Standard Historical Last Updated: May 13, 2013
ASTM D7600-09e1

Standard Test Method for Determination of Aldicarb, Carbofuran, Oxamyl and Methomyl by Liquid Chromatography/Tandem Mass Spectrometry

Significance and Use

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 NMCs 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.

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.

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.

TABLE 1 Detection Verification Level and Reporting Range

AnalyteDVL (μg/L)Reporting Range (μg/L)
Aldicarb1001100
Carbofuran1001100
Oxamyl1001100
Methomyl1001100

TABLE 2 Concentrations of Calibration Standards (PPB)

Analyte/Surrogate LV 1LV 2LV 3LV 4LV 5LV 6
Aldicarb15102550100
Carbofuran15102550100
Oxamyl15102550100
Methomyl15102550100
BDMC (Surrogate)2102050100200


FIG. 1 Example Primary SRM Chromatograms Signal/Noise Ratios


FIG. 2 Example Confirmatory SRM Chromatograms Signal/Noise Ratios

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Details
Book of Standards Volume: 11.02
Developed by Subcommittee: D19.06
Pages: 10
DOI: 10.1520/D7600-09E01
ICS Code: 13.060.50