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This paper investigated the degradation of sulfidic spent caustic by using photo-Fenton oxidation process. Response surface methodology was employed to study the interaction effect between process parameters namely ferrous ion and H2O2 dosage towards the oxidation efficiency of sulfidic spent caustic. Hence, the best conditions for photo-Fenton process were determine based on the developed empirical model. By comprehensive studies, the optimal conditions of photo-Fenton reaction are at dosage ratio Fe/H2O2 and H2O2/COD of 0.07 and 1.84 correspondingly.