The homogeneous advanced oxidation process of ultraviolet (UV) radiation in presence of hydrogen peroxide (H2O2) was utilized to degrade Alizarin Yellow R, one of the most commonly used azo dyes in the textile industry. In this study, the effects of initial H2O2 concentration, initial dye concentration, initial pH, and temperature were examined to determine the optimum conditions for maximum degradation. Complete degradation was achieved within 1 h, for all the experimental conditions studied in the present work. The Box-Behnken response surface methodology (RSM) was used for optimizing the variables of the degradation process. Based on the estimated optimum conditions, 92.7 of degradation was achieved. The degradation process was found to follow first order kinetics. The estimated rate constants, along with the optimized conditions will be of useful for the design and scale up of the combined UV/H2O2 process for the said purpose. Copyright © 2013 American Institute of Chemical Engineers Environ Prog.