ASTM_D_7599_-_09e2.pdf

Designation:D7599092Standard Test Method forDetermination of Diethanolamine,Triethanolamine,N-Methyldiethanolamine and N-Ethyldiethanolamine in Waterby Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry(LC/MS/MS)1This standard is issued under the fixed designation D7599;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.1NOTEThis test method was changed editorially in February 2012.2NOTEAdded research report footnote to Section 16 editorially in June 2013.1.Scope1.1 Thisprocedurecoversthedeterminationofdiethanolamine,triethanolamine,N-methyldiethanolamine andN-ethyldiethanolamine(referred to collectively as ethano-lamines in this test method)in surface water by direct injectionusing liquid chromatography(LC)and detected with tandemmass spectrometry(MS/MS).These analytes are qualitativelyand quantitatively determined by this method.This methodadheres to single reaction monitoring(SRM)mass spectrom-etry.1.2 This test method has been developed by US EPARegion5 Chicago Regional Laboratory(CRL).1.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4 The Detection Verification Level(DVL)and ReportingRange for the ethanolamines are listed in Table 1.1.4.1 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 at the DVLs and at higher concentrations forN-methyldiethanolamine.1.4.2 The reporting limit is the concentration of the Level 1calibration standard as shown in Table 2 for diethanolamine,triethanolamine,and N-ethyldiethanolamine and Level 2 forN-methyldiethanolamine.ThereportinglimitforN-methyldiethanolamine is set at 50 g/L due to poor sensi-tivity at a 5 g/L concentration which did not meet the DVLcriteria.The DVL for N-methyldiethanolamine is at 10 g/L,which forces a raised reporting limit(chromatograms areshown in Fig.1).However,the multi-laboratory validationrequired a spike of all target analytes at 25 g/L.The meanrecovery for N-methyldiethanolamine at this level was 88%asshown in Table 3.If your instruments sensitivity can meet therequirements in this test method,N-methyldiethanolamine mayhave a 25 g/L reporting limit.1.5 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 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 Techniques2.2 Other Documents:EPA publication SW-846 Test Methods for Evaluating SolidWaste,Physical/Chemical Methods31This 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 Dec.1,2009.Published January 2010.DOI:10.1520/D7599-09E02.2For 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 3.Terminology3.1 Definitions:3.1.1 detection verification level(DVL),na concentrationthat has a signal/noise ratio greater than 3:1 and is at least 3times below the reporting limit(RL).3.1.2 reporting limit(RL),nthe concentration of thelowest-level calibration standard used for quantification.3.1.3 ethanolamines,ninthistestmethod,diethanolamine,triethanolamine,N-methyldiethanolamine andN-ethyldiethanolamine collectively.3.2 Abbreviations:3.2.1 NDnon-detect4.Summary of Test Methods4.1 This is a performance-based method and modificationsare allowed to improve performance.4.2 For ethanolamines analysis,samples are shipped to thelab between 0C and 6C and analyzed wit