In this work, analytical methods based on room-temperature phosphorimetry were developed aiming the quantification of seven polycyclic aromatic compounds (PAC) containing sulfur and nitrogen present in petroleum. More specifically, the goal was to obtain analytical tool to allow the evaluation and the quantification of these PCA in sediment and gasoline. In addition, the phosphorimetric information displayed potential for the discrimination of samples (for instance, the identification of contaminated samples) by means of three dimension plots or level curves. The application of synchronized sweeping technique and the use of the selective external heavy atom effect had increased the degree of selectivity and discrimination between samples, since it induces phosphorescence from specific components of the sample and improved the spectral resolution of the results. Initially, a study of the phosphorescent characteristics of the compounds in different experimental conditions was made, followed of the signal maximization in the most appropriate experimental conditions for the observation of phosphorescence. Filter paper, previously treated for background reduction, was employed as solid substrate for the immobilization of analytes. The analytical figures of merit for each one of the methods had been obtained. The linear range varied between 1,0 x 10-7 mol L-1 and 5,0 x 10-4 mol L-1, taking into consideration the concentration of the solutions spotted on the substrate. The determination coefficient values (r2) were always above of 0.9784. The absolute limits of detection (5 µL sample) were in ng order, showing the sensitivity of the developed methods. The repeatability tests had enabled values varying between 12 and 18%, which can be considered satisfactory for solid substrate technique. Robustness and reproducibility studies were also carried out. Additionally, secondary experimental conditions, in terms of signal magnitude, were optimized since these could be relevant from the selective point of view. Recovery tests indicated, in most of the cases, satisfactory results for synthetic mixtures containing equimolar quantities of components (in these cases, several analyte/interferent combinations were tested) and containing interferents in concentrations five times higher than the one of the analytes. In the most critical cases in terms of interferences, instrumental or quimiometric approaches had been applied to improve selectivity and make the quantification possible. The developed methods had been tested in simulated gasoline samples, commercial gasoline and in a sediment sample fortified with the analytes of interest. The obtained recoveries had been considered satisfactory and within 90 and 117%. Total phosphorescence scanning (TPS) studies had been also carried out in order to get the characteristic fingerprint for each one of the compounds of interest. TPS tests in gasoline had indicated the presence of six out of seven of the studied analytes, since very similar fingerprints were obtained. Additional tests had demonstrated the capability of this procedure to detect gasoline contaminations with diesel or kerosene.