ASTM D7600-16
(Test Method)Standard Test Method for Determination of Aldicarb, Carbofuran, Oxamyl and Methomyl by Liquid Chromatography/Tandem Mass Spectrometry
Standard Test Method for Determination of Aldicarb, Carbofuran, Oxamyl and Methomyl by Liquid Chromatography/Tandem Mass Spectrometry
SIGNIFICANCE AND USE
5.1 The N-methyl carbamate (NMC) pesticides: aldicarb, carbaryl, carbofuran, formetanate hydrochloride, methiocarb, methomyl, oxamyl, pirimicarb, propoxur, and thiodicarb have been identified by EPA as working through a common mechanism. They affect the nervous system by reducing the ability of the enzyme cholinesterase. Cholinesterase inhibition was the primary toxicological effect of regulatory concern to EPA in assessing the NMC’s food, drinking water and residential risks. In most of the country, NMC residues in drinking water sources are at levels that are not likely to contribute substantially to the multi-pathway cumulative exposure. Shallow private wells extending through highly permeable soils into shallow, acidic ground water represent what the EPA believes to be the most vulnerable drinking water.4
5.2 This test method has been investigated for use with reagent and surface water for the selected carbamates: aldicarb, carbofuran, oxamyl, and methomyl.
SCOPE
1.1 This procedure covers the determination of aldicarb, carbofuran, oxamyl and methomyl (referred to collectively as carbamates in this test method) in surface water by direct injection using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this test method. This test method adheres to multiple reaction monitoring (MRM) mass spectrometry.
1.2 This test method has been developed by US EPA Region 5 Chicago Regional Laboratory (CRL).
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 The Detection Verification Level (DVL) and Reporting Range for the carbamates are listed in Table 1.
1.4.1 The DVL is required to be at a concentration at least 3 times below the Reporting Limit (RL) and have a signal/noise ratio greater than 3:1. Fig. 1 displays the signal/noise ratios of the primary single reaction monitoring (SRM) transitions and Fig. 2 displays the confirmatory SRM transitions at the DVLs for the carbamates.
1.4.2 The reporting limit is the concentration of the Level 1 calibration standard as shown in Table 2 for the carbamates.
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.
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Designation:D7600 −16
Standard Test Method for
Determination of Aldicarb, Carbofuran, Oxamyl and
Methomyl by Liquid Chromatography/Tandem Mass
1
Spectrometry
This standard is issued under the fixed designation D7600; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 This procedure covers the determination of aldicarb,
D1129Terminology Relating to Water
carbofuran, oxamyl and methomyl (referred to collectively as
D1193Specification for Reagent Water
carbamates in this test method) in surface water by direct
D2777Practice for Determination of Precision and Bias of
injection using liquid chromatography (LC) and detected with
Applicable Test Methods of Committee D19 on Water
tandemmassspectrometry(MS/MS).Theseanalytesarequali-
D3856Guide for Management Systems in Laboratories
tativelyandquantitativelydeterminedbythistestmethod.This
Engaged in Analysis of Water
test method adheres to multiple reaction monitoring (MRM)
D3694Practices for Preparation of Sample Containers and
mass spectrometry.
for Preservation of Organic Constituents
1.2 ThistestmethodhasbeendevelopedbyUSEPARegion
D5847Practice for Writing Quality Control Specifications
5 Chicago Regional Laboratory (CRL).
for Standard Test Methods for Water Analysis
1.3 The values stated in SI units are to be regarded as
E2554Practice for Estimating and Monitoring the Uncer-
standard. No other units of measurement are included in this
tainty of Test Results of a Test Method Using Control
standard.
Chart Techniques
3
2.2 Other Documents:
1.4 The Detection Verification Level (DVL) and Reporting
EPApublication SW-846Test Methods for Evaluating Solid
Range for the carbamates are listed in Table 1.
Waste, Physical/Chemical Methods
1.4.1 The DVL is required to be at a concentration at least
3 times below the Reporting Limit (RL) and have a signal/
3. Terminology
noise ratio greater than 3:1. Fig. 1 displays the signal/noise
3.1 Definitions:
ratios of the primary single reaction monitoring (SRM) transi-
3.1.1 For definitions of terms used in this standard, refer to
tions and Fig. 2 displays the confirmatory SRM transitions at
Terminology D1129.
the DVLs for the carbamates.
