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Abstract. In this work, problems related to calibration of solid phase microextraction (SPME) device were described. The effects of humidity and temperature on organic pollutants sampling from gaseous matrices on a 100 µm PDMS coated SPME fiber were studied. Standard gaseous mixtures used in these studies were generated by the permeation method and humidified to known levels of relative humidity. The SPME-GC-MS based procedure was used to determine organic vapours (carbon tetrachloride, toluene, chlorobenzene, p-xylene and n-decane) in a laboratory air. Key wo rd s. Solid phase micro ex t raction -gas ch ro m at ograp hy -calibration -vo l atile organic air pollutants -mass spectrometry.

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