ASTM D4457-85(1996)e1
(Test Method)Standard Test Method for Determination of Dichloromethane and 1,1,1-Trichloroethane in Paints and Coatings by Direct Injection into a Gas Chromatograph
Standard Test Method for Determination of Dichloromethane and 1,1,1-Trichloroethane in Paints and Coatings by Direct Injection into a Gas Chromatograph
SCOPE
1.1 This test method covers the determination of total amount of dichloromethane or 1,1,1-trichloroethane, or both, in paints and coatings. It has been evaluated for cellulose nitrate, alkyd, vinyl, and styrene-butadiene systems. It has not yet been evaluated for other formulations, but is believed to be applicable. The established working range of this test method is from 31 to 65 % for 1,1,1-trichloroethane and 32 to 78 % for dichloromethane. There is no reason to believe it will not work outside of these ranges. The presence of 1-propanol in paints and coatings requires the use of a different internal standard. (See also Practice E 260.)
1.2 The values stated in inch-pound units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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. Specific hazard statements are given in Section 7.
General Information
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e1
Designation: D 4457 – 85 (Reapproved 1996)
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Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Determination of Dichloromethane and 1,1,1-Trichloroethane
in Paints and Coatings by Direct Injection into a Gas
Chromatograph
This standard is issued under the fixed designation D4457; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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 other volatile compounds.
1.1 This test method covers the determination of total
4. Significance and Use
amountofdichloromethaneor1,1,1-trichloroethane,orboth,in
4.1 Use of 1,1,1-trichloroethane and dichloromethane,
paints and coatings. It has been evaluated for cellulose nitrate,
whichdonotmeasurablycontributetotheatmosphericoxidant
alkyd,vinyl,andstyrene-butadienesystems.Ithasnotyetbeen
level, is a way for industry to meet government or other
evaulated for other formulations, but is believed to be appli-
regulations on volatile organic compounds.This test method is
cable. The established working range of this test method is
designed to determine the content of these halohydrocarbon
from 31 to 65% for 1,1,1-trichloroethane and 32 to 78% for
solvents in paints and coatings. That content can subsequently
dichloromethane.Thereisnoreasontobelieveitwillnotwork
beusedincalculatingthevolatileorganiccompoundcontentof
outside of these ranges. The presence of 1-propanol in paints
a coating.
and coatings requires the use of a different internal standard.
(See also Practice E260.)
5. Apparatus
1.2 The values stated in inch-pound units are to be regarded
5.1 Chromatograph,anygas-liquidchromatographicinstru-
as the standard. The values given in parentheses are for
ment equipped with a thermal conductivity detector and
information only.
capable of being temperature programmed (see Table 1).
1.3 This standard does not purport to address all of the
Optionally, a flame ionization detector may be used if the
safety concerns, if any, associated with its use. It is the
sample is diluted so that no more than 1000 ppm each of
responsibility of the user of this standard to establish appro-
dichloromethane and 1,1,1-trichloroethane is present in the
priate safety and health practices and determine the applica-
injected specimen.
bility of regulatory limitations prior to use. Specific hazard
5.2 Recorder, a recording potentiometer with a full-scale
statements are given in Section 7.
deflection of 10 mV, a full-scale response time of 2 s or less,
2. Referenced Documents and a maximum noise of60.03% of full scale.
5.3 Pre-Column, 40 in. (100 mm) long by ⁄8 in. (3.2 mm)
2.1 ASTM Standards:
outside diameter stainless steel, packed with glass wool, fitted
E180 Practice for Determining the Precision of ASTM
2 on the entrance end of the column to retain any nonvolatile
Methods forAnalysis andTesting of Industrial Chemicals
materials and minimize sludge buildup in the column.
E260 Practice for Packed Column Gas Chromatography
5.4 Column, 4 ft (1.22 m) long by ⁄8 in. (3.2 mm) outside
3. Summary of Test Method diameter stainless steel, packed with 80/100 mesh (150 to 180
µm) porous polymer packing material, or other suitable
3.1 Anhydrous 1-propanol (see 10.5) is added as an internal
material.
standard to suitable aliquot of the whole paint. The aliquot is
5.5 LiquidChargingDevices,suchasmicrosyringesof5-µL
then diluted with dimethylformamide and injected onto a gas
or 10-µL capacity, cleaned with acetone or other suitable
chromatographiccolumncontainingaporouspolymerpacking
solvent. Visually inspect for plugs or cracks before and after
that separates dichloromethane and 1,1,1-trichloroethane from
each injection.
