Laser excited luminescence combined with Shpolskii matrix techniques were used for the detection and identification of PAH pollutants in the atmosphere of the northern part of Zarqa city in Jordan. The weather conditions in that area are dry and dusty most of the year. The presence of the oil refinery plant and the thermal power station in addition to most of the local industries are considered as the major sources of pollution to the atmosphere of that area. The extent of pollution was detected by measuring the concentration levels of Polycyclic Aromatic Hydrocarbons (PAHs). Air samples from the airborne of Zarqa were collected at different time intervals using high volume air sampler. A clean-up procedure, soxhlet extraction, was used before subjecting samples to analysis. Gas Chromatography (GC) was used for quantitative analysis of sample components. Cooling the samples down to 77K was sufficient to produce an environment similar to Shpolskii matrix which is necessary for resolving the complex fluorescence spectra of PAH compounds. PAHs of low molecular weights such as fluorine, phenanthrene, chrysene, and the most dangerous carcinogen namely benz(a)pyrene, were dominant in all samples. The total average of PAHs concentration varied from (7.3 ng/m3) for benz(a)pyrene to (48.3 ng/m3) for phenanthrene.