1、Designation:D773017Standard Test Method forDetermination of Dioctyl Sulfosuccinate in Sea Water byLiquid Chromatography/Tandem Mass Spectrometry(LC/MS/MS)1This standard is issued under the fixed designation D7730;the number immediately following the designation indicates the year oforiginal adoption
2、 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 dioctylsulfosuccinate(DOSS)in sea wate
3、r by direct injection usingliquid chromatography(LC)and detection with tandem massspectrometry(MS/MS).This analyte is qualitatively and quan-titatively determined by this test method.This test methodadheres to selected reaction monitoring(SRM)mass spectrom-etry.1.2 The detection verification level(D
4、VL)and reportingrange for DOSS are listed in Table 1.1.2.1 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 and Fig.2 display the signal/noiseratio of the selected reaction monitoring(SRM)transition.1.2.2 Th
5、e reporting limit is the concentration of the Level 1calibration standard as shown in Table 5 for DOSS,taking intoaccount the 50%sample preparation dilution factor.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 stan
6、dard 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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This internat
7、ional standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade(TBT)Committ
8、ee.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 Water2.2 Other Standards:3EPA Publication SW-846 Test Methods for Evaluating Solid
9、Waste,Physical/Chemical Methods3.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 detection verification level,DVL,na concentrationthat has a signal/noise ratio greater than 3:1 and is a
10、t least 3times below the reporting limit(RL).3.2.2 reporting limit,RL,nthe concentration of thelowest-level calibration standard used for quantification.3.3 Abbreviations:3.3.1 mMmillimolar,1 103moles/L3.3.2 NAno addition3.3.3 NDnon-detect3.3.4 ppbparts per billion,g/L4.Summary of Test Method4.1 Thi
11、s is a performance-based method,and modificationsare allowed to improve performance.4.2 For DOSS analysis,samples are shipped to the labbetween 0C and 6C and analyzed within 5 days.In the lab,the entire collected 20-mL sample is spiked with surrogate,1This test method is under the jurisdiction of AS
12、TM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.06 on Methods forAnalysis forOrganic Substances in Water.Current edition approved Dec.15,2017.Published January 2018.Originallyapproved in 2011.Last previous edition approved in 2011 as D7730 11.DOI:10.1520/D7730-17.2For r
13、eferenced 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),5301 Shawne
14、eRd.,Alexandria,VA 22312,http:/www.ntis.gov.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on
15、 Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.1 ammonium formate buffer solution and brought to a volume of40 mL with acetonitrile.This prepared sample is then filteredusing a syri
16、nge driven filter unit,and analyzed by LC/MS/MS.If visible oil is present,the prepared sample is allowed to settleresulting in an oil layer at the top of the 40-mL solution.Aportion of the aqueous(bottom)layer is filtered,leaving the oillayer behind,through a syringe driven filter assembly andanalyzed by LC/MS/MS.4.3 DOSS and DOSS surrogate are quantitated by retentiontime and one SRM transition.The final report issued for eachsample lists the concentration of DOSS and the surrogaterecovery.5.Si
