ASTM_D_7730_-_11.pdf

Designation:D773011Standard 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 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 dioctylsulfosuccinate(DOSS)in sea water by direct injection usingliquid chromatography(LC)and detection with tandem massspectrometry(MS/MS).This analyte is qualitatively and quan-titatively determined by this method.This method adheres toselected reaction monitoring(SRM)mass spectrometry.1.2 The Detection Verification Level(DVL)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/noise ratio greater than 3:1.Fig.1 and Fig.2 display thesignal/noise ratio of the selected reaction monitoring(SRM)transition.1.2.2 The 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 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 Water2.2 Other Standards:3EPApublication SW-846,Test Methods for Evaluating SolidWaste,Physical/Chemical Methods3.Terminology3.1 Definitions:3.1.1 detection verification level,DVL,n a 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.3.2 Abbreviations:3.2.1 ppbparts per billion,g/L3.2.2 mMmillimolar,1 x 10-3moles/L3.2.3 NAno addition3.2.4 NDnon-detect4.Summary of Test Method4.1 This 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,ammonium formate buffer solution and brought to a volume of40 mL with acetonitrile.This prepared sample is then filteredusing a syringe 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.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 May 1,2011.Published July 2011.DOI:10.1520/D773011.2For 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.htmCopyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 TABLE 1 Detection Verification Level and Reporting RangeAnalyteDVL(g/L)Reporting Range(g/L)DOSS320-400FIG.1 Detection Verification Level Signal/Noise Ratio.FIG.2 Reporting Level Signal/Noise Ratio.D7730 112 5.Significance and Use5.1 DOSS is an anionic detergent that is approved by theFood and DrugAdministration and is used widely as a laxative,emulsifying,solubilizing and dispersing agent,and is used inthe cosmetic industry.4DOSS may also be used as a dispersingagent to treat oil.DOSS may be released into the environmentat levels that may be harmful to aquatic life.The US EPAaquatic life benchmark for DOSS is 40 ppb.55.2 This method has been investigated for use with reagentand sea water.6.Interferences6.1 Method interferences may be caused by contaminants insolvents,reagents,glassware,and other apparatus producingdiscret