ASTM D4827-03(2009)

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 μ 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 standard. No other units of measurement are included in this standard.
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: 31-Jan-2009
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.21 - Chemical Analysis of Paints and Paint Materials

Relations

• Replaces: ASTM D4827-03 - 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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(Reapproved 2009)
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 D4827; 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 3. Summary of Test Method
3.1 A suitable aliquot of the latex is internally standardized
1.1 This test method is for the determination of the unre-
with isobutyl acrylate, diluted with water, and then injected
acted monomer content of acrylic latexes. Monomers that have
onto a capillary gas chromatographic column containing a
beensuccessfullydeterminedbythisprocedureinclude n-butyl
stationary phase that separates the internal standard and mono-
methacrylate, n-butyl acrylate, styrene, and methyl methacry-
mers in question from each other and from other volatile
late. The determination of other monomers has not been
compounds.
evaluated,butthistestmethodisbelievedtobeapplicable.The
established working range of this test method is from 100 to
4. Significance and Use
1000 µg/g, but there is no reason to believe it will not work
outside of this range, provided that appropriate dilutions and
4.1 Excessive amounts of unreacted monomer may cause
adjustments in specimen size are made.
concerns relating to toxicity and odor. This test method is
designedtomeasuretheunreactedmonomercontentoflatexes.
1.2 The unreacted monomer in acrylic latexes is expected to
The results may be used to monitor the extent of polymeriza-
change with time and environmental factors. This time depen-
tion during manufacture, as well as to establish maximum
dence of the determination may be seen as an artificially large
unreacted monomer content for regulatory purposes.
deviation of results, making the test method mostly applicable
for in-house quality control, where sampling and analysis
5. Apparatus
conditions can be better controlled.
5.1 Gas Chromatograph—Any gas-liquid chromatographic
1.3 The values stated in SI units are to be regarded as
instrument having a flame ionization detector and linear
standard. No other units of measurement are included in this
temperature programming and a capillary column inlet capable
standard.
of split operation.The split liner should be constructed of glass
andbereplacedorcleanedasneeded.On-columninjectioninto
1.4 This standard does not purport to address all of the
awideborecapillarycolumnwasnotevaluatedbutisexpected
safety concerns, if any, associated with its use. It is the
to also be satisfactory for this procedure.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5.2 Column—30-m by 0.25-mm inside diameter fused silica
bility of regulatory limitations prior to use. For specific hazard
coated witha1µm thick film of a phenyl methyl silicone
statements, see Section 7.
polymer. A bonded phase is preferred. Other columns having
equivalent or superior performance may also be used.
2. Referenced Documents
5.3 Recorder—A recording potentiometer with a full-scale
2
2.1 ASTM Standards: deflection of 10 mV, a full-scale response time of 2 s or less,
D1193 Specification for Reagent Water
and a maximum noise level of 60.03 % of full scale. The use
of a recording integrator or other data-handling device is
preferred.
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint 5.4 Liquid Charging Devices—A microsyringe, 1.0-µL
and Related Coatings, Materials, andApplications and is the direct responsibility of
capacity, or an automatic liquid sampling device using a
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
suitable syringe and appropriate change in split ratio.
Current edition approved Feb. 1, 2009. Published February 2009. Originally
approved in 1988. Last previous edition approved in 2003 as D4827 – 03. DOI:
5.5 Dropper Pipettes, glass, disposable.
10.1520/D4827-03R09.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 5.6 Vials,approximately7mLcapacity,withcaps.Opentop
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
screw-cap vials fitted with PTFE/silicone septa are preferred.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 5.7 Autosampler Vials, 2 mL capacity (optional).
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D4827 − 03 (2009)
TABLE 1 Instrument Conditions
5.8 Analytical Balance, ac
...

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:D4827–03 Designation:D4827–03(Reapproved2009)
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 (´) indicates an editorial change since the last revision or reapproval.
1. 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
determinationofothermonomershasnotbeenevaluated,butthistestmethodisbelievedtobeapplicable.Theestablishedworking
range of this test method is from 100 to 1000 µ 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.
1.3The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
3. Summary of Test Method
3.1 A suitable aliquot of the latex is internally standardized with isobutyl acrylate, diluted with water, and then injected onto
a capillary gas chromatographic column containing a stationary phase that separates the internal standard and monomers in
question from each other and from other volatile compounds.
4. Significance and Use
4.1 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.
5. Apparatus
5.1 Gas Chromatograph—Any gas-liquid chromatographic instrument having a flame ionization detector and linear tempera-
ture programming and a capillary column inlet capable of split operation. The split liner should be constructed of glass and be
replaced or cleaned as needed. On-column injection into a wide bore capillary column was not evaluated but is expected to also
be satisfactory for this procedure.
5.2 Column—30-m by 0.25-mm inside diameter fused silica coated witha1µm thick film of a phenyl methyl silicone polymer.
A bonded phase is preferred. Other columns having equivalent or superior performance may also be used.
5.3 Recorder—A recording potentiometer with a full-scale deflection of 10 mV, a full-scale response time of2sor less, and
a maximum noise level of 60.03 % of full scale. The use of a recording integrator or other data-handling device is preferred.
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved Dec.Feb. 1, 2003.2009. Published January 2004.February 2009. Originally approved in 1988. Last previous edition approved in 19932003 as
D4827–93(1998). D 4827 – 03.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ---------------
...

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:D4827–93 (Reapproved l998) Designation:D4827–03(Reapproved2009)
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 (´) indicates an editorial change since the last revision or reapproval.
1. 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
determinationofothermonomershasnotbeenevaluated,butthistestmethodisbelievedtobeapplicable.Theestablishedworking
range of this test method is from 100 to 1000 µ 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
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
3. Summary of Test Method
3.1 A suitable aliquot of the latex is internally standardized with isobutyl acrylate, diluted with water, and then injected onto
a capillary gas chromatographic column containing a stationary phase that separates the internal standard and monomers in
question from each other and from other volatile compounds.
4. Significance and Use
4.1 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.
5. Apparatus
5.1 Gas Chromatograph—Any gas-liquid chromatographic instrument having a flame ionization detector and linear tempera-
ture programming and a capillary column inlet capable of split operation. The split liner should be constructed of glass and be
replaced or cleaned as needed. On-column injection into a wide bore capillary column was not evaluated but is expected to also
be satisfactory for this procedure.
5.2 Column—30-m by 0.25-mm inside diameter fused silica coated witha1µm thick film of a phenyl methyl silicone polymer.
A bonded phase is preferred. Other columns having equivalent or superior performance may also be used.
5.3 Recorder—A recording potentiometer with a full-scale deflection of 10 mV, a full-scale response time of2sor less, and
a maximum noise level of 60.03 % of full scale. The use of a recording integrator or other data-handling device is preferred.
1
This test method is under the jurisdiction of ASTM Committee D-1D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved May 15, 1993.Feb. 1, 2009. Published July 1993.February 2009. Originally published as D4827–88.approved in 1988. Last previous edition
D4827–88.approved in 2003 as D 4827 – 03.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D4827–03 (2009)
5.4 Liquid Charging Devices—Amicrosyringe, 1.0-µLcapa
...