Determination of some PAHs in ambient air at Ulsan have been carried out by collection of the components into n-hexane followed by synchronous spectrofluorimetric technique. 10 PAHs, such as acenaphthene (Ace), anthracene (Anth), benz[a]anthracene (BaA), benzo[b]fluoranthene (BbFt), benzo[k]fluoranthene (BkFt) benzo[a]pyrene (BaP), chrysene (Chry), phenanthrene (Phen), fluoranthene (Ft), perlyrene (Per), and pyrene (Pyr) in air samples were able to determine separately by synchronous spectrofluorimetry. Calibration curves for those components were linear for the concentration range of 0.2∼166ppb PAHs with the correlation factor of 0.9985∼0.9999. The predominant contribution was phenanthrene which was included 36.9∼85.1% to the overall level of the 10 PAHs in some areas. Also benzo[a]pyrene which was known to carcinogenicity was detected from 6.4 to 55.8ng/㎥, benzo[a]anthracene of some areas was contained from 21.9∼153ng/㎥.