Application Method ME003

ASTM D-5765: Solvent extraction of Total Petroleum Hydrocarbons from soils

and sediments using closed vessel microwave heating

Introduction Results
This practice covers the solvent extraction of total petroleum Typical analyte recoveries are shown in tables below.
hydrocarbons (TPH) from soils and sediments, using closed
vessel microwave heating, for subsequent determination by Total petroleum hydrocarbon recovery data
gravimetric or gas chromatographic techniques.
TPH TPH
Measurement
Instrumentation Material Present Recovered
method
(%) (%)
Microwave heating system: a laboratory microwave heating
system capable of delivering a minimum of 900 W of microwave Soil 1.34 a 1.32 Gravimetric
energy. The system should be capable of 1% power
Soil b 0.214 0.223 Gravimetric
adjustments and 1-s time adjustments. The microwave unit
must be capable of measuring and controlling solvent Soil
b
0.099 0.094 GC-FID
temperature within an extraction vessel. The microwave cavity
should be constructed so as to prevent any possible metal to a
Value determined by Soxhlet extraction.
metal arcing from occurring within the cavity. The microwave
b
cavity should be equipped with an exhaust ventilation and Environmental Resource Associates (ERA) standard
should contain a sensor capable of detecting solvent reference soil.
concentrations below their lower explosive limits and shutting
the microwave source off. The cavity shall have a 360° Procedure
oscillating turntable to ensure even sample heating and be
1. Take a 5 g portion of the sample, weigh to the nearest
capable of removing contained vessel-vented solvents. Safety
0,1 mg and transfer into the extraction vessels.
interlocks to shut off the magnetron power output shall be
contained in the cavity door opening mechanism. 2. Add 30 ml of Acetone-Hexane (1:1 v/v) to each sample.
3. Close each extraction vessel.
Extraction vessel: the vessel consists of a fluoropolymer inner
liner and cover to contain and isolate a solvent solution from a 4. Place the closed extraction vessel onto the rotor body.
higher strength polymer outer pressure vessel body. The vessel 5. Place the rotor into the microwave cavity and make the
assembly shall be transparent to microwave energy and proper connection to the reference vessel.
capable of withstanding an internal pressure of 400 psi and a
6. Heat the vessels according to the microwave program.
temperature of 250°C. The vessel assembly shall contain a
safety pressure relief device that will prevent possible vessel 7. Allow the vessel to cool to room temperature.
rupture and be connected to a sealed venting system capable 8. Open the vessel, add 5 g of sodium sulphate and
of removing vented solvent vapours from the microwave cavity. solvent mixture to the sample and then gently swirl the
extraction mixture.
Sample
9. Filter the extract mixture through ashless filter paper
Up to 5 g of sample. rinsing and washing the extracted, sample, sodium
sulphate and filter paper thoroughly with
Acetone/Hexane (1:1 v/v) into an appropriate container.

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Extraction solvent 10. Proceed with an appropriate procedure for gravimetric
or gas chromatographic determination.
30 ml of Acetone-Hexane (1:1 v/v).

Comments
Microwave Program
Rapid heating in combination with temperatures in
excess of the atmospheric boiling point of organic solvents,
Time Power Temperature reduce sample extraction times. Small amounts of solvents
Step
(min) (W) (°C) (30 ml) are used resulting in reduced sample preparation
cost and time.
1 10 Up to 1000 * 150
Reference
2 15 Up to 1000 * 150
• D 3856 Guide for good laboratory practices in
laboratories engaged in sampling and analysis of
*Use up to 500 Watt for operations with 3 or less vessels water (Annual book of ASTM Standards, Vol 11.01).
simultaneously.
• D 3976 Practice for preparation of sample containers
and for preservation of organic constituents. (Annual
Temperature Profile book of ASTM Standards, Vol 11.02).

• D 5368 Test method for evaluating solid waste

volume 1A: Laboratory manual physical/chemical
methods (Annual book of ASTM Standards, Vol
11.04 ).

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