ASTM D3973-85(1995)e1
(Test Method)Standard Test Method for Low-Molecular Weight Halogenated Hydrocarbons in Water
Standard Test Method for Low-Molecular Weight Halogenated Hydrocarbons in Water
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn.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.
e1
Designation: D 3973 – 85 (Reapproved 1995)
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
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.
e NOTE—Section 15 was added editorially in June 1995.
1. Scope E 355 Practice for Gas Chromatography Terms and Rela-
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 halom-
method, refer to Terminology D 1129 and Practice E 355.
ethanes, haloethanes, and some related extractable organoha-
4. Summary of Test Method
lides amenable to gas chromatographic measurement. The
4.1 This test method employs liquid/liquid extraction to
applicable concentration range for trihalomethanes is from 1 to
isolate compounds of interest and provide a five-fold concen-
200 μg/L. Detection limits depend on the compound, matrix,
5,6,7
tration enhancement prior to measurement. A5-mL aqueous
and on the characteristics of the gas chromatographic system.
sample is extracted once with 1 mL of solvent. -μL aliquot of
1.3 For compounds not specifically included in the precision
the extract is analyzed in a gas chromatograph equipped with
and bias section the analyst should validate the test method by
an electron-capture detector.
collecting precision and bias data on actual samples.
4.2 Extraction efficiencies with the 1:5 solvent/sample ratio
1.4 Confirmation of component identities is obtained by
for trihalomethanes average above 90 %. To compensate for
observing retention times using gas chromatographic columns
extraction losses, calibration standards are extracted and ana-
of different polarities. When concentrations are sufficiently
lyzed in an identical manner.
high (>50 μg/L) confirmation with halogen specific detectors
4.3 The concentration of each component is calculated and
or gas chromatography/mass spectrometry (GC/MS) may be
reported in micrograms per litre.
used. Confirmation of purgeable compounds at levels down to
5. Significance and Use
1 μg/L can be obtained using Test Method D 3871 with GC/MS
detection. 5.1 The incidental conversion of organic material to triha-
lomethanes and other volatile organohalides during chlorina-
1.5 This standard does not purport to address all of the
tion of water is a possible health hazard and is the object of
safety concerns, if any, associated with its use. It is the
much research. This test method can be used as a rapid, simple
responsibility of the user of this standard to establish appro-
means for determining many volatile organohalides in raw and
priate safety and health practices and determine the applica-
processed water.
bility of regulatory limitations prior to use. Specific precau-
tionary statements are given in Section 8.
6. Interferences
6.1 Volatile compounds that are extractable and responsive
2. Referenced Documents
to electron-capture detection may interfere with this test
2.1 ASTM Standards: method.
D 1129 Terminology Relating to Water 6.2 Impurities in the extracting solvent can be a source of
D 1193 Specification for Reagent Water interference. Solvent blanks should be analyzed daily and
D 3871 Test Method for Purgeable Organic Compounds in before a new bottle of solvent is used for the first time.
Water Using Headspace Sampling Whenever interfering compounds are traced to the solvent, a
This test method is under the jurisdiction of ASTM Committee D-19 on Water
Annual Book of ASTM Standards, Vol 14.01.
and is the direct responsibility of Subcommittee D19.06 on Methods of Analysis for Mieure, J. P., “A Rapid and Sensitive Method for Determining Volatile
Organic Substances in Water. Organohalides in Water,” Journal AWWA, Vol 69, 1977, p. 60.
Current edition approved Jan. 25, 1985. Published March 1985. Originally Richard, J. J., and Junk, G. A., “Liquid Extraction for Rapid Determination of
published as D 3973 – 80. Last previous edition D 3973 – 80. Halomethanes in Water,” Journal AWWA, Vol 69, 1977, p. 62.
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Annual Book of ASTM Standards, Vol 11.01. “The Analysis of Trihalomethanes in Drinking Water by Liquid/Liquid Extrac-
Annual Book of ASTM Standards, Vol 11.02. tion,” U.S. Environmental Protection Agency, EMSL, Cincinnati, OH, Sept. 9, 1977.
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.¬
D 3973
new source of solvent should be obtained. Alternatively, carbon (8.3), or using a commercial water purification sys-
impurities may be removed by distillation, column chromatog- tem.
raphy or purging with high-purity nitrogen or helium. This
8.3 Activated Carbon.
procedure is quantitative as long as solvent interference con-
8.4 Dechlorinating Agent—Granular sodium thiosulfate or
tributes less than 10 % to the component concentration in the
ascorbic acid.
sample.
8.5 Detergent, suitable for laboratory glassware.
8.6 Isooctane, pesticide grade.
7. Apparatus
8.7 Methyl Alcohol, pesticide grade.
7.1 Extraction Vessel, 9-mL (2-dram) vial with aluminum
8.8 Sodium Chloride, granular.
foil or PTFE-lined caps.
