ASTM_D_7574_-_16.pdf

Designation:D757416Standard Test Method forDetermination of Bisphenol A in Environmental Waters byLiquid Chromatography/Tandem Mass Spectrometry1This standard is issued under the fixed designation D7574;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 procedure covers the determination of bisphenol A(BPA)extracted from water utilizing solid phase extraction(SPE),separated using liquid chromatography(LC)and de-tected with tandem mass spectrometry(MS/MS).BPA isqualitatively and quantitatively determined by this method.This method adheres to multiple reaction monitoring(MRM)mass spectrometry.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 The method detection limit(MDL)and reporting limit(RL)for BPA are listed in Table 1.1.4 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 WaterD5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water AnalysisD5905 Practice for the Preparation of Substitute Wastewater2.2 Other Documents:3The Code of Federal Regulations 40 CFR Part 136,Appen-dix B3.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 environmental water,nshall refer to water testedusing this method.See Section 5.3.2.2 independent reference material,IRM,na material ofknown purity and concentration obtained either from theNational Institute of Standards and Technology(NIST)or otherreputable supplier.The IRM shall be obtained from a differentlot of material than is used for calibration.3.3 Acronyms:3.3.1 CCC,nContinuing Calibration Check3.3.2 IC,nInitial Calibration3.3.3 LC,nLiquid Chromatography3.3.4 LCS/LCSD,nLaboratoryControlSample/Laboratory Control Sample Duplicate3.3.5 MDL,nMethod Detection Limit3.3.6 MeOH,nMethanol3.3.7 mM,nmillimolar,1 10-3moles/L3.3.8 MRM,nMultiple Reaction Monitoring3.3.9 MS/MSD,nMatrix Spike/Matrix Spike Duplicate3.3.10 NA,adjNot Available3.3.11 ND,nnon-detect3.3.12 P&A,nPrecision and Accuracy3.3.13 PPB,nparts per billion3.3.14 PPT,nparts per trillion3.3.15 QA,adjQuality Assurance3.3.16 QC,adjQuality Control1This 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 March 2016.Originallyapproved in 2009.Last previous edition approved in 2009 as D7574 09.DOI:10.1520/D7574-16.2For 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 U.S.Government Printing Office Superintendent of Documents,732 N.Capitol St.,NW,Mail Stop:SDE,Washington,DC 20401,http:/www.access.gpo.gov.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 3.3.17 RL,nReporting Limit3.3.18 RSD,nRelative Standard Deviation3.3.19 RT,nRetention Time3.3.20 SDS,nSafety Data Sheets3.3.21 SRM,nSingle Reaction Monitoring3.3.22 SS,nSurrogate Standard3.3.23 TC,nTarget Compound3.3.24 M,nmicromolar,1 10-6moles/L3.3.25 VOA,nVolatile Organic Analysis4.Summary of Test Method4.1 This is a performance based method and modificationsare allowed to improve performance.4.2 Solid phase extraction is used to extract water samples.4.2.1 Solid Phase Extraction250 milliliter volume ofsample adjusted to pH 2 is extracted using a solid phaseextraction cartridge.The resulting methyl tert-butyl ether(MTBE)extract is solvent exchanged into methanol,concen-trated to a volume of 0.2 mL,brought to a final volume of 1 mLwith water and then analyzed by LC/MS/MS operated in themultiple reaction monitoring(MRM)mode.4.3 The target compound,surrogate and internal standardsare identified by retention time and two SRM transitions.Thetarget analyte and surrogate are quantitated using the primarySRM transitions utilizing internal standard calibration.Thefinal report issued for