1、Designation:E278711(Reapproved 2016)Standard Test Method forDetermination of Thiodiglycol in Soil Using PressurizedFluid Extraction Followed by Single Reaction MonitoringLiquid Chromatography/Tandem Mass Spectrometry(LC/MS/MS)1This standard is issued under the fixed designation E2787;the number imme
2、diately 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 proced
3、ure covers the determination of thiodiglycol(TDG)in soil using pressurized fluid extraction(PFE).Acommercially available PFE system2was used,followed byanalysis using liquid chromatography(LC),and detected withtandem mass spectrometry(MS/MS).TDG is qualitatively andquantitatively determined by this
4、method.This method adheresto single reaction monitoring(SRM)mass spectrometry.1.2 The Method Detection Limit(MDL)and ReportingRange for TDG are listed in Table 1.1.2.1 The MDLis determined following the Code of FederalRegulations,40 CFR Part 136,Appendix B.1.2.2 The reporting limit(RL)is calculated
5、from the con-centration of the Level 1 calibration standard as shown in Table4.The RL for this method is 200 ppb.Reporting rangeconcentrations are calculated from Table 4 concentrationsassuming a 5 L injection of the lowest level calibrationstandard,5 g sample,and a 2 mL final extract volume.1.3 Uni
6、tsThe values stated in SI units are to be regardedas standard.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-pria
7、te safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:3D653 Terminology Relating to Soil,Rock,and ContainedFluidsD1193 Specification for Reagent WaterD3694 Practices for Preparation of Sample Containers andfor
8、Preservation of Organic ConstituentsD3740 Practice for Minimum Requirements for AgenciesEngaged in Testing and/or Inspection of Soil and Rock asUsed in Engineering Design and ConstructionE2554 Practice for Estimating and Monitoring the Uncer-tainty of Test Results of a Test Method Using ControlChart
9、 Techniques2.2 Other Documents:EPApublication SW-846,Test Methods for Evaluating SolidWaste,Physical/Chemical Methods440 CFR Part 136,Appendix B,The Code of Federal Regu-lations3.Terminology3.1 Abbreviations:3.1.1 mMmillimolar,1 10-3moles/L3.1.2 NDnon-detect3.1.3 SRMsingle reaction monitoring3.1.4 M
10、RMmultiple reaction monitoring4.Summary of Test Method4.1 This is a performance based method,and modificationsare allowed to improve performance.1This test method is under the jurisdiction of ASTM Committee E54 onHomeland Security Applications and is the direct responsibility of SubcommitteeE54.03 o
11、n Decontamination.Current edition approved June 1,2016.Published June 2016.Originallyapproved in 2011.Last previous edition approved in 2011 as E2787 11.DOI:10.1520/E2787-11R16.2The PFE system that was used to develop this test method was AcceleratedSolvent Extraction(ASE)which is a patented techniq
12、ue by Dionex,Sunnyvale,CA 94088.3For 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.4Available from National Technical
13、 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 4.2 For TDG analysis,samples are
14、 shipped to the labbetween 0 and 6C.In the lab,the soils are spiked with3,3-thiodipropanol(TDP,surrogate)and extracted by PFE.The extract is filtered using a syringe driven filter unit,reducedin volume,reconstituted with water,and analyzed directly byLC/MS/MS within 7 days.4.3 TDG and TDP are identi
15、fied by retention time and oneSRM transition.The target analyte and surrogate are quanti-tated using the SRM transitions utilizing an external calibra-tion.The final report issued for each sample lists the concen-tration of TDG and the TDP recovery.5.Significance and Use5.1 TDG is a Schedule 2 compo
16、und under the ChemicalWeapons Convention(CWC).Schedule 2 chemicals includethose that are precursors to chemical weapons,chemicalweapons agents or have a number of other commercial uses.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.TDG is both a mustard gas precursor and adegradant as well as an ingredient in water-based inks,ball-point pen inks,dyes,and som