ASTM_D_6520_-_06_2012.pdf

Designation:D652006(Reapproved 2012)Standard Practice forthe Solid Phase Micro Extraction(SPME)of Water and itsHeadspace for the Analysis of Volatile and Semi-VolatileOrganic Compounds1This standard is issued under the fixed designation D6520;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 practice covers procedures for the extraction ofvolatile and semi-volatile organic compounds from water andits headspace using solid-phase microextraction(SPME).1.2 The compounds of interest must have a greater affinityfor the SPME-absorbent polymer or adsorbent or combinationsof these than the water or headspace phase in which theyreside.1.3 Not all of the analytes that can be determined by SPMEare addressed in this practice.The applicability of the absor-bent polymer,adsorbent,or combination thereof,to extract thecompound(s)of interest must be demonstrated before use.1.4 This practice provides sample extracts suitable forquantitative or qualitative analysis by gas chromatography(GC)or gas chromatography-mass spectrometry(GC-MS).1.5 Where used,it is the responsibility of the user to validatethe application of SPME to the analysis of interest.1.6 The values stated in SI units are to be regarded as thestandard.1.7 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.For specific hazardstatements,see Section 10.2.Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD3370 Practices for Sampling Water from Closed ConduitsD3694 Practices for Preparation of Sample Containers andfor Preservation of Organic ConstituentsD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD4210 Practice for Intralaboratory Quality Control Proce-dures and a Discussion on Reporting Low-Level Data(Withdrawn 2002)3D4448 Guide for Sampling Ground-Water Monitoring Wells3.Terminology3.1 DefinitionsFor definitions of terms used in thispractice,refer to Terminology D1129.4.Summary of Practice4.1 This practice employs adsorbent/liquid or adsorbent/gasextraction to isolate compounds of interest.An aqueous sampleis added to a septum-sealed vial.The aqueous phase or itsheadspace is then exposed to an adsorbent coated on a fusedsilica fiber.The fiber is desorbed in the heated injection port ofa GC or GC-MS or the injector of an HPLC.4.2 The desorbed organic analytes may be analyzed usinginstrumental methods for specific volatile or semi-volatileorganic compounds.This practice does not include sampleextract clean-up procedures.5.Significance and Use5.1 This practice provides a general procedure for thesolid-phase microextraction of volatile and semi-volatile or-ganic compounds from an aqueous matrix or its headspace.Solid sorbent extraction is used as the initial step in theextraction of organic constituents for the purpose of quantify-ing or screening for extractable organic compounds.5.2 Typical detection limits that can be achieved usingSPME techniques with gas chromatography with flame ioniza-tion detector(FID),electron capture detector(ECD),or with a1This practice is under the jurisdiction of ASTM Committee D19 on Water andis the direct responsibility of Subcommittee D19.06 on Methods for Analysis forOrganic Substances in Water.Current edition approved June 15,2012.Published June 2012.Originallyapproved in 2000.Last previous edition approved in 2012 as D6520 06.DOI:10.1520/D6520-06R12.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 mass spectrometer(MS)range from mg/L to g/L.Thedetection limit,linear concentration range,and sensitivity ofthe test method for a specific organic compound will dependupon the aqueous matrix,the fiber phase,the sampletemperature,sample volume,sample mixing,and the determi-native technique employed.5.3 SPME has the advantages of speed,no desorptionsolvent,simple extraction device,and the use of small amountsof sample.5.3.1 Extraction devices vary from a manual SPME fiberholder to automated commercial device specifically designedfor SPME.5.3.2 Listed below are examples of organic compounds thatcan be determined by this practice.This list includes both highand low boiling compounds.The numbers in pare