3.2 Definitions of Terms Specific to This Standard:
1.4.2 The reporting limit is the concentration of the Level 1
3.2.1 detection verification level, DVL, n—a concentration
calibration standard as shown in Table 2 for the carbamates.
that has a signal/noise ratio greater than 3:1 and is at least 3
1.5 This standard does not purport to address all of the
times below the reporting limit (RL).
safety concerns, if any, associated with its use. It is the
3.2.2 carbamates, n—in this test method, aldicarb,
responsibility of the user of this standard to establish appro-
carbofuran, oxamyl and methomyl collectively.
priate safety and health practices and determine the applica-
3.2.3 independent reference material, IRM, n—amaterialof
bility of regulatory limitations prior to use.
known purity and concentration obtained either from the
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This test method is under the jurisdiction ofASTM Committee D19 on Water contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor Standards volume information, refer to the standard’s Document Summary page on
Organic Substances in Water. the ASTM website.
3
Current edition approved Feb. 1, 2016. Published May 2016. Originally Available from National Technical Information Service (NTIS), U.S. Depart-
ɛ3
approved in 2009. Last previous edition approved in 2009 as D7600 – 09 . DOI: ment of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://
10.1520/D7600-16. www.epa.gov/epawaste/hazard/testmethods/index.htm.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D7600−16
TABLE 1 Detection Verification Level and Reporting Range
SRM transitions utilizing an external calibration. The final
Analyte DVL (ng/L) Reporting Range (µg/L) report issued for each sample lists the concentration of
Aldicarb 100 1–100
aldicarb, carbofuran, oxamyl, methomyl and the BDMC sur-
Carbofuran 100 1–100
rogate recovery.
Oxamyl 100 1–100
Methomyl 100 1–100
5. Significance and Use
5.1 The N-methyl carbamate (NMC) pesticides: aldicarb,
carbaryl, carbofuran, formetanate hydrochloride, methiocarb,
methomyl, oxamyl, pirimicarb, propoxur, and thiodicarb have
NationalI
...
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.
´3
Designation: D7600 − 09 D7600 − 16
Standard Test Method for
Determination of Aldicarb, Carbofuran, Oxamyl and
Methomyl by Liquid Chromatography/Tandem Mass
1
Spectrometry
This standard is issued under the fixed designation D7600; 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
ε NOTE—This test method was changed editorially in February 2012.
2
ε NOTE—Table 1 was editorially corrected in May 2013.
3
ε NOTE—Added research report footnote to Section 16 editorially in June 2013.
1. Scope
1.1 This procedure covers the determination of aldicarb, carbofuran, oxamyl and methomyl (referred to collectively as
carbamates in this test method) in surface water by direct injection using liquid chromatography (LC) and detected with tandem
mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this test method. This test method
adheres to multiple reaction monitoring (MRM) mass spectrometry.
1.2 This test method has been developed by US EPA Region 5 Chicago Regional Laboratory (CRL).
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 The Detection Verification Level (DVL) and Reporting Range for the carbamates are listed in Table 1.
1.4.1 The DVL is required to be at a concentration at least 3 times below the Reporting Limit (RL) and have a signal/noise ratio
greater than 3:1. Fig. 1 displays the signal/noise ratios of the primary single reaction monitoring (SRM) transitions and Fig. 2
displays the confirmatory SRM transitions at the DVLs for the carbamates.
1.4.2 The reporting limit is the concentration of the Level 1 calibration standard as shown in Table 2 for the carbamates.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water
D3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
E2554 Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques
3
2.2 Other Documents:
EPA publication SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.
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. 1, 2009Feb. 1, 2016. Published January 2010May 2016. Originally approved in 2009. Last previous edition approved in 2009 as D7600
ɛ3
– 09 . DOI: 10.1520/D7600-09E03.10.1520/D7600-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from National Technical Information Service (NTIS), U.S. Department of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://www.epa.gov/
epawaste/hazard/testmethods/index.htm.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D7600 − 16
TABLE 1 Detection Verification Level and Reporting Range
Analyte DVL (ng/L)† Reporting Range (μg/L)
Analyte DVL (ng/L) Reporting Range (μg/L)
Aldicarb 100 1–100
Carbofuran 100 1–100
Oxamyl 100 1–100
Methomyl 100 1–100
† Measurement editorially corrected.
3.2 Definitions:Definitions of Terms Specific to This Standard:
3.2.1 detection verification level (DVL),level, DVL, n—a concentration that has a signal/noise rati
...
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