1、Designation: D5765 05 (Reapproved 2010)D5765 16Standard 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 th
2、e 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 tot
3、al petroleum hydrocarbon (TPH) from soils and sediments, using closedvessel microwave heating, for subsequent determination by gravimetric or gas chromatographic techniques.1.2 This practice is recommended only for solid samples that can pass through a ten mesh screen (approximately 2 mmopenings).1.
4、3 The solvent extract obtained by this practice may be analyzed for total or specific nonvolatile and semivolatile petroleumhydrocarbons but may require sample clean-up procedures prior to specific compound analysis.1.4 This practice is limited to solvents that are recommended for use in microwave s
5、olvent extraction systems.1.5 The values stated in pounds per square inch (psi) SI units are to be regarded as the standard. The SI units given inparentheses are for information only.standard.1.5.1 ExceptionThe inch-pound values given for units of pressure are to be regarded as standard; SI unit con
6、versions areshown in parentheses.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitatio
7、ns prior to use. Specific hazard statements are given in Section 89.2. Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD3694 Practices for Preparation of Sample Containers and for Preservation of Organic ConstituentsD3856 Guide for Management Systems in Laboratories Engage
8、d in Analysis of WaterD3974 Practices for Extraction of Trace Elements from SedimentsD3976 Practice for Preparation of Sediment Samples for Chemical AnalysisD5368 Test Methods for Gravimetric Determination of Total Solvent Extractable Content (TSEC) of Solid Waste Samples(Withdrawn 2014)32.2 Federal
9、 Standard:Code of Federal Regulations,Regulations Title 21, Part 1030,1030; and Title 47, Part 1843. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.1 This practice is under the jurisdiction of ASTM Committee D19 on Water and is the direct
10、responsibility of Subcommittee D19.07 on Sediments, Geomorphology, andOpen-Channel Flow.Current edition approved June 15, 2010Jan. 1, 2016. Published December 2010January 2016. Originally approved in 1995. Last previous edition approved in 20052010as D5765 05.D5765 05 (2010). DOI: 10.1520/D5765-05R1
11、0.10.1520/D5765-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this histor
12、ical standard is referenced on www.astm.org.4 Available 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.This document is not an ASTM standard and is intended only to provide the user of an ASTM s
13、tandard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by
14、ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14. Summary of Practice4.1 The chemical portion of this practice involves solvent extraction to dissociate petroleum hydrocarbons from the m
15、atrix.4.2 The sample is extracted with acetone/hexane in a sealed microwave transparent vessel using microwave heating to aninternal temperature of 150 C.150C.4.3 This practice provides a sample suitable for analysis by gas chromatography or gravimetric measurements.5. Significance and Use5.1 Solven
16、t extraction of soils and sediments can provide information on the availability of petroleum hydrocarbons to leaching,water quality changes, or other site conditions.5.2 Rapid heating, in combination with temperatures in excess of the atmospheric boiling point of acetone/hexane, reducessample prepar
17、ation or extraction times.5.3 Reduced amounts of solvents are required and solvent loss due to boiling and evaporation are eliminated by use of closedextraction vessels.6. Interferences6.1 No interferences to the extraction of soils and sediments using microwave heating have been observed.6.2 Precau
18、tions should be exercised to avoid those interferences normally associated with the final determination of totalpetroleum hydrocarbons using gas chromatography or gravimetric techniques.7. Apparatus7.1 Microwave Heating SystemA laboratory microwave heating system capable of delivering a minimum of 9
19、00 W ofmicrowave energy. The system should be capable of 1 % power adjustments and 1 s time adjustment. The microwave cavity shouldbe constructed so as to prevent any possible metal to metal arcing from occurring within the cavity. The oven cavity should beequipped with an exhaust ventilation suffic
20、ient to provide ten chamber exchanges per minute. The ventilation exhaust shouldcontain a solvent sensor capable of detecting solvent concentrations below their lower explosive limits and shutting the microwavesource off. The cavity shall have a 360 oscillating turntable to ensure even sample heatin
21、g, and be capable of monitoring andcontrol of solvent temperature using either an in-situ control vessel or by external vessel monitoring. Safety interlocks, to shut offmagnetron power output shall be contained in the cavity door opening mechanism. The system shall comply with Department ofHealth an