8.9 Reference Standards:
7.2 Sample Containers, 40-mL screw cap vials sealed with
8.9.1 Bromoform.
PTFE-faced silicone septa.
8.9.2 Bromodichloromethane.
7.3 Micro Syringes, 10, 100-μL.
8.9.3 Chlorodibromomethane.
7.4 Pipets, 1.0 and 5.0-mL transfer.
8.9.4 Chloroform.
7.5 Glass-Stoppered Volumetric Flasks, 10 and 100-mL.
8.9.5 Tetrachloroethylene.
7.6 Gas Chromatograph, with electron-capture detector.
7.7 Columns, either of the following columns have been 8.9.6 1,1,1-Trichloroethane.
found suitable for this analysis. See Fig. 1 for chromatograms.
8.10 Stock Solutions—Prepare a stock solution (2 to 10
If other column conditions are used, it is up to the analyst to
mg/mL) for each standard as follows:
demonstrate the precision and bias statements are met by
8.10.1 Warning—Because of the toxicity of trihalom-
collecting precision, bias, and recovery data.
ethanes it is necessary to prepare primary dilutions in a hood.
7.7.1 Nonpolar, 3-mm inside diameter by 2-m long boro-
It is further recommended that a NIOSH/MESA-approved
silicate glass packed with 100/120 mesh support coated with
toxic gas respirator be used when the analyst handles high
a methyl silicone liquid phase and operated at 60°C with 45
concentrations of such materials.
mL/min carrier flow.
8.10.2 Fill a 10.0-mL ground-glass-stoppered volumetric
7.7.2 Polar, 3-mm inside diameter by 2-m long borosilicate
flask with approximately 9.8 mL of methyl alcohol.
glass packed with 100/120 mesh support coated with a polar
8.10.3 Allow the flask to stand unstoppered about 10 min or
liquid phase such as polyethylene glycol and operated at
until all alcohol wetted surfaces dry.
50°C with 60 mL/min carrier flow.
8.10.4 Weigh the unstoppered flask to the nearest 0.1 mg.
8.10.5 Using a 100-μL syringe, immediately add 5 to 25
8. Reagents
drops of one of the reference standards (8.9) to the flask, then
8.1 Purity of Reagents—Reagent grade chemicals shall be
reweigh. Be sure that the drops fall directly into the alcohol
used in all tests. Unless otherwise indicated, it is intended that
without contacting the neck of the flask.
all reagents shall conform to the specifications of the Commit-
8.10.6 Dilute to volume with the alcohol, stopper, then mix
tee on Analytical Reagents of the American Chemical Soci-
by inverting the flask several times.
ety, where such specifications are available. Other grades
8.10.7 Calculate the concentration in micrograms per mil-
may be used, provided it is first ascertained that the reagent is
lilitre from the net gain in weight.
of sufficiently high purity to permit its use without lessening
8.10.8 Store the solutions at 4°C. Warm to room tempera-
the accuracy of the determination.
ture before use.
8.2 Purity of Water—Unless otherwise indicated, Specifica-
tion D 1193 reagent water, Type II, will be used in this test
NOTE 1—Standard solutions prepared in methyl alcohol are stable up to
method. In addition the water is made organic-free by passing
4 weeks when stored under these conditions. They should be discarded
it through a filter bed containing about 0.4 kg of activated after that time has elapsed.
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13075 vials and 12722 septa, available from Pierce Chemical Co., P.O. Box Super Q water system, available from Millipore Corp. Ashby Rd., Bedford,
117, Rockford, IL 61105, have been found suitable; other sources that are equivalent MA 01730, has been found suitable; other sources that are equivalent may be
may be substituted. substituted.
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Gas-Chrom Q, available from Applied Science Laboratory, Inc., P.O. Box 440, Filtrasorb 200, available from Calgon Corp., Box 1346, Pittsburgh, PA 15230,
State College, PA 16801, has been found suitable; other sources that are equivalent has been found suitable; other sources that are equivalent may be substituted.
may be substituted. Pesticide grade, available from Burdick & Jackson Labs, Inc., 1953 S. Harvey
OV-101, available from Ohio Valley Specialty Chemical, Inc., Route 6, St., Muskegon, MI 49442, or Spectro Grade, available from Phillips Chemical Co.,
Marietta, OH 45750, has been found suitable; other sources that are equivalent may Specialty Chemicals, Drawer “O”, Borger, TX 79007, have been found suitable;
be substituted. other sources that are equivalent may be substituted.
11 16
SP-1000, available from Supelco, Inc., Supelco Park, Bellafonte, PA 16823, Pesticide grade, available from Burdick & Jackson Labs, Inc., has been found
has been found suitable; other sources that are equivalent may b
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