ASTM_D_7968_-_14.pdf

Designation:D796814Standard Test Method forDetermination of Perfluorinated 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 selectedperfluorinated compounds(PFCs)in a soil matrix using solventextraction,filtration,followed by liquid chromatography(LC)and detection with tandem mass spectrometry(MS/MS).Theseanalytes are qualitatively and quantitatively determined by thismethod.This method adheres to multiple reaction monitoring(MRM)mass spectrometry.This procedure utilizes a quickextraction and is not intended to generate an exhaustiveaccounting of the content of PFCs in difficult soil matrices.Anexhaustive extraction procedure for polyfluoralkyl substances,such as published by Washington et al.2,for difficult matricesshould 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 perfluorinatedcompounds 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 be 10mL 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 and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:5D653 Terminology Relating to Soil,Rock,and ContainedFluidsD1193 Specification for Reagent WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on 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 and Rock asUsed in Engineering Design and ConstructionD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD5681 Terminology for Waste and Waste ManagementD5847 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 Nov.1,2014.Published December 2014.DOI:10.1520/D7968-14.2Washington,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 C