This study aimed to evaluate the implementation of an advanced oxidation system based on UV radiation and UV/H 2 O 2 for degradation of TCS and IBU in synthetic effluent. The assays occurred in a 2-L reactor, protected from external light and equipped with a UV lamp ( λ = 254 nm). The effect of contaminant concentration, fractions of chemical species present, and mineralization were evaluated. In the UV/ H 2 O 2 system, different concentrations of H 2 O 2 were studied for oxidation of the contaminants. The kinetic experiments took place between 75 and 270 min of UV irradiation. The results showed > 99% oxidation of TCS in the direct photolysis system at pH 9.4 after 12 min. The degradation of IBU in the UV/H 2 O 2 system, when 10 mg L −1 of H 2 O 2 was used, was 97.39% oxidation. We obtained k′ values of 0.189 min −1 for TCS when its highest oxidation occurred and k′ values of 0.0219 min −1 for IBU. The system was not able to completely mineralize the contaminants, presenting high values of TOC and COD after treatment, thus suggesting the occurrence of phototransformation. Supplementary Information The online version contains supplementary material available at 10.1007/s11270-022-05583-z.