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In this work, a study of the main operating variables affecting TiO₂/UV photocatalysis was carried out. The treatment of an industrial effluent containing aniline and benzothiazole from the manufacture of accelerants for vulcanization was performed in a TiO₂-supported commercial photoreactor. The degradation of both contaminants was monitored by GC-MS analysis. The proposed experiments were able to properly identify the phenomenon of adsorption, as well as to improve the performance of the commercial photoreactor by adding small amounts of TiO₂ in suspension. The removal performance, durability of the photocatalytic material, and energy costs were analysed. The results showed that the use of suspensions intensifies the degradation obtaining an improvement of 23.15% with respect to the use of the supported catalyst. For an aniline and benzothiazole solution, the best operating conditions were found at pH = 12.0, introducing 60.0 mg L^−1 of suspended TiO₂ together with the existing supported catalyst.