ASTM D7645-10e1
(Test Method)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)
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
This test method has been developed by US EPA Region 5 Chicago Regional Laboratory (CRL).
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.
This 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 test method 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 method. This 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.
TABLE 1 Detection Verification Level and Reporting Range AnalyteDVL
(ng/L)Reporting Range
(μg/L) Aldicarb2501-100 Aldicarb Sulfone2501-100 Aldicarb Sulfoxide2501-100 Carbofuran2501-100 Methomyl2501-100 Oxamyl2501-100 Thiofanox2501-100
TABLE 2 Concentrations of Calibration Standards (PPB) Analyte/SurrogateLV 1LV 2LV 3LV 4LV 5LV 6LV 7LV 8 Aldicarb151025355075100 Aldicarb Sulfone151025355075100 Aldicarb Sulfoxide151025355075100 Carbofuran151025355075100 Methomyl151025355075100 Oxamyl151025355075100 Thiofanox151025355075100 Carbofuran-13C6 (Surrogate)151025355075100 Methomyl-13C2,15N (Surrogate)151025355075100
FIG. 1 Example Primary SRM Chromatograms Signal/Noise Ratios
FIG. 2 Example Confirmatory SRM Chromatograms Signal/Noise Ratios
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Designation:D7645 −10
StandardTest Method for
Determination of Aldicarb, Aldicarb Sulfone, Aldicarb
Sulfoxide, Carbofuran, Methomyl, Oxamyl and Thiofanox in
Water by Liquid Chromatography/Tandem Mass
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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.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
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´ NOTE—This Test Method was changed editorially in 2012.
1. Scope 2. Referenced Documents
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1.1 This test method covers the determination of aldicarb, 2.1 ASTM Standards:
aldicarb sulfone, aldicarb sulfoxide, carbofuran, methomyl, D1129Terminology Relating to Water
oxamyl, and thiofanox (referred to collectively as carbamates D1193Specification for Reagent Water
in this test method) in water by direct injection using liquid D2777Practice 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- D3694Practices for Preparation of Sample Containers and
titatively determined by this method. This method adheres to for Preservation of Organic Constituents
multiple reaction monitoring (MRM) mass spectrometry. D3856Guide for Management Systems in Laboratories
Engaged in Analysis of Water
1.2 The Detection Verification Level (DVL) and Reporting
D4841Practice for Estimation of Holding Time for Water
Range for the carbamates are listed in Table 1.
Samples Containing Organic and Inorganic Constituents
1.2.1 The DVL is required to be at a concentration at least
D5847Practice for Writing Quality Control Specifications
3 times below the Reporting Limit (RL) and have a signal/
for Standard Test Methods for Water Analysis
noise ratio greater than 3:1. Fig. 1 displays the signal/noise
E2554Practice for Estimating and Monitoring the Uncer-
ratios of the primary single reaction monitoring (SRM)
tainty of Test Results of a Test Method in a Single
transitions, and Fig. 2 displays the confirmatory SRM transi-
Laboratory Using a Control Sample Program
tions at the DVLs for the carbamates.
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2.2 Other Documents:
1.2.2 The reporting limit is the concentration of the Level 1
EPApublication SW-846Test Methods for Evaluating Solid
calibration standard as shown in Table 2 for the carbamates.
Waste, Physical/Chemical Methods
1.3 Units—The values stated in SI units are to be regarded
EPA Method 531Measurement of N-Methyl Carbamoylox-
asstandard.Nootherunitsofmeasurementareincludedinthis
imes and N-Methyl Carbamates in Drinking Water by
standard.
Direct Aqueous Injection HPLC with Post Column De-
1.4 This standard does not purport to address all of the
rivatization
safety concerns, if any, associated with its use. It is the
EPA Method 531.2 Measurement of
responsibility of the user of this standard to establish appro-
N-Methylcarbamoyloximes and N-Methylcarbamates in
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
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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
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This test method is under the jurisdiction ofASTM Committee D19 on Water Standardsvolumeinformation,refertothestandard’sDocumentSummarypageon
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor the ASTM website.
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Organic Substances in Water. Available from National Technical Information Service (NTIS), U.S. Depart-
CurrenteditionapprovedJune1,2010.PublishedFebruary2012.DOI:10.1520/ ment of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://
D7645-10E01. 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
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D7645−10
TABLE 1 Detection Verification Level and Reporting Range
regulatory concern to EPA in assessing the NMC’s food,
DVL Reporting Range drinking water, and residential risks. In most of the country,
Analyte
(ng/L) (µg/L)
NMC residues in drinking water sources are at levels that are
Aldicarb 250 1-100
not likely to contribute substantially to the multi-pathway
Aldicarb Sulfone 250 1-100
cumulative exposure. Shallow private wells extending through
Aldicarb Sulfoxide 250 1-100
Carbofuran 250 1-100 highly permeable soils into shallow, acidic ground water
Methomyl 250 1-100
represent what the EPA believes to be the most vulnerable
Oxamyl 250 1-100
drinking water. Aldicarb sulfone and aldicarb sulfoxide are
Thiofanox 250 1-100
bre
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