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paint and Paint Materials.
Current edition approved July 16, 1985. Published October 1985.
2 4
Annual Book of ASTM Standards, Vol 15.05. Porapak Rt, available from Waters Associates, Inc., Milford, MA, has been
Annual Book of ASTM Standards, Vol 14.02. found satisfactory for this purpose.
COPYRIGHT American Society for Testing and MaterialsCOPYRIGHT American Society for Testing and Materials
Licensed by Information Handling ServicesLicensed by Information Handling Services
TABLE 1 Typical Instrument Conditions
of the detector with the column bleed. Set the helium flow rate
Detector thermal conductivity at 30 mL/min if a ⁄8 in. (3.2 mm) outside diameter column is
Column 4 ft (1.22 m) by ⁄8in. (3.2 mm) outside
used. Purge the column 5 to 10 min before heating. Heat the
diameter packed with 80–100 mesh
column from room temperature to 200°C at 5°C/min and hold
porous polymer packing
Temperature, °C this temperature for at least 12 h (overnight).At the end of this
Injection port 200
periodoftime,heatthecolumnto240°Cata5°C/minrateand
Detector block 250
hold this temperature for several hours. The maximum tem-
Column
Initial 100
perature for this packing is 250°C. Cool the column to 100°C
Final 230 (for 8 min)
and reheat to 240°C at 5°C/min to observe the column bleed.
°C/min 8
Optimum conditioning of this column may take several cycles
Carrier gas helium
Flow rate, mL/min 30 of the heating program before a good recorder baseline is
Specimen size, µL 1
achieved. Conditioning of any column other than that sug-
gested (5.4) should be in accordance with the manufacturer’s
recommendations.
5.6 Vials, 25-mL to minimize head space, capable of being
8.2 Install the column in the chromatograph and use the
septum sealed.
information in Table 1 as a guide to establish the conditions
6. Reagents and Materials
required to give the desired separation. Allow sufficient time
for the instrument to reach equilibrium as indicated by a stable
6.1 Purity of Reagents—Reagent grade chemicals shall be
recorderbaseline.Adjustthecarrier-gasflowtoaconstantrate.
used in all tests, unless otherwise specified (as in 6.7). Unless
Before each calibration and series of determinations (or daily),
otherwise indicated, it is intended that all reagents shall
condition the column at 200°C for 1 h with carrier-gas flow.
conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society, where such
9. Calibration
specifications are available. Other grades may be used pro-
9.1 Preparation of Standards—All standards, as well as
vided it is first ascertained that the reagent is of sufficient high
samples and blanks, should be at a constant temperature. The
purity to permit its use without lessening the accuracy of the
given order of ingredient addition should be observed to
determination.
minimize loss of volatile ingredients.
6.2 Carrier Gas, helium of 99.995% or higher purity. High
9.1.1 Weighingto1.0mg,add16.0gofdimethylformamide
purity nitrogen may also be used.
to a vial capable of being septum sealed. Add 2.0 g of
6.3 Dimethylformamide (DMF), reagent grade.
1,1,1-trichloroethane, 2.0 g of 1-propanol (see 10.5) and 2.0 g
6.4 1-Propanol, gas chromatography spectrophotometric
of dichloromethane. Seal the vial with a crimp-on or septum
quality (see 10.5).
seal.
6.5 1,1,1-Trichloroethane (see 6.7).
9.2 Determine the retention time of each component by
6.6 Dichloromethane (see 6.7).
injecting small amounts either separately or in known mix-
6.7 Halogenated Hydrocarbon Stabilizers—Allcommercial
tures. The components should elute close to the typical
grades of these halogenated hydrocarbons contain stabilizers.
retentiontimesgiveninTable1andthechromatogramsshould
Eitherobtainthesamesolventusedinthecoatingforuseasthe
closely approximate those shown in
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