ASTM_D_7645_-_14.pdf

Designation:D764514Standard Test Method forDetermination of Aldicarb,Aldicarb Sulfone,AldicarbSulfoxide,Carbofuran,Methomyl,Oxamyl,and Thiofanox inWater by Liquid Chromatography/Tandem MassSpectrometry(LC/MS/MS)1This standard is issued under the fixed designation D7645;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope1.1 This procedure covers the determination of aldicarb,aldicarb sulfone,aldicarb sulfoxide,carbofuran,methomyl,oxamyl,and thiofanox(referred to collectively as carbamatesin this test method)in water by direct injection using liquidchromatography(LC)and detected with tandem mass spec-trometry(MS/MS).These analytes are qualitatively and quan-titatively determined by this method.This test method adheresto multiple reaction monitoring(MRM)mass spectrometry.1.2 The Detection Verification Level(DVL)and ReportingRange for the carbamates are listed in Table 1.1.2.1 The DVL is required to be at a concentration at least3 times below the Reporting Limit(RL)and have a signal/noise ratio greater than 3:1.Fig.1 displays the signal/noiseratios of the primary single reaction monitoring(SRM)transitions,and Fig.2 displays the confirmatory SRM transi-tions at the DVLs for the carbamates.1.2.2 The reporting limit is the concentration of the Level 1calibration standard as shown in Table 2 for the carbamates.1.3 UnitsThe values stated in SI units are to be regardedas standard.No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD3694 Practices for Preparation of Sample Containers andfor Preservation of Organic ConstituentsD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD4841 Practice for Estimation of Holding Time for WaterSamples Containing Organic and Inorganic ConstituentsD5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water AnalysisE2554 Practice for Estimating and Monitoring the Uncer-tainty of Test Results of a Test Method Using ControlChart Techniques2.2 Other Documents:3EPA Publication SW-846 Test Methods for Evaluating SolidWaste,Physical/Chemical MethodsEPA Method 531 Measurement of N-Methyl Carbamoylox-imes and N-Methyl Carbamates in Drinking Water byDirect Aqueous Injection HPLC with Post Column De-rivatizationEPAMethod531.2 MeasurementofN-Methylcarbamoyloximes and N-Methylcarbamates inWater by Direct Aqueous Injection HPLC with Postcol-umn Derivatization1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.06 on Methods forAnalysis forOrganic Substances in Water.Current edition approved Jan.1,2014.Published March 2014.Originallyapproved in 2010.Last previous edition approved in 2010 as D7645 101.DOI:10.1520/D7645-14.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.3Available from National Technical Information Service(NTIS),U.S.Depart-ment 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 States1 EPA Method 538 Determination of Selected Organic Con-taminants in Drinking Water by Direct Aqueous Injection-Liquid Chromatography/Tandem Mass Spectrometry(DAI-LC/MS/MS)3.Terminology3.1 Definitions:3.1.1 carbamates,nin this test method,aldicarb,aldicarbsulfone,aldicarb sulfoxide,carbofuran,methomyl,oxamyl,and thiofanox collectively.3.1.2 detection verification level,DVL,na concentrationthat has a signal/noise ratio greater than 3:1 and is at least 3times below the Reporting Limit(RL).3.1.3 reporting limit,RL,nthe concentration of thelowest-level calibration standard used for quantification.3.2 Abbreviations:3.2.1 mMmillimolar,1 10-3moles/L3.2.2 NDnon-detect3.2.3 pptparts per trillion,ng/L4.Summary of Test Method4.1 This is a performance-based method,and modificationsare allowed to improve performance.4.2 For carbamate analysis,samples are shipped to the labacidified between 0C and 6C and analyzed within 14 days ofcollection.In the lab,the samples are spiked with surrogates,filtere