ASTM D7645-16

Standard Test Method for Determination of Aldicarb, Aldicarb Sulfone, Aldicarb Sulfoxide, Carbofuran, Methomyl, Oxamyl, and Thiofanox in Water by Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

SIGNIFICANCE AND USE
5.1 This test method has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).  
5.2 The N-methyl carbamate (NMC) pesticides: aldicarb, carbofuran, methomyl, oxamyl, and thiofanox have been identified by EPA as working through a common mechanism. These affect the nervous system by reducing the ability of enzymes. Enzyme 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. Aldicarb sulfone and aldicarb sulfoxide are breakdown products of aldicarb and should also be monitored due to their toxicological effects.4  
5.3 This test method has been investigated for use with reagent, surface, and drinking water for the selected carbamates: aldicarb, aldicarb sulfone, aldicarb sulfoxide, carbofuran, methomyl, oxamyl, and thiofanox.
SCOPE
1.1 This procedure covers the determination of aldicarb, aldicarb sulfone, aldicarb sulfoxide, carbofuran, methomyl, oxamyl, and thiofanox (referred to collectively as carbamates in this test method) in 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 The Detection Verification Level (DVL) and Reporting Range for the carbamates are listed in Table 1.    
1.2.1 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.  
1.2.2 The reporting limit is the concentration of the Level 1 calibration standard as shown in Table 2 for the carbamates.  
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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.

General Information

• Status: Historical
• Publication Date: 31-Jan-2016
• 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

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
Designation: D7645 − 16
Standard Test Method for
Determination of Aldicarb, Aldicarb Sulfone, Aldicarb
Sulfoxide, Carbofuran, Methomyl, Oxamyl, and Thiofanox in
Water by Liquid Chromatography/Tandem Mass
1
Spectrometry (LC/MS/MS)
This standard is issued under the fixed designation D7645; 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 2. Referenced Documents
2
1.1 This procedure covers the determination of aldicarb, 2.1 ASTM Standards:
aldicarb sulfone, aldicarb sulfoxide, carbofuran, methomyl, D1129 Terminology Relating to Water
oxamyl, and thiofanox (referred to collectively as carbamates D1193 Specification for Reagent Water
in this test method) in water by direct injection using liquid D2777 Practice for Determination of Precision and Bias of
chromatography (LC) and detected with tandem mass spec- Applicable Test Methods of Committee D19 on Water
trometry (MS/MS). These analytes are qualitatively and quan- D3694 Practices for Preparation of Sample Containers and
titatively determined by this test method. This test method for Preservation of Organic Constituents
adheres to multiple reaction monitoring (MRM) mass spec- D3856 Guide for Management Systems in Laboratories
trometry. Engaged in Analysis of Water
D4841 Practice for Estimation of Holding Time for Water
1.2 The Detection Verification Level (DVL) and Reporting
Samples Containing Organic and Inorganic Constituents
Range for the carbamates are listed in Table 1.
D5847 Practice for Writing Quality Control Specifications
1.2.1 The DVL is required to be at a concentration at least
for Standard Test Methods for Water Analysis
3 times below the Reporting Limit (RL) and have a signal/
E2554 Practice for Estimating and Monitoring the Uncer-
noise ratio greater than 3:1. Fig. 1 displays the signal/noise
tainty of Test Results of a Test Method Using Control
ratios of the primary single reaction monitoring (SRM)
Chart Techniques
transitions, and Fig. 2 displays the confirmatory SRM transi-
3
2.2 Other Documents:
tions at the DVLs for the carbamates.
EPA Publication SW-846 Test Methods for Evaluating Solid
1.2.2 The reporting limit is the concentration of the Level 1
Waste, Physical/Chemical Methods
calibration standard as shown in Table 2 for the carbamates.
EPA Method 531 Measurement of N-Methyl Carbamoylox-
1.3 Units—The values stated in SI units are to be regarded
imes and N-Methyl Carbamates in Drinking Water by
as standard. No other units of measurement are included in this
Direct Aqueous Injection HPLC with Post Column De-
standard.
rivatization
1.4 This standard does not purport to address all of the
EPA Method 531.2 Measurement of
safety concerns, if any, associated with its use. It is the N-Methylcarbamoyloximes and N-Methylcarbamates in
responsibility of the user of this standard to establish appro-
Water by Direct Aqueous Injection HPLC with Postcol-
priate safety and health practices and determine the applica- umn Derivatization
bility of regulatory limitations prior to use.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This test method is under the jurisdiction of ASTM Committee D19 on Water contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for 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-
approved in 2010. Last previous edition approved in 2014 as D7645 – 14. DOI: ment of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://
10.1520/D7645-16. 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

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D7645 − 16
TABLE 1 Detection Verification Level and Reporting Range
3.3.20 SRM, n—Single Reaction Monitoring
DVL Reporting Range
3.3.21 SS, n—Surrogate Standard
Analyte
(ng/L) (µg/L)
3.3.22 TC, n—Target Compound
Aldicarb 250 1-100
-6
Aldicarb Sulfone 250 1-100
3.3.23 µM, n—micromolar, 1 × 10 moles/L
Aldicarb Sulfoxide 250 1-100
Carbofuran 250 1-100
3.3.24 VOA, n—Volatile Organic Analysis
Methomyl 250 1-100
Oxamyl 250 1-100
4. Summary of Test Method
Thiofanox 250 1-100
4.1 This is a performance-based method, and modifications
are allowed to improve performance.
4.2 For carbamate analysis, samples
...

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: D7645 − 14 D7645 − 16
Standard Test Method for
Determination of Aldicarb, Aldicarb Sulfone, Aldicarb
Sulfoxide, Carbofuran, Methomyl, Oxamyl, and Thiofanox in
Water by Liquid Chromatography/Tandem Mass
1
Spectrometry (LC/MS/MS)
This standard is issued under the fixed designation D7645; 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 procedure covers the determination of aldicarb, aldicarb sulfone, aldicarb sulfoxide, carbofuran, methomyl, oxamyl,
and thiofanox (referred to collectively as carbamates in this test method) in 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 The Detection Verification Level (DVL) and Reporting Range for the carbamates are listed in Table 1.
1.2.1 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.
1.2.2 The reporting limit is the concentration of the Level 1 calibration standard as shown in Table 2 for the carbamates.
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this
standard.
1.4 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
D3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water
D4841 Practice for Estimation of Holding Time for Water Samples Containing Organic and Inorganic 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
EPA Method 531 Measurement of N-Methyl Carbamoyloximes and N-Methyl Carbamates in Drinking Water by Direct Aqueous
Injection HPLC with Post Column Derivatization
EPA Method 531.2 Measurement of N-Methylcarbamoyloximes and N-Methylcarbamates in Water by Direct Aqueous Injection
HPLC with Postcolumn Derivatization
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 Jan. 1, 2014Feb. 1, 2016. Published March 2014May 2016. Originally approved in 2010. Last previous edition approved in 20102014 as D7645
ε1
– 1014. . DOI: 10.1520/D7645-14.10.1520/D7645-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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 ----------------------
D7645 − 16
TABLE 1 Detection Verification Level and Reporting Range
DVL Reporting Range
Analyte
(ng/L) (μg/L)
Aldicarb 250 1-100
Aldicarb Sulfone 250 1-100
Aldicarb Sulfoxide 250 1-100
Carbofuran 250 1-100
Methomyl 250 1-100
Oxamyl 250 1-100
Thiofanox 250 1-100
EPA Method 538 Determination of
...