ASTM D5765-95
(Practice)Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating
Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating
SCOPE
1.1 This practice covers the solvent extraction of total petroleum hydrocarbon (TPH) from soils and sediments, using closed vessel 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-mm openings).
1.3 The solvent extract obtained by this practice may be analyzed for total or specific nonvolatile and semivolatile petroleum hydrocarbons 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 solvent extraction systems.
1.5 The values stated in pounds per square inch (psi) are to be regarded as the standard. The SI units given in parentheses are for information only.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 8.
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Designation: D 5765 – 95
AMERICAN SOCIETY FOR TESTING AND MATERIALS
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Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Practice for
Solvent Extraction of Total Petroleum Hydrocarbons from
Soils and Sediments Using Closed Vessel Microwave
1
Heating
This standard is issued under the fixed designation D 5765; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope Total Solvent Extractable Content (TSEC) of Solid Waste
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Samples
1.1 This practice covers the solvent extraction of total
2.2 Federal Standard:
petroleum hydrocarbon (TPH) from soils and sediments, using
Code of Federal Regulations, Title 21, Part 1030, and Title
closed vessel microwave heating, for subsequent determination
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47, Part 18
by gravimetric or gas chromatographic techniques.
1.2 This practice is recommended only for solid samples
3. Summary of Practices
that can pass through a ten mesh screen (approximately 2-mm
3.1 The chemical portion of this practice involves solvent
openings).
extraction to dissociate petroleum hydrocarbons from the
1.3 The solvent extract obtained by this practice may be
matrix.
analyzed for total or specific nonvolatile and semivolatile
3.2 The sample is extracted with acetone/hexane in a sealed
petroleum hydrocarbons but may require sample clean-up
microwave transparent vessel using microwave heating to an
procedures prior to specific compound analysis.
internal temperature of 150°C.
1.4 This practice is limited to solvents that are recom-
3.3 This practice provides a sample suitable for analysis by
mended for use in microwave solvent extraction systems.
gas chromatography or gravimetric measurements.
1.5 The values stated in pounds per square inch (psi) are to
4. Significance and Use
be regarded as the standard. The SI units given in parentheses
4.1 Solvent extraction of soils and sediments can provide
are for information only.
information on the availability of petroleum hydrocarbons to
1.6 This standard does not purport to address all of the
leaching, water quality changes, or other site conditions.
safety concerns, if any, associated with its use. It is the
4.2 Rapid heating, in combination with temperatures in
responsibility of the user of this standard to establish appro-
excess of the atmospheric boiling point of acetone/hexane,
priate safety and health practices and determine the applica-
reduces sample preparation or extraction times.
bility of regulatory limitations prior to use. Specific hazard
4.3 Reduced amounts of solvents are required and solvent
statements are given in Section 8.
loss due to boiling and evaporation are eliminated by use of
closed extraction vessels.
2. Referenced Documents
5. Interferences
2.1 ASTM Standards:
D 3694 Practices for Preparation of Sample Containers and
5.1 No interferences to the extraction of soils and sediments
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for Preservation of Organic Constituents
using microwave heating have been observed.
D 3856 Guide for Good Laboratory Practices in Laborato-
5.2 Precautions should be exercised to avoid those interfer-
3
ries Engaged in Sampling and Analysis of Water
ences normally associated with the final determination of total
D 3974 Practice for Extraction of Trace Elements from
petroleum hydrocarbons using gas chromatography or gravi-
2
Sediments
metric techniques.
D 3976 Practice for Preparation of Sediment Samples for
2
6. Apparatus
Chemical Analysis
D 5368 Test Method for the Gravimetric Determination of
6.1 Microwave Heating System—A laboratory microwave
heating system capable of delivering a minimum of 900 W of
microwave energy. The system should be capable of 1 %
1
This practice is under the jurisdiction of ASTM Committee D-19 on Water and
power adjustments and 1-s time adjustment. The microwave
is the direct responsibility of Subcommittee D19.07 on Sediments, Geomorphology,
and Open-Channel Flow.
Current edition approved Aug. 15, 1995. Published October 1995.
2 4
Annual Book of ASTM Standards, Vol 11.02. Annual Book of ASTM Standards, Vol 11.04.
3 5
Annual Book of ASTM Standards, Vol 11.01. Available from the U.S. Government Printing Office, Washington, DC.
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D 5765
cavity should be constructed so as to prevent any possible in accordance with the manufacturer’s recommended safety
metal to metal arcing from occurring within the cavity. The precautions.
oven cavity should be equipped with an exhaust ventilation 8.2 The extraction vessels shall be used and maintained in
sufficient to provide ten chamber exchanges per minute. The a
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