ASTM D4457-02(2008)
(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
SIGNIFICANCE AND USE
Use of 1,1,1-trichloroethane and dichloromethane, which do not measurably contribute to the atmospheric oxidant level, is a way for industry to meet government or other regulations on volatile organic compounds. This test method is designed to determine the content of these halohydrocarbon solvents in paints and coatings. That content can subsequently be used in calculating the volatile organic compound content of a coating.
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.
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Designation: D4457 − 02 (Reapproved2008)
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 D4457; 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 Anhydrous 1-propanol (see 10.5) is added as an internal
1.1 This test method covers the determination of total
amountofdichloromethaneor1,1,1-trichloroethane,orboth,in standard to suitable aliquot of the whole paint. The aliquot is
then diluted with dimethylformamide and injected onto a gas
paints and coatings. It has been evaluated for cellulose nitrate,
alkyd,vinyl,andstyrene-butadienesystems.Ithasnotyetbeen chromatographic column containing a porous polymer packing
that separates dichloromethane and 1,1,1-trichloroethane from
evaluated for other formulations, but is believed to be appli-
cable. The established working range of this test method is other volatile compounds.
from 31 to 65 % for 1,1,1-trichloroethane and 32 to 78 % for
4. Significance and Use
dichloromethane.There is no reason to believe it will not work
outside of these ranges. The presence of 1-propanol in paints
4.1 Use of 1,1,1-trichloroethane and dichloromethane,
and coatings requires the use of a different internal standard.
which do not measurably contribute to the atmospheric oxidant
(See also Practice E260.)
level, is a way for industry to meet government or other
regulations on volatile organic compounds. This test method is
1.2 The values stated in inch-pound units are to be regarded
designed to determine the content of these halohydrocarbon
as the standard. The values given in parentheses are for
solvents in paints and coatings. That content can subsequently
information only.
beusedincalculatingthevolatileorganiccompoundcontentof
1.3 This standard does not purport to address all of the
a coating.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Apparatus
priate safety and health practices and determine the applica-
5.1 Chromatograph, any gas-liquid chromatographic instru-
bility of regulatory limitations prior to use. Specific hazard
ment equipped with a thermal conductivity detector and
statements are given in Section 7.
capable of being temperature programmed (see Table 1).
Optionally, a flame ionization detector may be used if the
2. Referenced Documents
sample is diluted so that no more than 1000 ppm each of
2
2.1 ASTM Standards:
dichloromethane and 1,1,1-trichloroethane is present in the
E180 Practice for Determining the Precision of ASTM
injected specimen.
Methods for Analysis and Testing of Industrial and Spe-
5.2 Recorder, a recording potentiometer with a full-scale
3
cialty Chemicals (Withdrawn 2009)
deflection of 10 mV, a full-scale response time of 2 s or less,
E260 Practice for Packed Column Gas Chromatography
and a maximum noise of 60.03 % of full scale.
1
5.3 Pre-Column, 40 in. (100 mm) long by ⁄8 in. (3.2 mm)
outside diameter stainless steel, packed with glass wool, fitted
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
on the entrance end of the column to retain any nonvolatile
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials. materials and minimize sludge buildup in the column.
Current edition approved Feb. 1, 2008. Published March 2008. Originally
1
5.4 Column, 4 ft (1.22 m) long by ⁄8 in. (3.2 mm) outside
approved in 1985. Last previous edition approved in 2002 as D4457 - 02. DOI:
10.1520/D4457-02R08. diameter stainless steel, packed with 80/100 mesh (150 to
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
180 µm) porous polymer packing material, or other suitable
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
3 4
The last approved version of this historical standard is referenced on Porapak R, a registered trademark ofWatersAssociates, Inc., Milford, MA, has
www.astm.org. been found satisfactory for this purpose.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D4457 − 02 (Reapproved2008)
material.
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D4457 − 02 (2008)
TABLE 1 Typica
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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.
e1
Designation:D4457–85 (Reapproved 1996)
Designation: D 4457 – 02 (Reapproved 2008)
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
e NOTE—Unit of measurement statement added to the Scope Section editorially in May 1997.
1. 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
evaulatedevaluated 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.
2. Referenced Documents
2
2.1 ASTM Standards:
E 180 Practice for Determining the Precision ofASTM Methods forAnalysis andTesting of Industrial and Specialty Chemicals
E 260 Practice for Packed Column Gas Chromatography
3. Summary of Test Method
3.1 Anhydrous 1-propanol (see 10.5) is added as an internal standard to suitable aliquot of the whole paint. The aliquot is then
diluted with dimethylformamide and injected onto a gas chromatographic column containing a porous polymer packing that
separates dichloromethane and 1,1,1-trichloroethane from other volatile compounds.
4. Significance and Use
4.1 Use of 1,1,1-trichloroethane and dichloromethane, which do not measurably contribute to the atmospheric oxidant level, is
a way for industry to meet government or other regulations on volatile organic compounds. This test method is designed to
determine the content of these halohydrocarbon solvents in paints and coatings. That content can subsequently be used in
calculating the volatile organic compound content of a coating.
5. Apparatus
5.1 Chromatograph, any gas-liquid chromatographic instrument equipped with a thermal conductivity detector and capable of
being temperature programmed (see Table 1). Optionally, a flame ionization detector may be used if the sample is diluted so that
no more than 1000 ppm each of dichloromethane and 1,1,1-trichloroethane is present in the injected specimen.
1
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
Subcommittee D01.21 on Chemical Analysis of Paint and Paint Materials.
Current edition approved July 16, 1985. Published October 1985.
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 Feb. 1, 2008. Published March 2008. Originally approved in 1985. Last previous edition approved in 2002 as D 4457 - 02.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 15.05.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 ----------------------
D 4457 – 02 (2008)
TABLE 1 Typical Instrument Conditions
Detector thermal conductivity
1
Column 4 ft (1.22 m) by ⁄8 in. (3.2 mm) outside
diameter packed with 80–100 mesh
porous polymer packing
Temperature, °C
Injection
...
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