ASTM_D_7968_-_17a.pdf

Designation:D796817aStandard Test Method forDetermination of Polyfluorinated Compounds in Soil byLiquid Chromatography Tandem Mass Spectrometry(LC/MS/MS)1This standard is issued under the fixed designation D7968;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 selectedpolyfluorinated compounds(PFCs)in a soil matrix usingsolvent extraction,filtration,followed by liquid chromatogra-phy(LC)and detection with tandem mass spectrometry(MS/MS).These analytes are qualitatively and quantitatively deter-mined by this method.This method adheres to multiplereaction monitoring(MRM)mass spectrometry.This proce-dure utilizes a quick extraction and is not intended to generatean exhaustive accounting of the content of PFCs in difficult soilmatrices.An exhaustive extraction procedure for polyfluo-ralkyl substances,such as published by Washington et al.,2fordifficult matrices should be considered when analyzing PFCs.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 of Detection Limit3and Reporting Range4for the target analytes are listed in Table 1.1.3.1 The reporting limit in this test method is the minimumvalue below which data are documented as non-detects.Ana-lyte detections between the method detection limit and thereporting limit are estimated concentrations and are not re-ported following this test method.In most cases,the reportinglimit is calculated from the concentration of the Level 1calibration standard as shown in Table 2 for the polyfluorinatedcompounds after taking into account a 2-g sample weight anda final extract volume of 10 mL,50%water/50%MeOH with0.1%acetic acid.The final extract volume is assumed to be10 mL because 10 mL of 50%water/50%MeOH with 0.1%acetic acid was added to each soil sample and only the liquidlayer after extraction is filtered,leaving the solid and anyresidual solvent behind.It is raised above the Level 1 calibra-tion concentration for PFOS,PFHxA,FHEA,and FOEA;thesecompounds can be identified at the Level 1 concentration butthe standard deviation among replicates at this lower spikelevel resulted in a higher reporting limit.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,health and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international 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)Committee.2.Referenced Documents2.1 ASTM Standards:5D1193 Specification for Reagent WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water AnalysisE2554 Practice for Estimating and Monitoring the Uncer-tainty of Test Results of a Test Method Using ControlChart Techniques1This test method is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.06 onAnalytical Methods.Current edition approved Sept.1,2017.Published September 2017.Originallyapproved in 2014.Last previous edition approved in 2017 as D7968 17.DOI:10.1520/D7968-17A.2Washington,J.W.,Naile,J.E.,Jenkins,T.M.,and Lynch,D.G.,“Character-izing Fluorotelomer and Polyfluoroalkyl Substances in New and AgedFluorotelomer-Based Polymers for Degradation Studies with GC/MS and LC/MS/MS,”Environmental Science and Technology,Vol 48,2014,pp.57625769.3The MDL is determined following the Code of Federal Regulations,40 CFRPart 136,Appendix B utilizing solvent extraction of soil.Two-gram sample ofOttawa sand was utilized.A detailed process determining the MDL is explained inthe reference and is beyond the scope of this standard to be explained here.4Reporting range concentration is calculated from Table 2 concentrationsassuming a 30-L injection of the Level 1 calibration standard for the PFCs,and thehighest level calibration standard with a 10-mL final extract volume of a 2-g soilsample.Volume variations will change the reporting limit and ranges.5For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,We