ASTM D5317-20

Standard Test Method for Determination of Chlorinated Organic Acid Compounds in Water by Gas Chromatography with an Electron Capture Detector

SIGNIFICANCE AND USE
5.1 Chlorinated phenoxyacid herbicides, and other organic acids are used extensively for weed control. Esters and salts of 2,4-D and silvex have been used as aquatic herbicides in lakes, streams, and irrigation canals. Phenoxy acid herbicides can be toxic even at low concentrations. For example, the 96 h, TLm for silvex is 2.4 mg/L for bluegills (1).8 These reasons make apparent the need for a standard test method for such compounds in water.
SCOPE
1.1 This test method covers a gas chromatographic procedure for the quantitative determination of selected chlorinated acids and other acidic herbicides in water. Similar chemicals may also be determined by this test method, but it is the user’s responsibility to verify the applicability of this test method to any compounds not listed in this scope. The acid form of the following compounds were interlaboratory tested using this test method, and the results were found acceptable:2    
Analyte  
Chemical Abstract Services
Registry Number  
Bentazon  
25057-89-0  
2,4-D  
94-75-7  
2,4-DB  
94-82-6  
DCPA acid metabolites 2  
Dicamba  
1918-00-9  
3,5-Dichlorobenzoic acid  
51-36-5  
Dichlorprop  
120-36-5  
5-Hydroxydicamba  
7600-50-2  
Pentachlorophenol (PCP)  
87-86-5  
Picloram  
1918-02-1  
2,4,5-T  
93-76-5  
2,4,5-TP (Silvex)  
93-72-1  
1.2 This test method may be applicable to the determination of salts and esters of analyte compounds. The form of each acid is not distinguished by this test method. Results are calculated and reported for each listed analyte as the total free acid.  
1.3 This test method has been validated in an interlaboratory test for reagent water and finished tap water. The analyst should recognize that precision and bias reported in Section 18 may not be applicable to other waters.  
1.4 This test method is restricted to use by or under the supervision of analysts experienced in the use of gas chromatography (GC) and in the interpretation of gas chromatograms. Each analyst must demonstrate the ability to generate acceptable results with this test method using the procedure described in 19.3. It is the user’s responsibility to ensure the validity of this test method for waters of untested matrices.  
1.5 Analytes that are not separated chromatographically, that is, which have very similar retention times, cannot be individually identified and measured in the same calibration mixture or water sample unless an alternate technique for identification and quantitation exists (16.6, 16.7, and 16.8).  
1.6 When this test method is used to analyze unfamiliar samples for any or all of the analytes given in 1.1, analyte identifications must be confirmed by at least one additional qualitative technique.  
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see Sections 6, 8, 9, and 10.  
1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 14-Aug-2020
• ICS: 71.080.40 - Organic acids
• Technical Committee: D19 - Water
• Drafting Committee: D19.06 - Methods for Analysis for Organic Substances in Water

