Luminescence techniques are sensitive, selective, and widely used in analysis. Luminescence intensity is attenuated by quenchers. This research has focused on the use of surfactants such as CTAB, SDS, and TX-100 singly or together with TiO2 nanoparticles to evaluate their individual and combined effects on some fluorescent aromatic compounds such as pyrene, fluoranthene, anthracene, phenanthrene, and carbazole. Rutile phase TiO2 was synthesized using the low temperature sol-gel method. Carbazole and phenanthrene were severely quenched by all surfactants singly or in combination with TiO2. Anthracene and fluoranthene showed some enhancement in their luminescence intensity. The most dramatic effect was observed on the fluorescence intensity of pyrene. Pyrene showed enhanced fluorescence after degassing the solution alone or with the addition of the surfactants alone or in combination with TiO2 after degassing. These results showed that surfactants and TiO2 nanoparticles either singly or in combination should be useful for analysis employing luminescence techniques.