ASTM_D_7065_-_11.pdf

Designation:D706511Standard Test Method forDetermination of Nonylphenol,Bisphenol A,p-tert-Octylphenol,Nonylphenol Monoethoxylate and NonylphenolDiethoxylate in Environmental Waters by GasChromatography Mass Spectrometry1This standard is issued under the fixed designation D7065;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 determination of nonylphenol(NP),nonylphenol ethoxylate(NP1EO),nonylphenol di-ethoxylate(NP2EO),octylphenol(OP),and bisphenolA(BPA)that are partitioned into organic solvent,separated using gaschromatography and detected with mass selective detection.These compounds or isomer mixtures are qualitatively andquantitatively determined by this method.This method adheresto selected ion monitoring mass spectrometry but full scanmass spectrometry has also been shown to work well underthese conditions.Either analysis may be used.1.2 The method detection limit(MDL)and reporting limit(RL)for NP,NP1EO,NP2EO,OP,and BPA are listed in Table1.1.3 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 to determine theapplicability of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent 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 WastewaterE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3.Terminology3.1 Definitions:3.1.1 Nonylphenol,NP,nnonylphenol is mixed isomersof branched p-nonylphenol.3.1.1.1 DiscussionCommercial nonylphenol is producedby the reaction of phenol with commercial nonene.Commer-cial nonene is not simply a linear C9H18alpha 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.3.1.2 Octylphenol,OP,nOP represents 4-(1,1,3,3-tetramethylbutyl)phenol.3.1.2.1 DiscussionCommercial octylphenol is producedby the reaction of phenol and diisobutylene to produce pre-dominantly the 4-(1,1,3,3-tetramethylbutyl)phenol isomer.3.1.3 Bisphenol A,BPA,n-BPA represents 4,4-dihydroxy-2,2-diphenylpropane.3.1.3.1 DiscussionCommercial bisphenol A is producedby the condensation reaction of phenol and acetone to producepredominantly the 4,4-dihydroxy-2,2-diphenylpropane.3.1.4 Environmental water,nit shall refer to water testedusing this method.See Section 5.3.2 Abbreviations:3.2.1 NP1EObranched nonylphenol monoethoxylate.3.2.2 NP2EObranched nonylphenol diethoxylate.3.2.3 n-NPnormal straight chain nonylphenol.3.2.3.1 Discussionn-NP is used in this method as asurrogate for NP,OP and BPA.n-NP is not produced commer-cially and is not expected to be found in environmental waters.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 15,2011.Published July 2011.Originallypublished in 2006.Last previous version approved in 2006 as D7065 06.DOI:10.1520/D7065-11.2For 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 3.2.4 n-NP1EOnormalstraightchainnonylphenolethoxylate.3.2.4.1 Discussionn-NP1EO is used in this method as asurrogate for NP1EO and NP2EO.n-NP1EO is not producedcommercially and is not expected to be found in environmentalwaters.4.Summary of Test Method4.1 This is a performance-based method and modificationsare allowed to improve performance.4.2 For NP,NP1EO,NP2EO,BPA,and OP analysis,con-tinuous liquid-liquid extraction technique is used for watersamples.4.3 Continuous Liquid-Liquid Extraction TechniqueA 1-Lvolume of sample adjusted to pH 2 is extracted with methylenechloride.The methylene chloride extract is dried using sodiumsulfate if needed,concentrated to a volume of 0.5