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ASTM D5812-96

(Test Method)

Standard Test Method for Determination of Organochlorine Pesticides in Water by Capillary Column Gas Chromatography

Standard Test Method for Determination of Organochlorine Pesticides in Water by Capillary Column Gas Chromatography

SCOPE
1.1 This test method covers the capillary gas chromatographic determination of various organochlorine pesticides, including some of their degradation products and related compounds in finished drinking water. This test method is not limited to this particular aqueous matrix; however, its applicability to other aqueous matrices must be determined. The tested compounds include the following:  Chemical Abstract Pesticide Service Registry Number A Aldrin 309-00-2 [alpha]-BHC 319-84-6 [beta]-BHC 319-85-7 [gamma]-BHC 319-86-8 [delta]-BHC 58-89-9 [alpha]-Chlordane 5103-71-9 [gamma]-Chlordane 5103-74-2 Chlorobenzilate 501-15-6 Chloroneb 2675-77-6 Chlorothalonil 2921-88-2 DCPA 1897-45-6 4,4'-DDD 72-54-8 4,4'-DDE 72-55-9 4,4'-DDT 50-29-3 Dieldrin 60-57-1 Endosulfan I 959-98-8 Endosulfan II 33213-65-9 Endosulfan sulfate 1031-0708 Endrin 72-20-8 Endrin aldehyde 7421-93-4 Etridiazole 2593-15-9 Heptachlor 76-44-8 Heptachlor epoxide 1024-57-3 Hexachlorobenzene 118-74-1 Methoxychlor 72-43-5 cis-Permethrin 52645-53-1 trans-Permethrin 52645-53-1 Propachlor 1918-16-7 Trifluralin 1582-09-8 A Numbering system of CAS Registry Services, P.O. Box 3343, Columbus, OH 43210-0334.
1.2 Tables 1 and 1 list the applicable concentration ranges and precision and bias statements for this test method. The applicability of this test method to other compounds must be demonstrated.  
1.3 The extraction conditions of this test method are comparable to Test Method D3534, which determines commercial polychlorinated biphenyl (PCB) mixtures (Aroclors). The extract derived from this procedure may be analyzed for these constituents by using the gas chromatography (GC) conditions prescribed in either Test Method D3534 (packed column) or Test Method D5175 (capillary column). Although the columns used in this test method may be adequate for analyzing PCBs, no data were collected for any multi-congener constituents during methods development.  
1.4 This test method is restricted to use by or under the supervision of analysts experienced in the use of GC and interpretation of gas chromatograms. Each analyst must demonstrate the ability to generate acceptable results using the procedures described in Section 12.  
1.5 Analytes that are not separated chromatographically by either the primary or secondary chromatographic columns (for example, analytes having very similar retention times) cannot be identified and measured individually in the same calibration mixture or water sample unless an alternative technique for identification and quantitation exists (see 7.9 and 13.4).  
1.6 When this test method is used to analyze unfamiliar samples for any or all of the analytes listed in 1.1, analyte identifications and concentrations should be confirmed by at least one additional technique.  
1.7 The values stated in SI units are to be regarded as the standard.  
1.8 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 hazards statements are given in Section 9.

General Information

Status
Historical
Publication Date
31-Dec-1995
Technical Committee
D19 - Water
Drafting Committee
D19.06 - Methods for Analysis for Organic Substances in Water
Current Stage
Ref Project

Relations

Replaced By
ASTM D5812-96(2002)e1 - Standard Test Method for Determination of Organochlorine Pesticides in Water by Capillary Column Gas Chromatography (Withdrawn 2011)
Effective Date
10-May-1996

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ASTM D5812-96 - Standard Test Method for Determination of Organochlorine Pesticides in Water by Capillary Column Gas ChromatographyASTM D5812-96 - Standard Test Method for Determination of Organochlorine Pesticides in Water by Capillary Column Gas Chromatography
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ASTM D5812-96 - Standard Test Method for Determination of Organochlorine Pesticides in Water by Capillary Column Gas Chromatography
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Standards Content (Sample)

