1、Designation:D802516Standard Test Method forDetermination of Select Pesticides in Water by MultipleReaction Monitoring Liquid Chromatography Tandem MassSpectrometry1This standard is issued under the fixed designation D8025;the number immediately following the designation indicates the year oforiginal
2、 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 a method for analysis of selectedpesticides in a wat
3、er matrix by filtration followed with liquidchromatography/electrospray ionization tandem mass spec-trometry analysis.The samples are prepared in 20%methanol,filtered,and analyzed by liquid chromatography/tandem massspectrometry.This method was developed for an agriculturalrun-off study,not for low
4、level analysis of pesticides indrinking water.This method may be modified for lower levelanalysis.The analytes are qualitatively and quantitativelydetermined by this method.This method adheres to multiplereaction monitoring(MRM)mass spectrometry.1.2 A full collaborative study to meet the requirement
5、s ofPractice D2777 has not been completed.This standard containssingle-operator precision and bias based on single-operatordata.Publication of standards that have not been fully validatedis done to make the current technology accessible to users ofstandards,and to solicit additional input from the u
6、ser com-munity.1.3 A reporting limit check sample(RLCS)is analyzedduring every batch to ensure that if an analyte was present ina sample at or near the reporting limit it would be positivelyidentified and accurately quantitated within set quality controllimits.Amethod detection limit(MDL)study was n
7、ot done forthis method,the method detection limits would be much lowerthan the reporting limits in this method and would be irrel-evant.A RLCS was determined to be more applicable for thisstandard.If this method is adapted to report much lower or nearthe MDL then a MDL study would be warranted.1.4 U
8、nitsThe values stated in SI units are to be regardedas standard.No other units of measurement are included in thisstandard.1.5 The Reporting Range for the target analytes are listed inTable 1.1.5.1 The reporting limit in this test method is the minimumvalue below which data are documented as non-det
9、ects.Thereporting limit is calculated from the concentration of the Level1 calibration standard as shown in Table 6 after taking intoaccount an 8 mL water sample volume and a final dilutedsample volume of 10 mL(80%water/20%methanol).1.6 This standard does not purport to address all of thesafety conc
10、erns,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 Sp
11、ecification for Reagent WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD4841 Practice for Estimation of Holding Time for WaterSamples Containing Organic and I
12、norganic 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 Document:EPA publication SW-846 Test Methods
13、 for Evaluating SolidWaste,Physical/Chemical Methods33.Terminology3.1 Definitions:1This 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 June 1,20
14、16.Published August 2016.DOI:10.1520/D8025-16.2For 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 Nati
15、onal 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.htmCopyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 3.1.1 For definiti
16、ons of terms used in this standard,refer toTerminology D1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 batch QC,nall the quality control samples andstandards included in an analytical procedure.3.2.2 independent reference material,IRM,na material ofknown purity and concentration obtained either from theNational Institute of Standards and Technology(NIST)or otherreputable supplier.3.2.2.1 DiscussionThe IRM shall be obtained from adifferent lot of material than is used for calibrati
