ASTM D7600-09e2
(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 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 method. This 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. TABLE 1 Detection Verification Level and Reporting Range
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.
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.
FIG. 1 Example Primary SRM Chromatograms Signal/Noise Ratios
FIG. 2 Example Confirmatory SRM Chromatograms Signal/Noise Ratios
1.4.2 The reporting limit is the concentration of the Level 1 calibration standard as shown in Table 2 for the carbamates.TABLE 2 Concentrations of Calibration Standards (PPB)
Analyte/Surrogate
LV 1
LV 2
LV 3
LV 4
LV 5
LV 6
Aldicarb
1
5
10
25
50
100
Carbofuran
1
5
10
25
50
100
Oxamyl
1
5
10
25
50
100
Methomyl
1
5
10
25
50
100
BDMC (Surrogate)
2
10
20
50
100
200
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.
General Information
Relations
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
´2
Designation:D7600 −09
StandardTest 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
ε NOTE—This test method was changed editorially in February 2012.
2
ε NOTE—Table 1 was editorially corrected in May 2013.
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
tatively and quantitatively determined by this method. This
Engaged in Analysis of Water
method adheres to multiple reaction monitoring (MRM) mass
D3694Practices for Preparation of Sample Containers and
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
E2554Practice for Estimating and Monitoring the Uncer-
1.3 The values stated in SI units are to be regarded as
tainty of Test Results of a Test Method in a Single
standard. No other units of measurement are included in this
Laboratory Using a Control Sample Program
standard.
2.2 Other Documents:
1.4 The Detection Verification Level (DVL) and Reporting EPApublication SW-846Test Methods for Evaluating Solid
3
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. Terminology
3 times below the Reporting Limit (RL) and have a signal/
3.1 Definitions:
noise ratio greater than 3:1. Fig. 1 displays the signal/noise
ratios of the primary single reaction monitoring (SRM) transi- 3.1.1 detection verification level (DVL), n—a concentration
that has a signal/noise ratio greater than 3:1 and is at least 3
tions and Fig. 2 displays the confirmatory SRM transitions at
times below the reporting limit (RL).
the DVLs for the carbamates.
1.4.2 The reporting limit is the concentration of the Level 1 3.1.2 reporting limit (RL), n—the concentration of the
lowest-level calibration standard used for quantification.
calibration standard as shown in Table 2 for the carbamates.
3.1.3 carbamates, n—in this test method, aldicarb,
1.5 This standard does not purport to address all of the
carbofuran, oxamyl and methomyl collectively.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3.2 Abbreviations:
priate safety and health practices and determine the applica- 3.2.1 ppt—parts per trillion, ng/L
bility of regulatory limitations prior to use.
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
1
This test method is under the jurisdiction ofASTM Committee D19 on Water Standards volume information, refer to the standard’s Document Summary page on
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor the ASTM website.
3
Organic Substances in Water. Available from National Technical Information Service (NTIS), U.S. Depart-
Current edition approved Dec. 1, 2009. Published January 2010. DOI: 10.1520/ ment of Commerce, 5285 Port Royal Road, Springfield, VA, 22161 or at http://
D7600-09E02. 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 ----------------------
´2
D7600−09
TABLE 1 Detection Verification Level and Reporting Range
6.2 All glassware is washed in hot water with a detergent,
Analyte DVL (ng/L)† Reporting Range (µg/L) rinsed in hot water followed by distilled water. The glassware
Aldicarb 100 1–100
is then dried and heated in an oven at 250°C for 15 to 30
Carbofuran 100 1–100
minutes. All glassware is subsequently cleaned with acetone,
Oxamyl 100 1–100
Methomyl 100 1–100 then methanol.
† Measurement editorially corrected.
6.3 All reagents and solvents should be pesticide residue
purity or higher to minimize interference problems.
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.