ASTM D5765-05(2010)
(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
SIGNIFICANCE AND USE
Solvent extraction of soils and sediments can provide information on the availability of petroleum hydrocarbons to leaching, water quality changes, or other site conditions.
Rapid heating, in combination with temperatures in excess of the atmospheric boiling point of acetone/hexane, reduces sample preparation or extraction times.
Reduced amounts of solvents are required and solvent loss due to boiling and evaporation are eliminated by use of closed extraction vessels.
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: D5765 − 05(Reapproved 2010)
Standard Practice for
Solvent Extraction of Total Petroleum Hydrocarbons from
Soils and Sediments Using Closed Vessel Microwave
Heating
This standard is issued under the fixed designation D5765; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope D3974 Practices for Extraction of Trace Elements from
Sediments
1.1 This practice covers the solvent extraction of total
D3976 Practice for Preparation of Sediment Samples for
petroleum hydrocarbon (TPH) from soils and sediments, using
Chemical Analysis
closedvesselmicrowaveheating,forsubsequentdetermination
D5368 Test Methods for Gravimetric Determination ofTotal
by gravimetric or gas chromatographic techniques.
Solvent Extractable Content (TSEC) of Solid Waste
1.2 This practice is recommended only for solid samples
Samples
that can pass through a ten mesh screen (approximately 2 mm
2.2 Federal Standard:
openings).
Code of Federal Regulations, Title 21, Part 1030, and Title
1.3 The solvent extract obtained by this practice may be
47, Part 18
analyzed for total or specific nonvolatile and semivolatile
3. Summary of Practice
petroleum hydrocarbons but may require sample clean-up
procedures prior to specific compound analysis.
3.1 The chemical portion of this practice involves solvent
extraction to dissociate petroleum hydrocarbons from the
1.4 This practice is limited to solvents that are recom-
mended for use in microwave solvent extraction systems. matrix.
3.2 The sample is extracted with acetone/hexane in a sealed
1.5 The values stated in pounds per square inch (psi) are to
be regarded as the standard. The SI units given in parentheses microwave transparent vessel using microwave heating to an
internal temperature of 150 °C.
are for information only.
1.6 This standard does not purport to address all of the
3.3 This practice provides a sample suitable for analysis by
safety concerns, if any, associated with its use. It is the
gas chromatography or gravimetric measurements.
responsibility of the user of this standard to establish appro-
4. Significance and Use
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazard
4.1 Solvent extraction of soils and sediments can provide
statements are given in Section 8.
information on the availability of petroleum hydrocarbons to
leaching, water quality changes, or other site conditions.
2. Referenced Documents
4.2 Rapid heating, in combination with temperatures in
2.1 ASTM Standards:
excess of the atmospheric boiling point of acetone/hexane,
D3694 Practices for Preparation of Sample Containers and
reduces sample preparation or extraction times.
for Preservation of Organic Constituents
4.3 Reduced amounts of solvents are required and solvent
D3856 Guide for Management Systems in Laboratories
loss due to boiling and evaporation are eliminated by use of
Engaged in Analysis of Water
closed extraction vessels.
This practice is under the jurisdiction of ASTM Committee D19 on Water and
5. Interferences
is the direct responsibility of Subcommittee D19.07 on Sediments, Geomorphology,
and Open-Channel Flow.
5.1 No interferences to the extraction of soils and sediments
Current edition approved June 15, 2010. Published December 2010. Originally
using microwave heating have been observed.
approved in 1995. Last previous edition approved in 2005 as D5765 – 05. DOI:
10.1520/D5765-05R10.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
Standards volume information, refer to the standard’s Document Summary page on 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
the ASTM website. www.access.gpo.gov.
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D5765 − 05 (2010)
TABLE 1 Extraction Heating Parameters
5.2 Precautions should be exercised to avoid those interfer-
ences normally associated with the final determination of total Microwave power 100 %
Vessels pressure 200 psi
petroleum hydrocarbons using gas chromatography or gravi-
Vessels temperature 150 °C
metric techniques.
Heating time at 150°C 15 min
6. Apparatus
6.1 Microwave Heating System—A laboratory microwave
heating system capable of delivering a minimum of 900 W of
7.2 Acetone, HPLC grade.
microwave energy. The system should be capable of 1 %
power adjustments and 1 s time adjustment. The microwave
7.3 Hexane, HPLC grade.
cavity should be constructed so as to prevent any possible
7.4 Sodium Sulfate—Reagent grade, granular, anhydrous,
metal to metal arcing from occurring within the cavity. The
prepared by heating at 400°C for a minimum of 4 h.
oven cavity should be equipped with an exhaust ventilation
7.5 Ashless Filter Paper.
sufficient to provide ten chamber exchanges per minute. The
ventilation exhaust should contain a solvent sensor capable of
8. Hazards
detecting solvent concentrations below their lower explosive
limits and shutting the microwave source off. The cavity shall
8.1 Themicrowavesystemshallbeoperatedandmaintained
have a 360° oscillating turntable to ensure even sample
in accordance with the manufacturer’s recommended safety
heating, and be capable of monitoring and control of solvent
precautions.
temperature using either an in-situ control vessel or by external
8.2 The extract
...
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