1、Designation: D 5765 05Standard Practice forSolvent Extraction of Total Petroleum Hydrocarbons fromSoils and Sediments Using Closed Vessel MicrowaveHeating1This standard is issued under the fixed designation D 5765; the number immediately following the designation indicates the year oforiginal adopti
2、on or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice covers the solvent extraction of totalpetroleum hydrocarbon
3、 (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 obta
4、ined 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、.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 stan
6、dard 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:2D 3694 Practices for Preparation of Sample Containers andfor Preservation of
7、 Organic ConstituentsD 3856 Guide for Good Laboratory Practices in Laborato-ries Engaged in Sampling and Analysis of WaterD 3974 Practice for Extraction of Trace Elements fromSedimentsD 3976 Practice for Preparation of Sediment Samples forChemical AnalysisD 5368 Test Method for the Gravimetric Deter
8、mination 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 from th
9、ematrix.3.2 The sample is extracted with acetone/hexane in a sealedmicrowave transparent vessel using microwave heating to aninternal temperature of 150C.3.3 This practice provides a sample suitable for analysis bygas chromatography or gravimetric measurements.4. Significance and Use4.1 Solvent extr
10、action 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
11、 extraction times.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 Aug. 15, 2005. Published August 2005. Originallyapproved in 1995. Last previous
12、edition approved in 2001 as D 5765 95 (2001).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
13、the U.S. Government Printing Office, Washington, DC.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4.3 Reduced amounts of solvents are required and solventloss due to boiling and evaporation are eliminated by use ofclosed extraction
14、 vessels.5. Interferences5.1 No interferences to the extraction of soils and sedimentsusing microwave heating have been observed.5.2 Precautions should be exercised to avoid those interfer-ences normally associated with the final determination of totalpetroleum hydrocarbons using gas chromatography
15、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 preven
16、t 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 low
17、er 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 of solventtemperature using either an in-situ control vessel or by externalvessel monitoring. Safety interlocks, to shut o
18、ff magnetronpower output shall be contained in the cavity door openingmechanism. The system shall comply with Department ofHealth and Human Services Standards under the Code ofFederal Regulations, Part 1030.10, Subparts (c) (1), (c) (2), and(c) (3), for microwave leakage. The system should haveFeder
19、al Communications Commission (FCC) type approval foroperations under FCC Rule Part 18.6.2 Extraction VesselsA closed lined extraction vessel ofapproximately 50 to 100 mL capacity. The vessel consists of afluoropolymer or glass inner liner and fluoropolymer cover tocontain and isolate a solvent solut
20、ion 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 300 psi (20.68 by 106dynes/cm2)and a temperature of 200C. The vessel assembly shall containa safety pressure relief device th
21、at will prevent possiblerupture.6.3 Temperature-Pressure Control VesselA closed linedextraction vessel with temperature and pressure monitoringports capable of withstanding an internal pressure of 300 psi(20.68 by 106dynes/cm2) and a temperature of 200C. Thevessel assembly shall contain a safety pre
22、ssure relief devicethat will prevent possible vessel rupture.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the commit-tee on Analytical Reagents of t
23、he 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,prepared 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
24、 maintainedin accordance with the manufacturers recommended safetyprecautions.8.2 The extraction vessels shall be used and maintained inaccordance with the manufacturers recommended safety pre-cautions.8.3 Use only microwave systems and vessels approved forsolvent use.9. Sampling9.1 Collect a soil o
25、r sediment sample using an appropriatesampling technique.9.2 Prepare the soil or sediment sample in accordance withPractice D 3976, Practice D 3974, or Practices D 3694.10. Vessel Cleaning10.1 Follow the manufacturers recommended cleaning pro-cedure.11. Procedure11.1 Takea5gportion of the sample pre
26、pared 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 control vessel shall contain5gofsample material.11.2 Add 30 mL of acetone/hexane (1 + 1) to each sampleand blank extraction ve
27、ssel.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 following the manufacturers suggestedprocedure.11.5 Heat the vessels according to the extraction heatingparameters in Table
28、 1.11.6 Allow the vessels to cool to room temperature.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.,
29、 Poole, Dorset, 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 150CHeating time at 150C 15 minD 5765 05211.7 Open the vesse
30、ls and add5gofsodium sulfate to thesample and solvent mixture and gently swirl the mixture.11.8 Filter the 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 G
31、uide D 3856.)NOTE 2For gravimetric TPH determination, filter extract solvent intoan appropriate pre-weighed evaporating dish. (See Test Method D 5368.)11.9 Proceed with an appropriate procedure for gravimetricor gas chromatographic TPH determination.12. Data12.1 Typical data are shown in Table 2.13.
32、 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.14. Keywords14.1 extraction; microwave; solvent; total petroleum hydro-carbon (TPH); vesselASTM International takes no positio
33、n respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.
34、This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM I
35、nternational Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address sho
36、wn 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 or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832
37、-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).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.D 5765 053
