We have evaluated an analytical method for the determination of polycyclic aromatic hydrocarbons (PAHs) and sulfur compounds in air by means of adsorption/temperature‐programmed thermal desorption (ATPTD) with small bed volume (0.08g) Tenax‐TA cartridges, followed by a cryogenic trap in a precolumn with liquid nitrogen as an appropriate concentration method before capillary gas chromatography is described. The enriched components from the adsorption cartridges are transferred to the capillary column with a valveless switching system. Recoveries were determined for the complete ATPTD method. Desorption recoveries near 100% were found for various of polycyclic aromatic hydrocarbons and sulfur compounds. The sulfur compounds known to cause nuisance odors in the atmosphere near sulfur recovery and sewerage treatment works were also determined.