1、Designation:E286612(Reapproved 2016)Standard Test Method forDetermination of Diisopropyl Methylphosphonate,EthylMethylphosphonic Acid,Isopropyl Methylphosphonic Acid,Methylphosphonic Acid and Pinacolyl MethylphosphonicAcid in Soil by Pressurized Fluid Extraction and Analyzedby Liquid Chromatography/
2、Tandem Mass Spectrometry1This standard is issued under the fixed designation E2866;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 e
3、psilon()indicates an editorial change since the last revision or reapproval.1.Scope1.1 This procedure covers the determination of DiisopropylMethylphosphonate(DIMP),Ethyl Methylphosphonic Acid(EMPA),Isopropyl Methylphosphonic Acid(IMPA),Methyl-phosphonicAcid(MPA)and Pinacolyl MethylphosphonicAcid(PM
4、PA),referred to collectively as organophosphonates(OPs)in this test method,in soil.This method is based upon solventextraction of a soil by pressurized fluid extraction(PFE).Theextract is filtered and analyzed by liquid chromatography/tandem mass spectrometry(LC/MS/MS).OPs are qualitativelyand quant
5、itatively determined by this method.1.2 UnitsThe values stated in SI units are to be regardedas standard.No other units of measurement are included in thisstandard.1.3 The Method Detection Limit2(MDL),electrosprayionization(ESI)mode and Reporting Range3for the OPs arelisted in Table 1.1.4 This stand
6、ard 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 S
7、tandards:4D653 Terminology Relating to Soil,Rock,and ContainedFluidsD1193 Specification for Reagent WaterD3694 Practices for Preparation of Sample Containers andfor Preservation of Organic ConstituentsD3740 Practice for Minimum Requirements for AgenciesEngaged in Testing and/or Inspection of Soil an
8、d Rock asUsed in Engineering Design and ConstructionD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterE2554 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 Tes
9、t Methods for Evaluating SolidWaste,Physical/Chemical Methods540 CFR Part 136 The Code of Federal Regulations,Appen-dix B63.Terminology3.1 Definitions:3.1.1 analytical column,nthe particles of the solid sta-tionary phase fill the whole inside volume of a tube(column)that the mobile phase passes thro
10、ugh using the pressuregenerated by the liquid chromatography system.1This test method is under the jurisdiction of ASTM Committee E54 onHomeland Security Applications and is the direct responsibility of SubcommitteeE54.03 on Decontamination.Current edition approved June 1,2016.Published July 2016.Or
11、iginally approvedin 2012.Last previous edition approved in 2012 as E2866 12.DOI:10.1520/E2866-12R16.2The MDL is determined following the Code of Federal Regulations,40 CFRPart 136,Appendix B utilizing solvent extraction of soil by PFE.A detailed processdetermining the MDL is explained in the referen
12、ce and is beyond the scope of thisStandard to be explained here.3Reporting range concentrations are calculated from Table 4 concentrationsassuming a 100 L injection of the lowest and highest level calibration standardswith a 40 mL final extract volume of a 10 gram soil sample.Volume variations willc
13、hange the reporting limit and ranges.The reporting limit(RL),lowest concentra-tion of the reporting range,is calculated from the concentration of the Level 1calibration standard as shown in Table 4.4For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at
14、serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.5Available 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/haza
15、rd/testmethods/index.htm6Available from U.S.Government Printing Office Superintendent of Documents,732 N.Capitol St.,NW,Mail Stop:SDE,Washington,DC 20401,http:/www.access.gpo.gov.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 3.1.2 filte
16、r unit,nin this standard,a filter that is supportedwith an inert housing to the solvents as described in Section 7of this standard.3.1.3 filtration device,na device used to remove particlesfrom the extract that may clog the liquid chromatographysystem.Described in section 7.3 of this standard.3.1.4 glass fiber filter,nA porous glass fiber material ontowhich solid particles present in the extraction fluid,whichflows through it,are largely caught and retained,thus removingthem from the extract.3.1