Standard Test Method for Low-Molecular Weight Halogenated Hydrocarbons in Water

SIGNIFICANCE AND USE
The incidental conversion of organic material to trihalomethanes and other volatile organohalides during chlorination of water is a possible health hazard and is the object of much research. This test method can be used as a rapid, simple means for determining many volatile organohalides in raw and processed water.
SCOPE
1.1 This test method covers the analysis of drinking water. It is also applicable to many environmental and waste waters when adequate validation is included.
1.2 This test method covers the determination of halomethanes, haloethanes, and some related extractable organohalides amenable to gas chromatographic measurement. The applicable concentration range for trihalomethanes is from 1 to 200 g/L. Detection limits depend on the compound, matrix, and on the characteristics of the gas chromatographic system.
1.3 For compounds not specifically included in the precision and bias section the analyst should validate the test method by collecting precision and bias data on actual samples.
1.4 Confirmation of component identities is obtained by observing retention times using gas chromatographic columns of different polarities. When concentrations are sufficiently high (>50 μg/L) confirmation with halogen specific detectors or gas chromatography/mass spectrometry (GC/MS) may be used. Confirmation of purgeable compounds at levels down to 1 μg/L can be obtained using Test Method D 3871 with GC/MS detection.
1.5 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 precautionary statements are given in Section 8.

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Publication Date
09-Jan-2003
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ASTM D3973-85(2003) - Standard Test Method for Low-Molecular Weight Halogenated Hydrocarbons in Water
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D 3973–85 (Reapproved 2003)
Standard Test Method for
1
Low-Molecular Weight Halogenated Hydrocarbons in Water
This standard is issued under the fixed designation D 3973; 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 E 355 Practice for Gas Chromatography Terms and Rela-
4
tionships
1.1 This test method covers the analysis of drinking water.
It is also applicable to many environmental and waste waters
3. Terminology
when adequate validation is included.
3.1 Definitions—For definitions of terms used in this test
1.2 This test method covers the determination of halometh-
method, refer to Terminology D 1129 and Practice E 355.
anes, haloethanes, and some related extractable organohalides
amenable to gas chromatographic measurement. The appli-
4. Summary of Test Method
cable concentration range for trihalomethanes is from 1 to 200
4.1 This test method employs liquid/liquid extraction to
µg/L.Detectionlimitsdependonthecompound,matrix,andon
isolate compounds of interest and provide a five-fold concen-
the characteristics of the gas chromatographic system.
5,6 ,7
trationenhancementpriortomeasurement. A5-mLaqueous
1.3 Forcompoundsnotspecificallyincludedintheprecision
sample is extracted once with 1 mL of solvent. -µL aliquot of
and bias section the analyst should validate the test method by
the extract is analyzed in a gas chromatograph equipped with
collecting precision and bias data on actual samples.
an electron-capture detector.
1.4 Confirmation of component identities is obtained by
4.2 Extraction efficiencies with the 1:5 solvent/sample ratio
observing retention times using gas chromatographic columns
for trihalomethanes average above 90 %. To compensate for
of different polarities. When concentrations are sufficiently
extraction losses, calibration standards are extracted and ana-
high (>50 µg/L) confirmation with halogen specific detectors
lyzed in an identical manner.
or gas chromatography/mass spectrometry (GC/MS) may be
4.3 The concentration of each component is calculated and
used. Confirmation of purgeable compounds at levels down to
reported in micrograms per litre.
1µg/LcanbeobtainedusingTestMethodD 3871withGC/MS
detection.
5. Significance and Use
1.5 This standard does not purport to address all of the
5.1 The incidental conversion of organic material to triha-
safety concerns, if any, associated with its use. It is the
lomethanes and other volatile organohalides during chlorina-
responsibility of the user of this standard to establish appro-
tion of water is a possible health hazard and is the object of
priate safety and health practices and determine the applica-
much research.This test method can be used as a rapid, simple
bility of regulatory limitations prior to use. Specific precau-
means for determining many volatile organohalides in raw and
tionary statements are given in Section 8.
processed water.
2. Referenced Documents
6. Interferences
2.1 ASTM Standards:
6.1 Volatile compounds that are extractable and responsive
2
D 1129 Terminology Relating to Water
to electron-capture detection may interfere with this test
2
D 1193 Specification for Reagent Water
method.
D 3871 Test Method for Purgeable Organic Compounds in
3 6.2 Impurities in the extracting solvent can be a source of
Water Using Headspace Sampling
interference. Solvent blanks should be analyzed daily and
before a new bottle of solvent is used for the first time.
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
4
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor Annual Book of ASTM Standards, Vol 14.01.
5
Organic Substances in Water. Mieure, J. P., “A Rapid and Sensitive Method for Determining Volatile
Current edition approved Jan. 10, 2003. Published January 2003. Originally Organohalides in Water,” Journal AWWA, Vol 69, 1977, p. 60.
e1 6
approved in 1980. Last previous edition approved in 1995 as D 3973 – 85 (1995) Richard, J. J., and Junk, G. A., “Liquid Extraction for Rapid Determination of
. Halomethanes in Water,” Journal AWWA , Vol 69, 1977, p. 62.
2 7
Annual Book of ASTM Standards, Vol 11.01. “TheAnalysis of Trihalomethanes in Drinking Water by Liquid/Liquid Extrac-
3
Annual Book of ASTM Standards, Vol 11.02. tion,”U.S.EnvironmentalProtectionAgency,EMSL,Cincinnati,OH,Sept.9,1977.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D 3973–85 (2003)
FIG. 1 Chromatograms of Standards
Whenever interfering compounds are traced to the solvent,
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