ASTM D4827-93(1998)
(Test Method)Standard Test Method for Determining the Unreacted Monomer Content of Latexes Using Capillary Column Gas Chromatography
Standard Test Method for Determining the Unreacted Monomer Content of Latexes Using Capillary Column Gas Chromatography
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 -butyl methacrylate, -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 [mu]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 This standard does not purport to address all of the safety problems, 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
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D4827–93 (Reapproved l998)
Standard Test Method for
Determining the Unreacted Monomer Content of Latexes
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 stationary phase that separates the internal standard and mono-
mers in question from each other and from other volatile
1.1 This test method is for the determination of the unre-
compounds.
acted monomer content of acrylic latexes. Monomers that have
beensuccessfullydeterminedbythisprocedureinclude n-butyl
4. Significance and Use
methacrylate, n-butyl acrylate, styrene, and methyl methacry-
4.1 Excessive amounts of unreacted monomer may cause
late. The determination of other monomers has not been
concerns relating to toxicity and odor. This test method is
evaluated,butthistestmethodisbelievedtobeapplicable.The
designedtomeasuretheunreactedmonomercontentoflatexes.
established working range of this test method is from 100 to
The results may be used to monitor the extent of polymeriza-
1000 µg/g, but there is no reason to believe it will not work
tion during manufacture, as well as to establish maximum
outside of this range, provided that appropriate dilutions and
unreacted monomer content for regulatory purposes.
adjustments in specimen size are made.
1.2 The unreacted monomer in acrylic latexes is expected to
5. Apparatus
change with time and environmental factors. This time depen-
5.1 Gas Chromatograph—Any gas-liquid chromatographic
dence of the determination may be seen as an artificially large
instrument having a flame ionization detector and linear
deviation of results, making the test method mostly applicable
temperature programming and a capillary column inlet capable
for in-house quality control, where sampling and analysis
of split operation.The split liner should be constructed of glass
conditions can be better controlled.
andbereplacedorcleanedasneeded.On-columninjectioninto
1.3 This standard does not purport to address all of the
a wide bore capillary column was not evaluated but is expected
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-
5.2 Column—30-m by 0.25-mm inside diameter fused silica
priate safety and health practices and determine the applica-
coated witha1µm thick film of a phenyl methyl silicone
bility of regulatory limitations prior to use. For specific hazard
polymer. A bonded phase is preferred. Other columns having
statements, see Section 7.
equivalent or superior performance may also be used.
5.3 Recorder—A recording potentiometer with a full-scale
2. Referenced Documents
deflection of 10 mV, a full-scale response time of 2 s or less,
2.1 ASTM Standards:
2 and a maximum noise level of 60.03 % of full scale. The use
D 1193 Specification for Reagent Water
of a recording integrator or other data-handling device is
3. Summary of Test Method preferred.
5.4 Liquid Charging Devices—A microsyringe, 1.0-µL ca-
3.1 A suitable aliquot of the latex is internally standardized
pacity, or an automatic liquid sampling device using a suitable
with isobutyl acrylate, diluted with water, and then injected
syringe and appropriate change in split ratio.
onto a capillary gas chromatographic column containing a
5.5 Dropper Pipettes, glass, disposable.
5.6 Vials,approximately7mLcapacity,withcaps.Opentop
This test method is under the jurisdiction of ASTM Committee D-1 on Paint screw-cap vials fitted with PTFE/silicone septa are preferred.
and Related Coatings, Materials, andApplications and is the direct responsibility of
5.7 Autosampler Vials, 2 mL capacity (optional).
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
5.8 Analytical Balance, accurate to 0.1 mg.
Current edition approved May 15, 1993. Published July 1993. Originally
published as D 4827 – 88. Last previous edition D 4827 – 88.
Annual Book of ASTM Standards, Vol 11.01.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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.
D4827
TABLE 1 Instrument Conditions
6. Reagents
Detector flame ionization
6.1 Purity of Reagents—Reagent grade chemicals shall be
A
Airflow, mL/min 240
used in all tests. Unless otherwise indicated, it is intended that
Hydrogen flow, mL/min 30
Makeup gas 30
all reagents shall conform to the specifications of the Commit-
Helium
tee onAnalytical Reagents of theAmerican Chemical Society,
B
Column:
where such specifications are available. Other grades may be
Length, m 30
used, provided it is first ascertained that the reagent is of Inside diameter, mm 0.25
Film thickness, µm 1
sufficiently high purity to permit its use without lessening the
Carrier gas helium
accuracy of the determination.
Flow rate 0.5 mL/min
Temperatures:
6.2 Purity of Water—Unless otherwise indicated, references
Injection port, °C 220
to water shall be understood to mean reagent water as defined
Detector block, °C 250
by Type II of Specification D 1193.
Column:
Initial, °C 60
6.3 Carrier Gas—Helium of 99.995 % or higher purity.
Hold time, min 4
High purity nitrogen may also be used.
Program rate, °C/min 8
6.4 Acetone.
Final, °C 200 (or higher as needed)
Final hold, min 10 (or longer)
6.5 Isobutyl Acrylate (internal standard), 99 + % pure.
Injection volume, µL 0.5
Split ratio 20:1
NOTE 1—Isobutyl acrylate was found to be a suitable internal standard,
A
but any other monomer not found in the sample may be substituted. The
Set at recommended flow according to the instrument manufacturer.
B
internal standard chosen should yield a clear chromatographic separation,
Cross-linked 50 % phenyl 50 % methyl silicone. A column of equivalent or
better performance may also be used.
and should be free of interferences.
6.6 Monomers of Interest, 99+ % pure.
6.7 Methanol.
9.2.1 Weigh to within 0.1 mg about 0.05 g of isobutyl
7. Hazards
acrylate and each monomer of interest into a vial (see 5.6).
Weigh approximately5gof acetone into the vial and mix well.
7.1 Acrylic and methacrylic monomers are considered haz-
9.2.2 Weigh approximately 0.05 g of the solution prepared
ardous. All sample preparations should be done in a well
in 9.2.1 into another vial, add approximately5gof acetone,
ventilated area, such as a fume hood.
and mix well.
8. Preparation of Apparatus
9.2.3 Inject a 0.5-µL aliquot of the solution from 9.2.2 onto
thecolumnandrecordthechromatogram.Theelutionorderfor
8.1 Column Conditioning—Attach one end of the column to
acetone and each of the monomers using the conditions given
the inlet side of the instrument leaving the exit end of the
in Table 1 is shown in Fig. 1.
column disconnected. This prevents the contamination of the
9.2.4 Measure the peak areas of the individual components
detector due to column bleed. Set the helium flow rate at 0.5
and calculate the relative response factor, RF, for the mono-
mL/min (approximately equivalent to a linear velocity of 20
mers of interest as follows:
cm/s) and purge the column at 220°C for 1 h.
8.2 Afterco
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