1、Designation:D7598092Standard Test Method forDetermination of Thiodiglycol in Water by Single ReactionMonitoring Liquid Chromatography/Tandem MassSpectrometry1This standard is issued under the fixed designation D7598;the number immediately following the designation indicates the year oforiginal adopt
2、ion 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 f
3、ootnote to Section 16 editorially in June 2013.1.Scope1.1 This procedure covers the determination of thiodiglycol(TDG)in surface water by direct injection using liquidchromatography(LC)and detected with tandem mass spec-trometry(MS/MS).TDG is qualitatively and quantitativelydetermined by this method
4、.This method adheres to singlereaction monitoring(SRM)mass spectrometry.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 Detecti
5、on Verification Level(DVL)and ReportingRange for TDG 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/noiseratio greater than 3:1.Fig.1 displays the signal/noise ratio atthe DVL.1.4.2 The RL is the concentration o
6、f the level 1 calibrationstandard as shown in Table 2.The reporting limit for thismethod is 100 g/L.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
7、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 Wat
8、erD3856 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 Esti
9、mating 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 Methods33.Terminology3.1 Definitions:3.1.1 detection verification level(DVL),na concentrationthat h
10、as 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.1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct respo
11、nsibility of Subcommittee D19.06 on Methods forAnalysis forOrganic Substances in Water.Current edition approved Dec.1,2009.Published January 2010.DOI:10.1520/D7598-09E02.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual B
12、ook 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.Cop
13、yright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 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 thiodiglycol analysis,samples are
14、 shipped to the labbetween 0C and 6C and analyzed within 7 days of collection.In the lab,the samples are spiked with surrogate,filtered usinga syringe driven Millex HV PVDF filter unit and analyzeddirectly by LC/MS/MS.4.3 Thiodiglycol and 3,3-thiodipropanol(surrogate)areidentified by retention time
15、and one SRM transition.The targetanalyte and surrogate are quantitated using the SRM transitionsutilizing an external calibration.The final report issued foreach sample lists the concentration of TDG and the 3,3-thiodipropanol surrogate recovery.5.Significance and Use5.1 Thiodiglycol is a Schedule 2
16、 compound under theChemical Weapons Convention(CWC).Schedule 2 chemicalsinclude those that are precursors to chemical weapons,chemi-cal weapons agents or have a number of other commercialuses.They are used as ingredients to produce insecticides,herbicides,lubricants,and some pharmaceutical products.Schedule 2 chemicals can be found in applications unrelated tochemical weapons.Thiodiglycol is both a mustard gas precur-sor and degradant as well as an ingredient in water-based inks,ballpoint pen in