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D5317 − 20
Standard Test Method for
Determination of Chlorinated Organic Acid Compounds in
Water by Gas Chromatography with an Electron Capture
1
Detector
This standard is issued under the fixed designation D5317; 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 Each analyst must demonstrate the ability to generate accept-
ableresultswiththistestmethodusingtheproceduredescribed
1.1 This test method covers a gas chromatographic proce-
in 19.3. It is the user’s responsibility to ensure the validity of
dure for the quantitative determination of selected chlorinated
this test method for waters of untested matrices.
acids and other acidic herbicides in water. Similar chemicals
may also be determined by this test method, but it is the user’s 1.5 Analytes that are not separated chromatographically,
responsibility to verify the applicability of this test method to that is, which have very similar retention times, cannot be
any compounds not listed in this scope. The acid form of the individually identified and measured in the same calibration
following compounds were interlaboratory tested using this mixture or water sample unless an alternate technique for
2
test method, and the results were found acceptable: identification and quantitation exists (16.6, 16.7, and 16.8).
Chemical Abstract Services
1.6 When this test method is used to analyze unfamiliar
Analyte
Registry Number
samples for any or all of the analytes given in 1.1, analyte
identifications must be confirmed by at least one additional
Bentazon 25057-89-0
2,4-D 94-75-7
qualitative technique.
2,4-DB 94-82-6
2
DCPA acid metabolites 1.7 The values stated in SI units are to be regarded as
Dicamba 1918-00-9
standard. No other units of measurement are included in this
3,5-Dichlorobenzoic acid 51-36-5
standard.
Dichlorprop 120-36-5
5-Hydroxydicamba 7600-50-2
1.8 This standard does not purport to address all of the
Pentachlorophenol (PCP) 87-86-5
safety concerns, if any, associated with its use. It is the
Picloram 1918-02-1
2,4,5-T 93-76-5
responsibility of the user of this standard to establish appro-
2,4,5-TP (Silvex) 93-72-1
priate safety, health, and environmental practices and deter-
1.2 This test method may be applicable to the determination
mine the applicability of regulatory limitations prior to use.
ofsaltsandestersofanalytecompounds.Theformofeachacid
For specific warning statements, see Sections 6, 8, 9, and 10.
is not distinguished by this test method. Results are calculated
1.9 This international standard was developed in accor-
and reported for each listed analyte as the total free acid.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
1.3 Thistestmethodhasbeenvalidatedinaninterlaboratory
Development of International Standards, Guides and Recom-
testforreagentwaterandfinishedtapwater.Theanalystshould
mendations issued by the World Trade Organization Technical
recognize that precision and bias reported in Section 18 may
Barriers to Trade (TBT) Committee.
not be applicable to other waters.
1.4 This test method is restricted to use by or under the
2. Referenced Documents
supervision of analysts experienced in the use of gas chroma-
3
2.1 ASTM Standards:
tography (GC) and in the interpretation of gas chromatograms.
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
Applicable Test Methods of Committee D19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
Organic Substances in Water.
Current edition approved Aug. 15, 2020. Published August 2020. Originally
3
approved in 1992. Last previous edition approved in 2017 as D5317 – 98 (2017). For referenced ASTM standards, visit the ASTM website, www.astm.org, or
DOI: 10.1520/D5317-20. contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
2
DCPA monoacid and diacid metabolites are included in the scope of this test Standards volume information, refer to the standard’s Document Summary page on
method; DCPA diacid metabolite is used for validation studies. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D5317 − 20
7
D
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
Designation: D5317 − 98 (Reapproved 2017) D5317 − 20
Standard Test Method for
Determination of Chlorinated Organic Acid Compounds in
Water by Gas Chromatography with an Electron Capture
1
Detector
This standard is issued under the fixed designation D5317; 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
1.1 This test method covers a gas chromatographic procedure for the quantitative determination of selected chlorinated acids and
other acidic herbicides in water. Similar chemicals may also be determined by this test method, but it is the user’suser’s
responsibility to verify the applicability of this test method to any compounds not listed in this scope. The acid form of the
2
following compounds were interlaboratory tested using this test method, and the results were found acceptable:
Chemical Abstract Services
Analyte
Registry Number
Bentazon 25057-89-0
2,4-D 94-75-7
2,4-DB 94-82-6
2
DCPA acid metabolites
Dicamba 1918-00-9
3,5-Dichlorobenzoic acid 51-36-5
Dichlorprop 120-36-5
5-Hydroxydicamba 7600-50-2
Pentachlorophenol (PCP) 87-86-5
Picloram 1918-02-1
2,4,5-T 93-76-5
2,4,5-TP (Silvex) 93-72-1
1.2 This test method may be applicable to the determination of salts and esters of analyte compounds. The form of each acid is
not distinguished by this test method. Results are calculated and reported for each listed analyte as the total free acid.
1.3 This test method has been validated in an interlaboratory test for reagent water and finished tap water. The analyst should
recognize that precision and bias reported in Section 18 may not be applicable to other waters.
1.4 This test method is restricted to use by or under the supervision of analysts experienced in the use of gas chromatography (GC)
and in the interpretation of gas chromatograms. Each analyst must demonstrate the ability to generate acceptable results with this
test method using the procedure described in 19.3. It is the user’suser’s responsibility to ensure the validity of this test method for
waters of untested matrices.
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
Current edition approved Dec. 15, 2017Aug. 15, 2020. Published January 2018August 2020. Originally approved in 1992. Last previous edition approved in 20112017
as D5317 – 93 (2011).D5317 – 98 (2017). DOI: 10.1520/D5317-98R17.10.1520/D5317-20.
2
DCPA monoacid and diacid metabolites are included in the scope of this test method; DCPA diacid metabolite is used for validation studies.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D5317 − 20
1.5 Analytes that are not separated chromatographically, that is, which have very similar retention times, cannot be individually
identified and measured in the same calibration mixture or water sample unless an alternate technique for identification and
quantitation exists (16.6, 16.7, and 16.8).
1.6 When this test method is used to analyze unfamiliar samples for any or all of the analytes given in 1.1, analyte identifications
must be confirmed by at least one additional qualitative technique.
1.7 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions to
inch-pound units that are provided for information only and are not considered No other units of measurement are included in this
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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use. For specific warning statements, see Sections 6, 8, 9, and 10.
1.9 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
3
2.1 ASTM Standards:
D1129 Terminology Relat
...