ASTM D5812-96(2002)e1

Standard Test Method for Determination of Organochlorine Pesticides in Water by Capillary Column Gas Chromatography (Withdrawn 2011)

SIGNIFICANCE AND USE
The extensive and widespread use of organochlorine pesticides and PCBs has resulted in their presence in all parts of the environment. These compounds are persistent and may have adverse effects on the environment. Thus, there is a need to identify and quantitate these compounds in water samples.
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: PesticideChemical Abstract Service Registry Number Aldrin309-00-2-BHC319-84-6-BHC319-85-7-BHC319-86-8-BHC58-89-9-Chlordane5103-71-9-Chlordane5103-74-2Chlorobenzilate501-15-6Chloroneb2675-77-6Chlorothalonil2921-88-2DCPA1897-45-64,4`-DDD72-54-84,4`-DDE72-55-94,4`-DDT50-29-3Dieldrin60-57-1Endosulfan I959-98-8Endosulfan II33213-65-9Endosulfan sulfate1031-0708Endrin72-20-8Endrin aldehyde7421-93-4Etridiazole2593-15-9Heptachlor76-44-8Heptachlor epoxide1024-57-3Hexachlorobenzene118-74-1Methoxychlor72-43-5cis-Permethrin52645-53-1trans-Permethrin52645-53-1Propachlor1918-16-7Trifluralin1582-09-8 Numbering system of CAS Registry Services, P.O. Box 3343, Columbus, OH 43210-0334.
1.2 and 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 extract derived from this procedure may be analyzed for these constituents by using the gas chromatography (GC) conditions prescribed in Test Method D 5175 (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.
WITHDRAWN RATIONALE
Formerly under the jurisdiction of Committee D19 on Water, this Test Method was withdrawn in 2011 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.

General Information

• Status: Withdrawn
• Publication Date: 09-May-1996
• Withdrawal Date: 31-Dec-2010
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: D19 - Water
• Drafting Committee: D19.06 - Methods for Analysis for Organic Substances in Water

Relations

• Replaces: ASTM D5812-96 - Standard Test Method for Determination of Organochlorine Pesticides in Water by Capillary Column Gas Chromatography
• Effective Date: 10-May-1996
• Referred By: ASTM D3694-96(2017) - Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
• Effective Date: 10-May-1996

