Determination of hydrocarbons in old creosote contaminated soil using headspace solid phase microextraction and GC-MS

Abstract

Headspace solid phase microextraction (HS-SPME) has been used together with GC-MS to analyze organic substances directly in a soil, heavily contaminated with PAHs/creosote (approximately 300 mg/kg soil), from an old gaswork site in Stockholm, Sweden. The HS-SPME results, both qualitative and quantitative, were compared with traditional liquid extraction using ethyl acetate/hexane (20:80). It was shown that the concentrations determined with HS-SPME at 60 degrees C correlated well, for compounds containing up to two and three aromatic rings (naphthalenes, acenaphthene, acenaphthylene and fluorenes, while a lower concentration was obtained for phenanthrene, anthracene, fluoranthene and pyrene. The total concentrations for each compound determined with HS-SPME ranged from 2 to 25 microg/g soil. Quantification was done using standard addition of compounds directly to the soil samples. The bioavailable fraction of the compounds in the contaminated soil at 20 degrees C was analyzed using external calibration by spiking sterile uncontaminated sand (same texture and particle size as the contaminated soil but without a heavily sorbed organic fraction) with hydrocarbon standards in different concentrations. Storage of exposed fibers at 20 degrees C showed that analysis should be done within two days to make qualitative measurements and earlier (as soon as possible) for quantitative determinations.