A solid-phase microextraction procedure has been developed for the determination of volatile organic compounds in water. Head-space extracted samples were analysed by gas chromatography with flame ionisation or electron capture detection and by mass spectrometry. The Carboxen/PDMS fiber was shown to have high affinity to selected aromatic and chlorinated compounds. The method showed good linearity between 0.1 µg.l^-1 and 8 µg.l^-1 with regression coefficients ranging from 0.9823 to 0.9995; the precision was from 1.0 to 17.9 %. The effect of septum used in head-space extraction was also investigated.