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
´1
Designation:D5812–96 (Reapproved 2002)
Standard Test Method for
Determination of Organochlorine Pesticides in Water by
Capillary Column Gas Chromatography
This standard is issued under the fixed designation D5812; 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.
´ NOTE—Editorial changes were made in July 2002.
1. Scope 1.2 Table 1 and Table 2 list the applicable concentration
ranges and precision and bias statements for this test method.
1.1 This test method covers the capillary gas chromato-
The applicability of this test method to other compounds must
graphic determination of various organochlorine pesticides,
be demonstrated.
including some of their degradation products and related
1.3 The extract derived from this procedure may be ana-
compounds in finished drinking water. This test method is not
lyzed for these constituents by using the gas chromatography
limited to this particular aqueous matrix; however, its applica-
(GC) conditions prescribed in Test Method D5175 (capillary
bilitytootheraqueousmatricesmustbedetermined.Thetested
column). Although the columns used in this test method may
compounds include the following:
beadequateforanalyzingPCBs,nodatawerecollectedforany
Chemical Abstract
Pesticide
A
multi-congener constituents 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
4,48-DDD 72-54-8 be identified and measured individually in the same calibration
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
Endrin aldehyde 7421-93-4 least one additional technique.
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
43210-0334. 2. Referenced Documents
2.1 ASTM Standards:
D1129 Terminology Relating to Water
This test method is under the jurisdiction of ASTM Committee D19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
Organic Substances in Water.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved July 10, 2002. Published July 1996. Originally
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
published as D5812 – 95. Last previous edition D5812 – 95. DOI: 10.1520/D5812-
Standards volume information, refer to the standard’s Document Summary page on
96R02E01.
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D5812–96 (2002)
TABLE 1 Regression Equations for Method Precision and Mean Recovery for Reagent Water
Compound Concentration Range,µ g/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 0.998C + 0.006
d-BHC 0.02–1.01 0.050X + 0.001 0.119X + 0.002 0.958C + 0.005
a-Chlordane 0.03–1.50 0.062X + 0.000 0.138X + 0.000 1.008C + 0.003
g-Chlordane 0.03–1.51 0.048X + 0.002 0.129X + 0.001 0.936C + 0.005
Chlorobenzilate 1.00–50.00 0.067X + 0.022 0.178X + 0.117 0.993C + 0.263
Chloroneb 1.00–50.08 0.111X − 0.016 0.159X + 0.275 0.942C + 0.280
Chlorothalonil 0.05–2.51 0.096X + 0.001 0.233X + 0.001 0.955C + 0.001
DCPA 0.05–2.51 0.047X + 0.002 0.161X + 0.002 0.998C + 0.013
4,48-DDD 0.05–2.50 0.087X − 0.001 0.150X + 0.000 0.970C + 0.006
4,48-DDE 0.02–1.00 0.093X + 0.001 0.166X + 0.000 0.982C + 0.000
4,48-DDT 0.12–6.01 0.044X + 0.017 0.140X + 0.002 0.976C + 0.006
Dieldrin 0.04–2.01 0.089X + 0.000 0.150X + 0.009 0.962C + 0.009
Endosulfan I 0.03–1.51 0.070X + 0.000 0.127X + 0.009 0.957C + 0.006
Endosulfan II 0.03–1.49 0.059X + 0.001 0.120X + 0.002 0.974C + 0.003
Endosulfan sulfate 0.03–1.51 0.115X + 0.003 0.158X + 0.007 0.988C + 0.004
Endrin 0.03–1.50 0.108X − 0.002 0.134X + 0.002 0.991C + 0.002
Endrin aldehyde 0.05–2.49 0.105X − 0.004 0.121X + 0.003 0.940C + 0.007
Etridiazole 0.05–2.48 0.049X + 0.002 0.149X + 0.010 0.960C + 0.007
Heptachlor 0.02–1.00 0.068X + 0.001 0.100X + 0.011 0.961C + 0.009
Heptachlor epoxide 0.03–1.50 0.049X + 0.002 0.122X + 0.005 0.950C + 0.006
Hexachlorobenzene 0.01–0.50 0.049X + 0.000 0.124X + 0.003 0.841C + 0.003
Methoxychlor 0.10–5.01 0.108X − 0.004 0.190X − 0.003 1.044C + 0.016
cis-Permethrin 1.00–50.08 0.077X + 0.034 0.138X + 0.204 0.938C + 0.314
trans-Permethrin 1.00–50.12 0.096X − 0.001 0.233X + 0.001 0.955C + 0.001
Propachlor 1.00–50.08 0.052X + 0.098 0.119X + 0.370 0.978C + 0.317
Trifluralin 0.05–2.51 0.064X + 0.003 0.144X + 0.004 0.888C + 0.004
A
