ASTM_D_7597_-_09e2.pdf

Designation:D7597092Standard Test Method forDetermination of Diisopropyl Methylphosphonate,EthylHydrogen Dimethylamidophosphate,EthylMethylphosphonic Acid,Isopropyl Methylphosphonic Acid,Methylphosphonic Acid and Pinacolyl MethylphosphonicAcid in Water by Liquid Chromatography/Tandem MassSpectrometry1This standard is issued under the fixed designation D7597;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.1NOTEThis test method was changed editorially in February 2012.2NOTEAdded research report footnote to Section 16 editorially in June 2013.1.Scope1.1 This procedure covers the determination of diisopropylmethylphosphonate(DIMP),ethyl hydrogen dimethylami-dophosphate(EHDMAP),ethyl methylphosphonic acid(EMPA),isopropyl methylphosphonic acid(IMPA),methyl-phosphonic acid(MPA)and pinacolyl methylphosphonic acid(PMPA)(referred to collectively as organophosphonates in thistest method)in surface water by direct injection using liquidchromatography(LC)and detected with tandem mass spec-trometry(MS/MS)using electrospray ionization(ESI).Theseanalytes are qualitatively and quantitatively determined by thismethod.This method adheres to single reaction monitoring(SRM)mass spectrometry.1.2 This test method has been developed by US EPARegion5 Chicago Regional Laboratory(CRL).1.3 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 organophosphonates are listed in Table 1.1.4.1 The DVL is required to be at a concentration at leastthree times below the reporting limit(RL)and have a signal/noise ratio greater than 3:1.Fig.1 displays the signal/noiseratios at the DVLs for the organophosphonates in the ESIpositive mode and Fig.2 in the ESI negative mode.1.4.2 The reporting limit is the concentration of the Level 1calibration standard as shown in Table 2 for the organophos-phonates except for MPA in the ESI negative mode which is atLevel 2 due to not meeting the DVL criteria at the lowerconcentration level.The DVL for MPA in the ESI negativemode is at 20 g/L,which forces a raised reporting limit.However,the multi-laboratory validation required a spike of alltarget analytes at Level 1 concentrations.The mean recoveryfor MPA in the ESI negative mode at this level was 98.7%asshown in Table 3.If your instruments sensitivity can meet therequirements in this test method,MPA may have a 50 g/Lreporting limit.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-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 Systems 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 Analysis1This 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 Dec.1,2009.Published January 2010.DOI:10.1520/D7597-09E02.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 E2554 Practice for Estimating and Monitoring the Uncer-tainty 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 than 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 organophosphonates,nin this test method,diisopro-pyl methylphosphonate(DIMP),ethyl hydrogen dimethylami-dophosphate(EHDMAP),ethyl methylphosphonic acid(EMPA),isopropyl methylphosphonic acid(IMPA),methyl-phosphonic acid(MPA)and pinacolyl methylphosphonic acid(PMPA).3.2 Abbreviations:3.2.1 NDnon-detect4.Summary of Test Methods4.1 This is a performance-based method and modifications