ASTM_D_6010_-_12.pdf

Designation:D601012Standard Practice forClosed Vessel Microwave Solvent Extraction of OrganicCompounds from Solid Matrices1This standard is issued under the fixed designation D6010;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 describes the closed vessel microwaveextraction of soils,sediments,sludges,and wastes for subse-quent determination of solvent extractable semivolatile andnonvolatile organic compounds by such techniques as gaschromatography and gas chromatography-mass spectrometry.1.1.1 Compounds listed in Tables 15 can be extracted fromthe preceding materials.1.2 This test method is applicable to samples that will passthrough a 10-mesh(approximately 2-mm opening)screen.1.3 The detection limit and linear concentration range foreach compound is dependent on the gas chromatograph or gaschromatograph-mass spectrometer technique employed andmay be found in the manual accompanying the instrumentused.1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.5 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:2D1193 Specification for Reagent WaterD3976 Practice for Preparation of Sediment Samples forChemical AnalysisD5368 Test Methods for Gravimetric Determination of TotalSolvent Extractable Content(TSEC)of Solid WasteSamplesD5681 Terminology for Waste and Waste Management2.2 Other Standards:United States Environmental Protection Agency(USEPA),Test Methods for Evaluating Solid Waste Volume1A:Laboratory Manual Physical/Chemical Methods3Title 21,Code of Federal Regulations(CFR),Part 1030,andTitle 47,Part 1833.Terminology3.1 DefinitionsFor definitions of terms used in thispractice,see Terminology D5681.4.Summary of Practice4.1 This procedure ensures intimate contact of the samplematrix with 115C extraction solvent.4.2 A1 to 5-g portion of a solid sample is extracted in asealed microwave transparent extraction vessel with 30 mL ofacetone-hexane(1+1).4.3 Up to 12 samples may be extracted simultaneously.4.4 After extraction the vessels are cooled to roomtemperature,opened,and the solvent and sample are separatedby decanting,filtration,or centrifuging.4.5 This practice provides a sample suitable for analysis bygas chromatography or gas chromatography-mass spectrom-etry.5.Significance and Use5.1 Extraction of organic pollutants from wastes can pro-vide information on the susceptibility of compounds toleeching,water quality changes,or other site conditions.5.2 Rapid heating,in combination with temperatures inexcess of the atmospheric boiling point of organic solvents,reduces sample extraction times.5.3 Small amounts of solvents(30 mL)are used resulting inreduced sample preparation cost and time.1This practice 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.1,2012.Published December 2012.Originallyapproved in 1996.Last previous edition approved in 2006 as D6010 96(2006).DOI:10.1520/D6010-12.2For 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.3Available from the Superintendent of Documents,U.S.Government PrintingOffice,Washington,DC 20402.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.Interferences6.1 Method interferences may be caused by contaminants insolvents,labware,and other hardware used in sample process-ing that lead to discrete artifacts or elevated baselines in gaschromatograms.The analyst must demonstrate,through theanalysis of reagent blanks,that the system and the materials arefree from interferents.6.2 The use of high-purity solvents helps to minimizeinterference problems.6.3 Matrix interferences are caused by contaminants that areco-extracted from the sample.The extent of matrix interfer-ences may vary considerably from sample to sample.6.4 After cleaning,vessel liners and covers should be storedin a clean environment to prevent accumulation of contami-nants.TABLE 1 Semivolatile Analyte Recovery from Freshly SpikedTopsoilAnalyteSpike Level,mg/kgAverageRecovery,%ARSD,%Acenaphthene5.097.69.8Acenaphthylene5.010010Acetophenone5.092.2124-Aminobiphenyl5.077.39.5Aniline5.068.17.5Anthracene5.01089.2Benzidine5.00Benzoic acid5.042.313Benzo(a)anthrac