ASTM_D_7485_-_16.pdf

Designation:D748516Standard Test Method forDetermination of Nonylphenol,p-tert-Octylphenol,Nonylphenol Monoethoxylate and Nonylphenol Diethoxylatein Environmental Waters by Liquid Chromatography/TandemMass Spectrometry1This standard is issued under the fixed designation D7485;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 test method covers the determination of nonylphe-nol(NP),nonylphenol ethoxylate(NP1EO),nonylphenol di-ethoxylate(NP2EO),and octylphenol(OP),extracted fromwater utilizing solid phase extraction(SPE),separated usingliquid chromatography(LC)and detected with tandem massspectrometry(MS/MS).These compounds are qualitativelyand quantitatively determined by this method.This methodadheres to single reaction monitoring(SRM)mass spectrom-etry.1.2 The method detection limit(MDL)and reporting limit(RL)for NP,NP1EO,NP2EO,and OP are listed in Table 1.1.3 The values stated in SI units are to be regarded asstandard.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 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 nonylphenol,NP,nis a mixture of branchedp-nonylphenol isomers.Commercial NP is produced by thereaction of phenol with commercial nonene.Commercialnonene is not simply a linear C9H18 alpha olefin;it is acomplex mixture of predominantly nine-carbon olefins,calledpropylene trimer,containing no linear isomers.This synthesisresults in a mixture of various branched nonylphenol isomersrather than a discrete chemical structure.The branched nonylgroup is positioned predominantly in the para position on thephenol ring.3.2.3 octylphenol,OP,ncommercial octylphenol is pro-duced by the reaction of phenol and diisobutylene to producepredominantly the 4-(1,1,3,3-tetramethylbutyl)phenol isomer.3.2.4 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: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 Feb.1,2016.Published March 2016.Originallyapproved in 2009.Last previous edition approved in 2009 as D7485 09.DOI:10.1520/D7485-16.2For 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 3.3.1 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 NP1EO,nrepresentsbranchednonylphenolmonoethoxylate.3.3.13 NP2EO,nrepresents branched nonylphenol di-ethoxylate.3.3.14 n-NP2EO,nrepresents normal straight chain non-ylphenol diethoxylate.n-NP2EO is used in this method as asurrogate.It is not produced commercially and is not expectedto be found in environmental waters.3.3.15 P&A,nPrecision and Accuracy3.3.16 PPB,n