ASTM D4747-87(1996)e1

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
e1
Designation: D 4747 – 87 (Reapproved 1996)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Determining Unreacted Monomer Content of Latexes Using
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.
e NOTE—Unit of measurement statement added to the Scope Section editorially in May 1997.
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, but this test method is believed to be applicable. The
concerns relating to toxicity and odor. This test method is
established working range of this test method is from 100 to
designed to measure the unreacted monomer content of latexes.
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
cable for in-house quality control, where sampling and analysis
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.
⁄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-
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 of2sor less,
2. Referenced Documents and a maximum noise level of 60.03 % of full scale (see
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, approximately 7-mL capacity, with caps. Open top
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.
6. Reagents
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, and Applications and is the direct responsibility of
6.1 Purity of Reagents—Reagent grade chemicals shall be
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved Nov. 27, 1987. Published January 1988.
2 4
Annual Book of ASTM Standards, Vol 06.01. Columns prepared from the stationary phases and supports have been found
Annual Book of ASTM Standards, Vol 14.02. suitable for this purpose and are available from scientific supply houses.
D 4747
TABLE 1 Instrument Conditions
min. Program the column oven from 50 to 220°C at 2°C/min
Detector flame ionization and maintain at 220°C overnight. In no case should the
Air flow 240 mL/min
temperature of the column be allowed to exceed 275°C.
Hydrogen flow 30 mL/min
8.2 After conditioning, connect the exit end of the column to
Column (suggested) 2 by 2 mm inside diameter glass, packed with
10 % the detector and establish the operating conditions required to
of a 2-nitroterephthalic acid derivative of Carbo-
give the desired separation (see Table 1). Allow sufficient time
wax 20M on 100/120 mesh acid washed, silane-
for the instrument to reach equilibrium as indicated by a stable
treated diatomaceous earth.
Carrier gas, flow rate Helium, 30 mL/min
baseline. Control the detector temperature so that is is constant
Temperatures:
to within 1°C without thermostat cycling which causes an
uneven baseline. Adjust the carrier gas flow rate to a constant
Injection port 250°C
Detector block 250°C
value.
Column
9. Calibration
Initial 80°C
9.1 Determine the retention of each component expected to
Hold time 4 min
Program rate 8°C/min
be present by injecting small amounts either separately or in
Final 200°C, or higher as needed (see 8.1)
known mixtures. Retention times should be determined each
Final hold 10 min, or as needed
day the method is used.
Injection volume 2 μL
9.2 Standardization—Determine in duplicate the relative
response of the monomers of interest to the isobutyl acrylate
used in all tests. Unless otherwise indicated, it is intended that
internal standard as follows:
all reagents shall conform to the specifications of the Commit-
9.2.1 Weigh to 0.1 mg about 0.05 g of isobutyl acrylate and
tee on Analytical Reagents of the American Chemical Society,
each monomer of interest into a vial (5.6). Weigh approxi-
where such specifications are available. Other grades may be
mately5gof acetone into the vial and mix well.
used, provided it is first ascertained that the reagent is of
9.2.2 Weigh approximately 0.05 g of the solution (9.2.1)
sufficiently high purity to permit its use without lessening the
into another vial, add approximately5gof acetone and mix
accuracy of the determination.
well.
6.2 Carrier Gas, helium of 99.995 % or higher purity. High
9.2.3 Inject a 1-μL aliquot of the solution from 9.2.2 onto
purity nitrogen may also be used.
the column and record the chromatogram. The elution order for
6.3 Acetone, reagent grade.
acetone and each of the monomers using the conditions given
6.4 Isobutyl Acrylate (internal standard), 99+ % pure.
in Table 1 is shown in Fig. 1.
NOTE 1—Isobutyl acrylate was found to be a suitable internal st
...