ASTM_D_5765_-_05_2010.pdf

Designation:D576505(Reapproved 2010)Standard Practice forSolvent Extraction of Total Petroleum Hydrocarbons fromSoils and Sediments Using Closed Vessel MicrowaveHeating1This standard is issued under the fixed designation D5765;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 the solvent extraction of totalpetroleum hydrocarbon(TPH)from soils and sediments,usingclosed vessel microwave heating,for subsequent determinationby gravimetric or gas chromatographic techniques.1.2 This practice is recommended only for solid samplesthat can pass through a ten mesh screen(approximately 2 mmopenings).1.3 The solvent extract obtained by this practice may beanalyzed for total or specific nonvolatile and semivolatilepetroleum hydrocarbons but may require sample clean-upprocedures prior to specific compound analysis.1.4 This practice is limited to solvents that are recom-mended for use in microwave solvent extraction systems.1.5 The values stated in pounds per square inch(psi)are tobe regarded as the standard.The SI units given in parenthesesare for information only.1.6 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.Specific hazardstatements are given in Section 8.2.Referenced Documents2.1 ASTM Standards:2D3694 Practices for Preparation of Sample Containers andfor Preservation of Organic ConstituentsD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD3974 Practices for Extraction of Trace Elements fromSedimentsD3976 Practice for Preparation of Sediment Samples forChemical AnalysisD5368 Test Methods for Gravimetric Determination of TotalSolvent Extractable Content(TSEC)of Solid WasteSamples2.2 Federal Standard:Code of Federal Regulations,Title 21,Part 1030,and Title47,Part 1833.Summary of Practice3.1 The chemical portion of this practice involves solventextraction to dissociate petroleum hydrocarbons from thematrix.3.2 The sample is extracted with acetone/hexane in a sealedmicrowave transparent vessel using microwave heating to aninternal temperature of 150 C.3.3 This practice provides a sample suitable for analysis bygas chromatography or gravimetric measurements.4.Significance and Use4.1 Solvent extraction of soils and sediments can provideinformation on the availability of petroleum hydrocarbons toleaching,water quality changes,or other site conditions.4.2 Rapid heating,in combination with temperatures inexcess of the atmospheric boiling point of acetone/hexane,reduces sample preparation or extraction times.4.3 Reduced amounts of solvents are required and solventloss due to boiling and evaporation are eliminated by use ofclosed extraction vessels.5.Interferences5.1 No interferences to the extraction of soils and sedimentsusing microwave heating have been observed.1This practice is under the jurisdiction of ASTM Committee D19 on Water andis the direct responsibility of Subcommittee D19.07 on Sediments,Geomorphology,and Open-Channel Flow.Current edition approved June 15,2010.Published December 2010.Originallyapproved in 1995.Last previous edition approved in 2005 as D5765 05.DOI:10.1520/D5765-05R10.2For 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 U.S.Government Printing Office Superintendent of Documents,732 N.Capitol St.,NW,Mail Stop:SDE,Washington,DC 20401,http:/www.access.gpo.gov.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.2 Precautions should be exercised to avoid those interfer-ences normally associated with the final determination of totalpetroleum hydrocarbons using gas chromatography or gravi-metric techniques.6.Apparatus6.1 Microwave Heating SystemA laboratory microwaveheating system capable of delivering a minimum of 900 W ofmicrowave energy.The system should be capable of 1%power adjustments and 1 s time adjustment.The microwavecavity should be constructed so as to prevent any possiblemetal to metal arcing from occurring within the cavity.Theoven cavity should be equipped with an exhaust ventilationsufficient to provide ten chamber exchanges per minute.Theventilation exhaust should contain a solvent sensor capable ofdetecting solvent concentrations below their lower explosivelimits and shutting the microwave source off.The cavity shallhave a 360 oscillating turntable to ensure even sampleheating,and be capable of monitoring a