Designation: D 5812 – 96
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
Determination of Organochlorine Pesticides in Water by
1
Capillary Column Gas Chromatography
This standard is issued under the fixed designation D 5812; 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 1.3 The extraction conditions of this test method are com-
parable to Test Method D 3534, which determines commercial
1.1 This test method covers the capillary gas chromato-
polychlorinated biphenyl (PCB) mixtures (Aroclors). The ex-
graphic determination of various organochlorine pesticides,
tract derived from this procedure may be analyzed for these
including some of their degradation products and related
constituents by using the gas chromatography (GC) conditions
compounds in finished drinking water. This test method is not
prescribed in either Test Method D 3534 (packed column) or
limited to this particular aqueous matrix; however, its applica-
Test Method D 5175 (capillary column). Although the columns
bility to other aqueous matrices must be determined. The tested
used in this test method may be adequate for analyzing PCBs,
compounds include the following:
no data were collected for any multi-congener constituents
Chemical Abstract
Pesticide
A
during methods development.
Service Registry Number
Aldrin 309-00-2
1.4 This test method is restricted to use by or under the
a-BHC 319-84-6
supervision of analysts experienced in the use of GC and
b-BHC 319-85-7
interpretation of gas chromatograms. Each analyst must dem-
g-BHC 319-86-8
d-BHC 58-89-9
onstrate the ability to generate acceptable results using the
a-Chlordane 5103-71-9
procedures described in Section 12.
g-Chlordane 5103-74-2
1.5 Analytes that are not separated chromatographically by
Chlorobenzilate 501-15-6
Chloroneb 2675-77-6
either the primary or secondary chromatographic columns (for
Chlorothalonil 2921-88-2
example, analytes having very similar retention times) cannot
DCPA 1897-45-6
be identified and measured individually in the same calibration
4,48-DDD 72-54-8
4,48-DDE 72-55-9
mixture or water sample unless an alternative technique for
4,48-DDT 50-29-3
identification and quantitation exists (see 7.9 and 13.4).
Dieldrin 60-57-1
Endosulfan I 959-98-8 1.6 When this test method is used to analyze unfamiliar
Endosulfan II 33213-65-9
samples for any or all of the analytes listed in 1.1, analyte
Endosulfan sulfate 1031-0708
identifications and concentrations should be confirmed by at
Endrin 72-20-8
least one additional technique.
Endrin aldehyde 7421-93-4
Etridiazole 2593-15-9
1.7 The values stated in SI units are to be regarded as the
Heptachlor 76-44-8
standard.
Heptachlor epoxide 1024-57-3
Hexachlorobenzene 118-74-1 1.8 This standard does not purport to address all of the
Methoxychlor 72-43-5
safety concerns, if any, associated with its use. It is the
cis-Permethrin 52645-53-1
responsibility of the user of this standard to establish appro-
trans-Permethrin 52645-53-1
Propachlor 1918-16-7 priate safety and health practices and determine the applica-
Trifluralin 1582-09-8
bility of regulatory limitations prior to use. Specific hazards
statements are given in Section 9.
A
Numbering system of CAS Registry Services, P.O. Box 3343, Columbus, OH
2. Referenced Documents
43210-0334.
1.2 Table 1 and Table 2 list the applicable concentration
2.1 ASTM Standards:
2
ranges and precision and bias statements for this test method.
D 1129 Terminology Relating to Water
The applicability of this test method to other compounds must
D 1192 Specification for Equipment for Sampling Water
2
be demonstrated.
and Steam in Closed Conduits
2
D 1193 Specification for Reagent Water
D 2777 Practice for Determination of Precision and Bias of
1
This test method is under the jurisdiction of ASTM Committee D-19 on Water
2
Applicable Methods of Committee D-19 on Water
and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
Current edition approved May 10, 1996. Published July 1996. Originally
2
published as D 5812 – 95. Last previous edition D 5812 – 95. Annual Book of ASTM Standards, Vol 11.01.
1

---------------------- Page: 1 ----------------------
D 5812
TABLE 1 Regression Equations for Method Precision and Mean Recovery for Reagent Water
Compound Concentration Range, μg/L Single-analyst Precision, s Overall Precision, s Mean Recovery, X
r R
Aldrin 0.03–1.38 0.061X + 0.004 0.130X + 0.009 0.909C + 0.007
a-BHC 0.02–1.00 0.059X + 0.001 0.127X + 0.005 1.015C + 0.004
b-BHC 0.02–1.00 0.034X + 0.004 0.148X + 0.005 0.975C + 0.006
g-BHC 0.03–1.51 0.047X + 0.005 0.147X + 0.007
...

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