22、d Human Services Standards under the Code of Federal Regulations, Part 1030.10, Subparts (c) (1), (c) (2), and (c) (3),for microwave leakage. The system should have Federal Communications Commission (FCC) type approval for operations underFCC Rule Part 18.7.2 Extraction VesselsA closed lined extract
23、ion vessel of approximately 50 to 100 mL capacity. The vessel consists of afluoropolymer or glass inner liner and fluoropolymer cover to contain and isolate a solvent solution from a higher strength polymerouter pressure vessel body. The vessel assembly shall be transparent to microwave energy and c
24、apable of withstanding an internalpressure of 300 psi (20.68 by 106dynes/cm2) and a temperature of 200 C. 200C. The vessel assembly shall contain a safetypressure relief device that will prevent possible rupture.7.3 Temperature-Pressure Control VesselA closed lined extraction vessel with temperature
25、 and pressure monitoring portscapable of withstanding an internal pressure of 300 psi (20.68 by 106 dynes/cm2) and a temperature of 200C. The vessel assemblyshall contain a safety pressure relief device that will prevent possible vessel rupture.8. Reagents and Materials8.1 Purity of ReagentsReagent
26、grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available. 58.2 Acetone, HPLC grade.8.3 Hexane, HPLC grad
27、e.8.4 Sodium SulfateReagent grade, granular, anhydrous, prepared by heating at 400C for a minimum of 4 h.8.5 Ashless Filter Paper.5 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe Amer
28、ican Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, MD.D5765 1629. Hazards9.1 The microwave system shall be operated and maintained in ac
29、cordance with the manufacturers recommended safetyprecautions.9.2 The extraction vessels shall be used and maintained in accordance with the manufacturers recommended safety precautions.9.3 Use only microwave systems and vessels approved for solvent use.10. Sampling10.1 Collect a soil or sediment sa
30、mple using an appropriate sampling technique.10.2 Prepare the soil or sediment sample in accordance with PracticePractices D3976, Practice D3974, or Practices D3694.11. Vessel Cleaning11.1 Follow the manufacturers recommended cleaning procedure.12. Procedure12.1 Take a 5 g portion of the sample prep
31、ared in 9.210.2, weigh to the nearest 0.1 mg, and transfer into extraction vessels.Include an empty extraction vessel in each set as a method blank.NOTE 1The temperature-pressure control vessel shall contain 5 g of sample material.12.2 Add 30 mL of acetone/hexane (1 + 1) to each sample and blank ext
32、raction vessel.12.3 Close each extraction vessel according to the manufacturers recommended procedures.12.4 Place the closed extraction vessels into the instrument turntable and assemble following the manufacturers suggestedprocedure.12.5 Heat the vessels according to the extraction heating paramete
33、rs in Table 1.12.6 Allow the vessels to cool to room temperature.12.7 Open the vessels and add 5 g of sodium sulfate to the sample and solvent mixture and gently swirl the mixture.12.8 Filter the extract mixture through ashless filter paper rinsing and washing the extracted, sample, sodium sulfate a
34、nd filterpaper thoroughly with (1 + 1) acetone/hexane into an appropriate container. (See Guide D3856.)NOTE 2For gravimetric TPH determination, filter extract solvent into an appropriate pre-weighed evaporating dish. (See Test MethodMethodsD5368.)12.9 Proceed with an appropriate procedure for gravim
35、etric or gas chromatographic TPH determination.13. Data13.1 Typical data are shown in Table 2.14. Precision and Bias14.1 It is the responsibility of the user to establish the precision and bias of the extraction practice in conjunction with theanalytical measuring method.15. Keywords15.1 extraction;
36、 microwave; solvent; total petroleum hydrocarbon (TPH); vesselTABLE 1 Extraction Heating Parameterscolwidth=“57.22*“/COLSPECMicrowave power 100 %Vessels pressure 200 psiVessels temperature 150 CVessels temperature 150CHeating time at 150C 15 minD5765 163ASTM International takes no position respectin
37、g 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.This standa
38、rd 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 International
39、 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 shown below.Thi
40、s 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), 610-832-9555 (fax),
41、 or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 2 Total Petroleum Hydrocarbon Recovery Datacolwidth=“32.47*“/COLSPECMaterial TPH Present(%) TPH Recovered(%) MeasurementMethodSoil 1.34 A 1.32 GravimetricSoil B 0.214 0.223 GravimetricSoil B 0.099 0.094 GC-FIDA Value determined by Soxhlet Extraction.B Environmental Resource Associates standard reference soil.D5765 164
