1、Designation:D7600093Standard Test Method forDetermination of Aldicarb,Carbofuran,Oxamyl andMethomyl by Liquid Chromatography/Tandem MassSpectrometry1This standard is issued under the fixed designation D7600;the number immediately following the designation indicates the year oforiginal adoption or,in
2、 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.1NOTEThis test method was changed editorially in February 2012.2NOTETable 1 was editorially correcte
3、d in May 2013.3NOTEAdded research report footnote to Section 16 editorially in June 2013.1.Scope1.1 This procedure covers the determination of aldicarb,carbofuran,oxamyl and methomyl(referred to collectively ascarbamates in this test method)in surface water by directinjection using liquid chromatogr
4、aphy(LC)and detected withtandem mass spectrometry(MS/MS).These analytes are quali-tatively and quantitatively determined by this method.Thismethod adheres to multiple reaction monitoring(MRM)massspectrometry.1.2 This test method has been developed by US EPARegion5 Chicago Regional Laboratory(CRL).1.
5、3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4 The Detection Verification Level(DVL)and ReportingRange for the carbamates are listed in Table 1.1.4.1 The DVL is required to be at a concentration at least3 times below the R
6、eporting 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)transi-tions and Fig.2 displays the confirmatory SRM transitions atthe DVLs for the carbamates.1.4.2 The reporting limit is the concentration of the Le
7、vel 1calibration standard as shown in Table 2 for the carbamates.1.5 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
8、-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 WaterD3856 Guide for Management System
9、s in LaboratoriesEngaged in Analysis of WaterD3694 Practices for Preparation of Sample Containers andfor Preservation of Organic ConstituentsD5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water AnalysisE2554 Practice for Estimating and Monitoring the Uncer-tai
10、nty of Test Results of a Test Method Using ControlChart Techniques2.2 Other Documents:EPA publication SW-846 Test Methods for Evaluating SolidWaste,Physical/Chemical Methods33.Terminology3.1 Definitions:3.1.1 detection verification level(DVL),na concentrationthat has a signal/noise ratio greater tha
11、n 3:1 and is at least 3times below the reporting limit(RL).3.1.2 reporting limit(RL),nthe concentration of thelowest-level calibration standard used for quantification.3.1.3 carbamates,nin this test method,aldicarb,carbofuran,oxamyl and methomyl collectively.3.2 Abbreviations:1This test method is un
12、der 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 Dec.1,2009.Published January 2010.DOI:10.1520/D7600-09E03.2For referenced ASTM standards,visit the ASTM website,ww
13、w.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,
14、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 3.2.1 pptparts per trillion,ng/L3.2.2 NDnon-detect4.Summary of Test Methods4.1 This is a performance-based method and m
15、odificationsare allowed to improve performance.4.2 For carbamate analysis,samples are shipped to the labbetween 0C and 6C and analyzed within 7 days of collection.In the lab,the samples are spiked with surrogate,filtered usinga syringe driven Millex HV PVDF filter unit and analyzeddirectly by LC/MS/
16、MS.4.3 Aldicarb,carbofuran,oxamyl,methomyl and 4-bromo-3,5-dimethylphenyl-N-methylcarbamate(BDMC,surrogate)are identified by retention time and two SRM transitions.Thetarget analytes and surrogate are quantitated using the primarySRM transitions utilizing an external calibration.The finalreport issued for each sample lists the concentration ofaldicarb,carbofuran,oxamyl,methomyl and the BDMC sur-rogate recovery.5.Significance and Use5.1 The N-methyl carbamate(NMC)pesticides:aldicarb,carbaryl,carb
