ASTM_D_7742_-_11.pdf

Designation:D774211Standard Practice forDetermination of Nonylphenol Polyethoxylates(NPnEO,3#n#18)and Octylphenol Polyethoxylates(OPnEO,2#n#12)in Water by Single Reaction Monitoring(SRM)LiquidChromatography/Tandem Mass Spectrometry(LC/MS/MS)1This standard is issued under the fixed designation D7742;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 nonylphenolpolyethoxylates(NPnEO,3 n 18)and octylphenol poly-ethoxylates(OPnEO,2 n 12)in water by Single ReactionMonitoring(SRM)Liquid Chromatography/Tandem MassSpectrometry(LC/MS/MS)using direct injection liquid chro-matography(LC)and detected with tandem mass spectrometry(MS/MS)detection.This is a screening Practice with qualifiedquantitative data to check for the presence of longer chainethoxylates in a water sample.1.1.1 All data are qualified because neat standards of eachalkylphenol ethoxylate(APEO)are not available and thesynthesis and characterization of these neat standards would bevery expensive.The Igepal Brand standards,which contain amixture of various chain lengths of the alkylphenol ethoxylates(APEOs),were used.The mixture was characterized in-houseassuming the instrument response at an optimum electrosprayionization cone and collision voltage for each APEO was thesame.This assumption,which may not be accurate,is used todetermine qualified amounts of each ethoxylate in the stan-dards.The n-Nonylphenol diethoxylate(n-NP2EO)surrogatewas available as a neat characterized standard,therefore,thisconcentration and recovery data was not estimated.APEOs arenot regulated by the EPA,but nonylphenol,a breakdownproduct of NPnEOs,is regulated for fresh and saltwaterdischargers.A request by a sewage treatment plant(STP)wasmade to make this Practice available throughASTM in order toscreen for the influent or effluent from sources of APEOscoming into the STP.The interest lies in stopping the source ofthe longer chainAPEOs from entering the STPin order to meeteffluent guidelines.Based upon the above,this is a Practicerather than a Standard Method.Acomparison between samplesis possible using this Practice to determine which has a higherconcentration of APEOs.1.2 UnitsThe values stated in SI units are to be regardedas standard.No other units of measurement are included in thisPractice.1.3 The estimated screening range shown in Table 1 wascalculated from the concentration of the Level 1 and 7calibration standards shown in Table 4.These numbers arequalified,as explained in Section 1,and must be reported assuch.Figs.1-5 show the SRM chromatograms of each analyteat the Level 1 concentration with the signal to noise(S/N)ratio.This is a screening Practice and method detection limits are notgiven.The S/N ratio for each analyte at the Level 1 concen-tration must be at least 5:1 for adequate sensitivity.If theinstrument can not meet the criteria,the screening limit mustbe raised to an acceptable level.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:2D1193 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 AnalysisE2554 Practice for Estimating and Monitoring the Uncer-tainty of Test Results of a Test Method Using ControlChart Techniques1This Practice is under the jurisdiction of ASTM Committee D19 on Water andis the direct responsibility of Subcommittee D19.06 on Methods for Analysis forOrganic Substances in Water.Current edition approved June 15,2011.Published July 2011.DOI:10.1520/D7742-11.2For 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 2.2 Other Standard:3EPA SW-846 Test Methods for Evaluating Solid Waste,Physical/Chemical Methods3.Terminology3.1 Definitions:3.1.1 Screening Limit,SL,nthe estimated concentration ofthe lowest-level calibration standard used for quantificationaccounting for the sample dilution.3.1.2 Alkylphenol Ethoxylates,nin this Practice,nonyl-phenol polyethoxy