1、Designation: D5765 05 (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 o
2、foriginal 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 totalpetrol
3、eum 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 solve
4、nt 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 extra
5、ction 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 us
6、er 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 P
7、reservation of Organic ConstituentsD3856 Guide for Good Laboratory Practices in Laborato-ries Engaged in Sampling and Analysis of WaterD3974 Practices for Extraction of Trace Elements fromSedimentsD3976 Practice for Preparation of Sediment Samples forChemical AnalysisD5368 Test Methods for Gravimetr
8、ic Determination ofTotal Solvent 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
9、 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 Sol
10、vent 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 prepa
11、ration 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 pract
12、ice 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
13、 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. Gover
14、nment Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.2 Precautions should be exercised to avoid tho
15、se 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 s
16、hould 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 pe
17、r 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 and control
18、 of solventtemperature using either an in-situ control vessel or by externalvessel monitoring. Safety interlocks, to shut off magnetronpower output shall be contained in the cavity door openingmechanism. The system shall comply with Department ofHealth and Human Services Standards under the Code ofF
19、ederal Regulations, Part 1030.10, Subparts (c) (1), (c) (2), and(c) (3), for microwave leakage. The system should haveFederal Communications Commission (FCC) type approval foroperations under FCC Rule Part 18.6.2 Extraction VesselsA closed lined extraction vessel ofapproximately 50 to 100 mL capacit
20、y. The vessel consists of afluoropolymer or glass inner liner and fluoropolymer cover tocontain and isolate a solvent solution from a higher strengthpolymer outer pressure vessel body. The vessel assembly shallbe transparent to microwave energy and capable of withstand-ing an internal pressure of 30
21、0 psi (20.68 by 106dynes/cm2)and a temperature of 200 C. The vessel assembly shall containa safety pressure relief device that will prevent possiblerupture.6.3 Temperature-Pressure Control VesselA closed linedextraction vessel with temperature and pressure monitoringports capable of withstanding an
22、internal pressure of 300 psi(20.68 by 106dynes/cm2) and a temperature of 200C. Thevessel assembly shall contain a safety pressure relief devicethat will prevent possible vessel rupture.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise
23、indicated, it is intended thatall reagents shall conform to the specifications of the commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.47.2 Acetone, HPLC grade.7.3 Hexane, HPLC grade.7.4 Sodium SulfateReagent grade, granular, anhydrous,prepar
24、ed by heating at 400C for a minimum of 4 h.7.5 Ashless Filter Paper.8. Hazards8.1 The microwave system shall be operated and maintainedin accordance with the manufacturers recommended safetyprecautions.8.2 The extraction vessels shall be used and maintained inaccordance with the manufacturers recomm
25、ended safety pre-cautions.8.3 Use only microwave systems and vessels approved forsolvent use.9. Sampling9.1 Collect a soil or sediment sample using an appropriatesampling technique.9.2 Prepare the soil or sediment sample in accordance withPractice D3976, Practice D3974, or Practices D3694.10. Vessel
26、 Cleaning10.1 Follow the manufacturers recommended cleaning pro-cedure.11. Procedure11.1 Takea5gportion of the sample prepared in 9.2, weighto the nearest 0.1 mg, and transfer into extraction vessels.Include an empty extraction vessel in each set as a methodblank.NOTE 1The temperature-pressure contr
27、ol vessel shall contain5gofsample material.11.2 Add 30 mL of acetone/hexane (1 + 1) to each sampleand blank extraction vessel.11.3 Close each extraction vessel according to the manufac-turers recommended procedures.11.4 Place the closed extraction vessels into the instrumentturntable and assemble fo
28、llowing the manufacturers suggestedprocedure.11.5 Heat the vessels according to the extraction heatingparameters in Table 1.11.6 Allow the vessels to cool to room temperature.11.7 Open the vessels and add5gofsodium sulfate to thesample and solvent mixture and gently swirl the mixture.11.8 Filter the
29、 extract mixture through ashless filter paperrinsing and washing the extracted, sample, sodium sulfate andfilter paper thoroughly with (1 + 1) acetone/hexane into anappropriate container. (See Guide D3856.)NOTE 2For gravimetric TPH determination, filter extract solvent intoan appropriate pre-weighed
30、 evaporating dish. (See Test Method D5368.)4Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Do
31、rset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.TABLE 1 Extraction Heating ParametersMicrowave power 100 %Vessels pressure 200 psiVessels temperature 150 CHeating time at 150C 15 minD5765 05 (2010)211.9 Proceed with an a
32、ppropriate procedure for gravimetricor gas chromatographic TPH determination.12. Data12.1 Typical data are shown in Table 2.13. Precision and Bias13.1 It is the responsibility of the user to establish theprecision and bias of the extraction practice in conjunction withthe analytical measuring method
33、.14. Keywords14.1 extraction; microwave; solvent; total petroleum hydro-carbon (TPH); vesselASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determinatio
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36、omments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single
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38、ww.astm.org/COPYRIGHT/).TABLE 2 Total Petroleum Hydrocarbon Recovery DataMaterialTPH Present(%)TPH Recovered(%)Measurement MethodSoil 1.34A1.32 GravimetricSoilB0.214 0.223 GravimetricSoilB0.099 0.094 GC-FIDAValue determined by Soxhlet Extraction.BEnvironmental Resource Associates standard reference soil.D5765 05 (2010)3
