ASTM D4457-02

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D 4457 – 02
Standard Test Method for
Determination of Dichloromethane and 1,1,1-Trichloroethane
in Paints and Coatings by Direct Injection into a Gas
1
Chromatograph
This standard is issued under the fixed designation D 4457; 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 chromatographic column containing a porous polymer packing
that separates dichloromethane and 1,1,1-trichloroethane from
1.1 This test method covers the determination of total
other volatile compounds.
amountofdichloromethaneor1,1,1-trichloroethane,orboth,in
paints and coatings. It has been evaluated for cellulose nitrate,
4. Significance and Use
alkyd,vinyl,andstyrene-butadienesystems.Ithasnotyetbeen
4.1 Use of 1,1,1-trichloroethane and dichloromethane,
evaluated for other formulations, but is believed to be appli-
which do not measurably contribute to the atmospheric oxidant
cable. The established working range of this test method is
level, is a way for industry to meet government or other
from 31 to 65 % for 1,1,1-trichloroethane and 32 to 78 % for
regulations on volatile organic compounds. This test method is
dichloromethane.There is no reason to believe it will not work
designed to determine the content of these halohydrocarbon
outside of these ranges. The presence of 1-propanol in paints
solvents in paints and coatings. That content can subsequently
and coatings requires the use of a different internal standard.
beusedincalculatingthevolatileorganiccompoundcontentof
(See also Practice E 260.)
a coating.
1.2 The values stated in inch-pound units are to be regarded
as the standard. The values given in parentheses are for
5. Apparatus
information only.
5.1 Chromatograph, any gas-liquid chromatographic instru-
1.3 This standard does not purport to address all of the
ment equipped with a thermal conductivity detector and
safety concerns, if any, associated with its use. It is the
capable of being temperature programmed (see Table 1).
responsibility of the user of this standard to establish appro-
Optionally, a flame ionization detector may be used if the
priate safety and health practices and determine the applica-
sample is diluted so that no more than 1000 ppm each of
bility of regulatory limitations prior to use. Specific hazard
dichloromethane and 1,1,1-trichloroethane is present in the
statements are given in Section 7.
injected specimen.
5.2 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:
and a maximum noise of 60.03 % of full scale.
E 180 Practice for Determining the Precision of ASTM
1
2 5.3 Pre-Column, 40 in. (100 mm) long by ⁄8 in. (3.2 mm)
Methods forAnalysis and Testing of Industrial Chemicals
3 outside diameter stainless steel, packed with glass wool, fitted
E 260 Practice for Packed Column Gas Chromatography
on the entrance end of the column to retain any nonvolatile
3. Summary of Test Method materials and minimize sludge buildup in the column.
1
5.4 Column, 4 ft (1.22 m) long by ⁄8 in. (3.2 mm) outside
3.1 Anhydrous 1-propanol (see 10.5) is added as an internal
diameter stainless steel, packed with 80/100 mesh (150 to 180
standard to suitable aliquot of the whole paint. The aliquot is
4
µm) porous polymer packing material, or other suitable
then diluted with dimethylformamide and injected onto a gas
material.
5.5 Liquid Charging Devices,suchasmicrosyringesof5-µL
or 10-µL capacity, cleaned with acetone or other suitable
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
solvent. Visually inspect for plugs or cracks before and after
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paint and Paint Materials. each injection.
Current edition approved Jan. 10, 2002. Published March 2002. Originally
{1
published as D 4457 - 85. Last previous edition D 4457 - 85 (1996) .
2 4
Annual Book of ASTM Standards, Vol 15.05. Porapak Rt, available from Waters Associates, Inc., Milford, MA, has been
3
Annual Book of ASTM Standards, Vol 14.02. found satisfactory for this purpose.
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D 4457
TABLE 1 Typical Instrument Conditions
nected from the detector. This will prevent any contamination
Detector thermal conductivity of the detector with the column bleed. Set the helium flow rate
1
Column 4 ft (1.22 m) by ⁄8in. (3.2 mm) outside
1
at
...