ASTM_D_5315_-_04_2011.pdf

Designation:D531504(Reapproved 2011)Standard Test Method forDetermination of N-Methyl-Carbamoyloximes andN-Methylcarbamates in Water by Direct Aqueous InjectionHPLC with Post-Column Derivatization1This standard is issued under the fixed designation D5315;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 is a high-performance liquid chromatographic(HPLC)test method applicable to the determination of certainn-methylcarbamoyloximes and n-methylcarbamates in groundwater and finished drinking water(1)2.This test method isapplicable to any carbamate analyte that can be hydrolyzed toa primary amine.The following compounds have been vali-dated using this test method:AnalyteChemical Abstract ServicesRegistry NumberAAldicarb116-06-3Aldicarb sulfone1646-88-4Aldicarb sulfoxide1646-87-3Baygon114-26-1Carbaryl63-25-2Carbofuran1563-66-23-Hydroxycarbofuran16655-82-6Methiocarb2032-65-7Methomyl16752-77-5Oxamyl23135-22-0_ANumbering system of Chemical Abstracts,Inc.1.2 This test method has been validated in a collaborativeround-robin study(2)and estimated detection limits(EDLs)have been determined for the analytes listed in 1.1(Table 1).Observed detection limits may vary between ground waters,depending on the nature of interferences in the sample matrixand the specific instrumentation used.1.3 This test method is restricted to use by,or under thesupervision of,analysts experienced in both the use of liquidchromatography and the interpretation of liquid chromato-grams.Each analyst should demonstrate an ability to generateacceptable results with this test method using the proceduredescribed in 12.3.1.4 When this test method is used to analyze unfamiliarsamples for any or all of the analytes listed in 1.1,analyteidentifications should be confirmed by at least one additionalqualitative technique.1.5 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.6 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.Additional guid-ance on laboratory safety is available and suitable referencesfor the information are provided(3-5).2.Referenced Documents2.1 ASTM Standards:3D1129 Terminology Relating to WaterD1192 Guide for Equipment for Sampling Water and Steamin Closed Conduits(Withdrawn 2003)4D1193 Specification for Reagent WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD3370 Practices for Sampling Water from Closed ConduitsD3694 Practices for Preparation of Sample Containers andfor Preservation of Organic ConstituentsE682 Practice for Liquid Chromatography Terms and Rela-tionships2.2 U.S.Environmental Protection Agency Standard:EPA Method531.1,Revision3.0,USEPA,EMSL-Cincinnati,198951This 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 May 1,2011.Published June 2011.Originallyapproved in 1992.Last previous edition approved in 2004 as D5315 04.DOI:10.1520/D5315-04R11.2The boldface numbers in parentheses refer to the references at the end of thistest method.3For 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.4The last approved version of this historical standard is referenced onwww.astm.org.5Published by the U.S.Environmental Protection Agency,EnvironmentalMonitoring and Support Laboratory,Cincinnati,OH 45268,1989.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 EPA Method531.2,Revision1.0,USEPA,EMSL-Cincinnati,200163.Terminology3.1 DefinitionsFor definitions of water terms used in thistest method,refer to Terminology D1129.For definitions ofother terms used in this test method,refer to Practice E682.3.2 Definitions of Terms Specific to This Standard:3.2.1 calibration standard(CAL)a solution prepared fromthe primary dilution standard solution and stock standardsolutions of the internal standards and surrogate analytes.CALsolutions are used to calibrate the instrument response withrespect to analyte concentration.3.2.2 field duplicates(FD1 and FD2)two separate samplescollectedatthesametime,placedunderidenticalcircumstances,and treated exactly the same throughout fieldand laboratory procedures.Analyses of FD1 and FD2 providea measure of the precision a