TABLE 2 Regression Equations for Method Precision and Mean Recovery for Finished Drinking Water
Compound Concentration Range,µ g/L Single-analyst Precision, s Overall Precision, s Mean Recovery, X
r R
Aldrin 0.03–1.49 0.048X + 0.008 0.175X + 0.005 0.826C + 0.008
a-BHC 0.02–1.00 0.094X − 0.000 0.198X + 0.000 0.940C + 0.003
b-BHC 0.02–1.00 0.142X − 0.001 0.227X + 0.003 0.923C + 0.005
g-BHC 0.03–1.51 0.070X − 0.001 0.138X + 0.006 0.938C + 0.002
d-BHC 0.02–1.01 0.066X + 0.005 0.133X + 0.004 0.905C + 0.007
a-Chlordane 0.03–1.50 0.070X + 0.000 0.164X + 0.000 0.870C + 0.005
g-Chlordane 0.03–1.51 0.072X + 0.000 0.138X + 0.001 0.865C + 0.005
Chlorobenzilate 1.00–50.00 0.146X − 0.042 0.243X + 0.292 0.874C + 0.207
Chloroneb 1.00–50.08 0.100X − 0.024 0.185X + 0.110 0.883C + 0.218
Chlorothalonil 0.05–2.51 0.100X + 0.001 0.180X + 0.004 0.920C + 0.000
DCPA 0.05–2.51 0.136X − 0.003 0.224X − 0.003 0.920C + 0.015
4,48-DDD 0.05–2.50 0.102X + 0.001 0.146X + 0.002 0.908C + 0.008
4,48-DDE 0.02–1.00 0.081X − 0.001 0.203X − 0.002 0.842C + 0.002
4,48-DDT 0.12–6.01 0.110X − 0.005 0.162X + 0.012 0.858C + 0.009
Dieldrin 0.04–2.01 0.065X − 0.000 0.140X − 0.000 0.882C + 0.006
Endosulfan I 0.03–1.51 0.072X + 0.001 0.117X + 0.003 0.898C + 0.004
Endosulfan II 0.03–1.49 0.064X − 0.000 0.119X + 0.002 0.901C + 0.002
Endosulfan sulfate 0.03–1.51 0.132X − 0.000 0.233X + 0.007 0.948C + 0.009
Endrin 0.03–1.50 0.062X + 0.001 0.120X + 0.002 0.893C + 0.001
Endrin aldehyde 0.05–2.49 0.076X − 0.001 0.097X + 0.005 0.874C + 0.003
Etridiazole 0.05–2.48 0.074X + 0.001 0.240X − 0.000 0.916C + 0.009
Heptachlor 0.02–1.00 0.072X + 0.001 0.075X + 0.009 0.980C + 0.005
Heptachlor epoxide 0.03–1.50 0.066X + 0.001 0.084X + 0.004 0.944C + 0.006
Hexachlorobenzene 0.01–0.50 0.013X + 0.002 0.097X + 0.005 0.833C + 0.004
Methoxychlor 0.10–5.01 0.142X − 0.004 0.285X − 0.007 0.936C + 0.017
cis-Permethrin 1.00–50.08 0.112X + 0.012 0.161X + 0.292 0.833C + 0.200
trans-Permethrin 1.00–50.12 0.184X − 0.087 0.410X − 0.063 0.814C + 0.287
Propachlor 1.00–50.08 0.087X + 0.061 0.158X + 0.185 0.925C + 0.353
Trifluralin 0.05–2.51 0.066X + 0.002 0.147X + 0.004 0.847C + 0.006
A
X = mean recovery; C = analyte true concentration.
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D5812–96 (2002)
D1192 Guide for Equipment for SamplingWater and Steam 3.2.2 field reagent blank (FRB)—reagent water placed in a
in Closed Conduits samplecontainerinthelaboratoryandtreatedasasampleinall
D1193 Specification for Reagent Water respects, including exposure to sampling site conditions, stor-
D2777 Practice for Determination of Precision and Bias of age, preservation, and all analytical procedures. The reagent
Applicable Test Methods of Committee D19 on Water water must be transferred to an empty, clean sample container
D3370 Practices for Sampling Water from Closed Conduits in the field. The purpose of the FRB is to determine whether
D3694 Practices for Preparation of Sample Containers and analytes or other interferences are present in the field environ-
for Preservation of Organic Constituents ment.
D3856 Guide for Good Laboratory Practices in Laborato-
3.2.3 instrument performance check (IPC) solution—a so-
ries Engaged in Sampling and Analysis of Water
lution of analytes used to evaluate the performance of the
D4128 Guide for Identification and Quantitation of Organic
instrument system with respect to test method criteria.
Compounds in Water by Combined Gas Chromatography
3.2.4 laboratory duplicates (LD 1 and LD 2)—two sample
and Electron Impact Mass Spectrometry
aliquots taken in the analytical laboratory and analyzed sepa-
D4210 Practice for Intralaboratory Quality Control Proce-
rately with identical procedures. Analyses of LD 1 and LD 2
dures and a Discussion on Reporting Low-Level Data
provide a measure of the precision associated with laboratory
D5175 Test Method for Organohalide Pesticides and Poly-
procedures, but not with sample collection, preservation, or
chlorinated Biphenyls in Water by Microextraction and
storage procedures.
Gas Chromatography
3.2.4.1 Discussion—Analysis of laboratory duplicates or
D5810 Guide for Spiking into Aqueous Samples
