1、Designation:D7731111Standard Test Method forDetermination of Dipropylene Glycol Monobutyl Ether andEthylene Glycol Monobutyl Ether in Sea Water by LiquidChromatography/Tandem Mass Spectrometry(LC/MS/MS)1This standard is issued under the fixed designation D7731;the number immediately following the de
2、signation 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
3、in August 2011.1.Scope1.1 This procedure covers the determination of DipropyleneGlycol Monobutyl Ether(DPGBE)and Ethylene GlycolMonobutyl Ether(EGBE)in sea water by direct injection usingliquid chromatography(LC)and detection with tandem massspectrometry(MS/MS).These analytes are qualitatively andqu
4、antitatively determined by this method.This method adheresto selected reaction monitoring(SRM)mass spectrometry.1.2 The Detection Verification Level(DVL)and ReportingRange for DPGBE and EGBE are listed in Table 1.1.2.1 The DVL is required to be at a concentration at least3 times below the Reporting
5、Limit(RL)and have a signal/noise ratio greater than 3:1.Fig.1 and Fig.2 display thesignal/noise ratio of the single reaction monitoring(SRM)transition.1.2.2 The reporting limit is the concentration of the Level 1calibration standard as shown in Table 4 for DPGBE andEGBE,taking into account the 20%sa
6、mple preparation dilu-tion 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 t
7、his 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 o
8、f Committee D19 on Water2.2 Other Standards:3EPA publication SW-846 Test Methods for Evaluating SolidWaste,Physical/Chemical Methods3.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 Repo
9、rting Limit(RL).3.1.2 reporting limit,RL,nthe concentration of thelowest-level calibration standard used for quantification.3.1.2.1 DiscussionIn this test method,a 20 mL samplealiquot is diluted to a 25 mL final volume after thoroughlyrinsing the collection vial with acetonitrile for quantitativetra
10、nsfer.In this case,the lowest calibration level of 100 ppb forEGBE would allow for a reporting limit of 125 ppb to beachieved.3.2 Symbols:3.2.1 ppbparts per billion,g/L3.2.2 pptparts per trillion,ng/L3.2.3 mMmillimolar,1 x 10-3moles/L3.2.4 NAno addition3.2.5 NDnon-detect1This test method is under th
11、e 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 June 2011.DOI:10.1520/D7731-11E01.2For referenced ASTM standards,visit the ASTM website,www.astm.or
12、g,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
13、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 4.Summary of Test Method4.1 This is a performance based method,and modificationsare allowed to improve performance.4.2 For DPGBE
14、and EGBE analysis,samples are shipped tothe lab between 0C and 6C and analyzed within 5 days ofcollection.The DOW MSDS sheet on DOWANOL*DPNBglycol ether(DPGBE)Issue Date:06/18/2010 lists that thematerial is readily biodegradable.The Organisation for Eco-nomic Co-Operation and Development(OECD)302B T
15、est lists96%biodegradation in 28 days.4.3 In the lab,the entire collected 20 mL sample is spikedwith surrogate and brought to a volume of 25 mL withacetonitrile.This prepared sample is then filtered using asyringe driven filter unit,and analyzed by LC/MS/MS.Ifvisible oil is present,the prepared samp
16、le is allowed to settleresulting in an oil layer at the top of the 25 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.4.4 DPGBE,EGBE and surrogate are identified by retentiontime and one SRM transition.The target analytes and surrogateare quantitated using the SRM transitions utilizing an externalcalibration.The final report issued for each sample lists theconcentration of DPGBE,EGBE and the
