Published:Journal of Chromatographic Science,
ISSN 0021-9665Volume
39, Number 11, November 2001, pp. 481-486
Determination
of Petroleum Hydrocarbons in Contaminated Soils Using Solid-Phase Microextraction
with Gas Chromatography–Mass SpectrometryD.
Cam* and S. Gagni Montecatini Environmental Research Center, Via
Ciro Menotti 48, 48023 Marina di Ravenna (RA), Italy
Manual solid-phase microextraction (SPME) coupled with gas chromatography–mass
spectrometry is investigated as a possible alternative for the determination
of petroleum hydrocarbons in soils. Spiked onto an agricultural soil is a commercial
diesel fuel (DF) with the following composition by weight: 12% linear alkanes,
52% saturated hydrocarbons (branched and cyclic), 21% alkylated aromatic hydrocarbons,
6% polycyclic aromatic hydrocarbons, and 9% unidentified compounds. The spiked
soil samples are aged three days at room temperature before analysis. The optimal
conditions for the SPME of DF from soils are examined and maximum sensitivity
is obtained using a 100-µm polydimethylsiloxane fiber at a sampling temperature
of 47°C by sonication both in the headspace and directly through a water
medium. The reproducibility of the whole technique showed a relative standard
deviation of 10%. The parameters that can influence the recovery of DF (such
as the time of SPME extraction, the presence of organic solvent and water, and
the matrix) are investigated. The linearity is verified in the range of 40 to
1200 mg/L for the direct injection of DF, 0.1 to 1 mg/L for the SPME of DF from
water, and 1 to 50 mg/Kg of dry soil for the SPME of DF from soils. The detection
limits are respectively 0.5 mg/L, 0.02 mg/L, and 0.1 mg/Kg of dry soil. The
method is corroborated by comparing the results with those obtained by the traditional
way.
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