The solid-phase microextraction (SPME) technique coupled with gas chromatog
raphy and atomic emission detection was successfully applied for the determ
ination of selected organometallic species of Pb, As and He in aqueous samp
les. To obtain a high extraction yield, the SPME conditions were optimised
for each element by fibre selection and varying the exposure time, stir-rin
g rate, pH range and desorption time. All the organometallic compounds test
ed were extracted from the aqueous phase using SPME. The preconcentration f
actors attained ranged between 40 and 150, depending on the compound. Detec
tion limits in the pg/L and ng/L ranges were achieved.