ASTM_D_7644_-_16.pdf

Designation:D764416Standard Test Method forDetermination of Bromadiolone,Brodifacoum,Diphacinoneand Warfarin in Water by Liquid Chromatography/TandemMass Spectrometry(LC/MS/MS)1This standard is issued under the fixed designation D7644;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 Thisprocedurecoversthedeterminationofbromadiolone,brodifacoum,diphacinone and warfarin(re-ferred to collectively as rodenticides in this test method)inwater by direct injection using liquid chromatography(LC)anddetected with tandem mass spectrometry(MS/MS).Theseanalytes are qualitatively and quantitatively determined by thistest method.This test method adheres to multiple reactionmonitoring(MRM)mass spectrometry.1.2 The Detection Verification Level(DVL)and ReportingRange for the rodenticides 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 rodenticides.1.2.2 The reporting limit was calculated from the concen-tration of the Level 1 calibration standard,as shown in Table 4,accounting for the dilution of a 40 mL water sample up to afinal volume of 50 mL with methanol to ensure analytesolubility.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:3U.S.EPA publication SW-846 Test Methods for EvaluatingSolid Waste,Physical/Chemical Methods3.Terminology3.1 Definitions:3.1.1 For definitions of terms used in this standard,refer toTerminology D1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 detection verification level,DVL,na concentrationthat has a signal/noise(S/N)ratio greater than 3:1 and is at least3 times below the Reporting Limit(RL).3.2.2 independent reference material,IRM,na material ofknown purity and concentration obtained either from the1This 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 Feb.1,2016.Published May 2016.Originallyapproved in 2010.Last previous edition approved in 2010 as D7644 102.DOI:10.1520/D7644-16.2For 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 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 National Institute of Standards and Technology(NIST)or otherreputable supplier.The IRM shall be obtained from a differentlot of material than is used for calibration.3.2.3 reporting limit,RL,nthe concentration of thelowest-level calibration standard used for quantification ac-counting for the sample dilution.3.2.3.1 DiscussionIn this test method,a 40 mL samplealiquot is diluted to a 50 mL final volume after thoroughlyrinsing the collection vial with methanol for quantitativetransfer.In this case,the lowest calibration level of 100 pptwould allow a reporting limit of 125 ppt to be achieved.3.2.4 rodenticides,nin this test method,bromadiolone,brodifacoum,diphacinone,and warfarin collectively.3.3 Acronyms:3.3.1 CCC,nContinuing Calibration Check3.3.2 IC,nInitial Calibration3.3.3 LC,nLiquid Chromatography3.3.4 LCS