality control, where sampling and analysis conditions can be better controlled.
1.3 The values stated in SI 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. For specific hazard statements, see Section 7.

General Information

• Status: Historical
• Publication Date: 30-Nov-2003
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.21 - Chemical Analysis of Paints and Paint Materials

Relations

• Replaces: ASTM D4827-93(1998) - Standard Test Method for Determining the Unreacted Monomer Content of Latexes Using Capillary Column Gas Chromatography
• Effective Date: 01-Dec-2003
• Replaced By: ASTM D4827-03(2009) - Standard Test Method for Determining the Unreacted Monomer Content of Latexes Using Capillary Column Gas Chromatography
• Effective Date: 01-Feb-2009

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:D4827–03
Standard Test Method for
Determining the Unreacted Monomer Content of Latexes
1
Using Capillary Column Gas Chromatography
This standard is issued under the fixed designation D 4827; 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 onto a capillary gas chromatographic column containing a
stationary phase that separates the internal standard and mono-
1.1 This test method is for the determination of the unre-
mers in question from each other and from other volatile
acted monomer content of acrylic latexes. Monomers that have
compounds.
beensuccessfullydeterminedbythisprocedureinclude 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 unreacted monomer in acrylic latexes is expected to
change with time and environmental factors. This time depen-
5. Apparatus
dence of the determination may be seen as an artificially large
5.1 Gas Chromatograph—Any gas-liquid chromatographic
deviation of results, making the test method mostly applicable
instrument having a flame ionization detector and linear
for in-house quality control, where sampling and analysis
temperature programming and a capillary column inlet capable
conditions can be better controlled.
of split operation.The split liner should be constructed of glass
1.3 The values stated in SI units are to be regarded as the
andbereplacedorcleanedasneeded.On-columninjectioninto
standard. The values given in parentheses are for information
a wide bore capillary column was not evaluated but is expected
only.
to also be satisfactory for this procedure.
1.4 This standard does not purport to address all of the
5.2 Column—30-mby0.25-mminsidediameterfusedsilica
safety concerns, if any, associated with its use. It is the
coated witha1µm thick film of a phenyl methyl silicone
responsibility of the user of this standard to establish appro-
polymer. A bonded phase is preferred. Other columns having
priate safety and health practices and determine the applica-
equivalent or superior performance may also be used.
bility of regulatory limitations prior to use. For specific hazard
5.3 Recorder—A recording potentiometer with a full-scale
statements, see Section 7.
deflection of 10 mV, a full-scale response time of 2 s or less,
2. Referenced Documents and a maximum noise level of 60.03 % of full scale. The use
2 of a recording integrator or other data-handling device is
2.1 ASTM Standards:
preferred.
D 1193 Specification for Reagent Water
5.4 Liquid Charging Devices—A microsyringe, 1.0-µL ca-
3. Summary of Test Method pacity, or an automatic liquid sampling device using a suitable
syringe and appropriate change in split ratio.
3.1 A suitable aliquot of the latex is internally standardized
5.5 Dropper Pipettes, glass, disposable.
with isobutyl acrylate, diluted with water, and then injected
5.6 Vials,approximately7mLcapacity,withcaps.Opentop
screw-cap vials fitted with PTFE/silicone septa are preferred.
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
5.7 Autosampler Vials, 2 mL capacity (optional).
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 Dec. 1, 2003. Published January 2004. Originally
approved in 1988. Last previous edition approved in 1993 as D 4827 – 93 (1998).
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
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D4827–03
TABLE 1 Instrument Conditions
5.8 Analytical Balance, accurate to 0.1 mg.
Detector flame ioniza
...