spiked samples requires the collection of duplicate 1-L sample
E260 Practice for Packed Column Gas Chromatography
bottles or the use of 2-L sample containers.
E355 Practice for Gas Chromatography Terms and Rela-
3.2.5 laboratory fortified blank (LFB)—an aliquot of re-
tionships
agent water to which known quantities of analytes are added in
E697 Practice for Use of Electron-Capture Detectors in Gas
the laboratory. The LFB is analyzed exactly like a sample, and
Chromatography
its purpose is to determine whether the methodology is in
E1510 Practice for Installing Fused Silica Open Tubular
control and whether the laboratory is capable of making
Capillary Columns in Gas Chromatographs
accurate and precise measurements.
2.2 U.S. EPA Standards:
3.2.6 laboratory fortified sample matrix (LFM)—an aliquot
Method 508, Determination of Chlorinated Pesticides in
of an environmental sample to which known quantities of
Water by Gas Chromatography with an Electron Capture
analytes are added in the laboratory. The LFM is analyzed
Detector (Revision 3.0, 1988)
exactly like a sample, and its purpose is to determine whether
Analytical Methods for Pesticides/Aroclors (February
the sample matrix contributes bias to the analytical results.The
1991)
background concentrations of analytes in the sample matrix
Method 680, Determination of Pesticides and PCBs in
must be determined in a separate aliquot and the measured
Water and Soil/Sediment by Gas Chromatography/Mass
values in the LFM corrected for background concentrations
Spectrometry (Revision 3.0, 1988)
(see 3.2.4.1).
2.3 AOAC Standard:
3.2.7 laboratory reagent blank (LRB)—an aliquot of re-
Method 990.06, Organochlorine Pesticides in Water
agent water that is treated exactly like a sample, including
3. Terminology exposure to all glassware, equipment, solvents, and reagents
thatareusedwithothersamples.TheLRBisusedtodetermine
3.1 Definitions—For definitions of terms used in this test
whether method analytes or other interferences are present in
method, refer to Terminology D1129 and Practice E355.
the laboratory environment, reagents, or apparatus.
3.2 Definitions of Terms Specific to This Standard:
3.2.8 quality control sample (QCS)—a sample containing
3.2.1 field duplicates (FD 1 and FD 2)—two separate
analytes or a solution of analytes in a water-miscible solvent
samples collected at the same time and placed under identical
that is used to fortify reagent water or environmental samples.
circumstances and treated exactly the same throughout field
The QCS must be independent of solutions used to prepare
and laboratory procedures.Analyses of FD 1 and FD 2 provide
standards and should be obtained from a source external to the
a measure of the precision associated with sample collection,
laboratory. The QCS is used to check laboratory performance
preservation, and storage, as well as with laboratory proce-
with externally prepared test materials and is analyzed exactly
dures.
like a sample.
3 3.2.9 spike—an addition of a known quantity of a compo-
Withdrawn. The last approved version of this historical standard is referenced
on www.astm.org. nent of known identity to a known volume of a sample in order
Available from U.S. Environmental ProtectionAgency, Office of Research and
to determine the efficiency with which the added component is
Development, Environmental Monitoring Systems Laboratory, Cincinnati, OH
recovered. Spike components should be prepared from a
45268.
different source than that used for calibration standards. Refer
U.S. EPA CLP Statement of Work for Organics Analysis, Document
OLM01.1.1, Available from U.S. EPA Contracts Management Division (MD33),
to Guide D5810 for guidance on spiking organics into aqueous
Administration Building Lobby, Alexander Drive, Research Triangle Park, NC
samples.
27711.
3.2.10 standard solution, secondary dilution—a solution of
Available from Association of Official Analytical Chemists, Suite 400, 2200
Wilson Boulevard, Arlington, VA 22201. several analytes prepared in the laboratory from stock analyte
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D5812–96 (2002)
solutions and diluted as necessary to prepare calibratio
...