An advanced oxidation treatment, UV/H2O2, was applied to an azo dye, Hispamin Black CA, widely used in the Peruvian textile industry. Rates of color removal and degradation of the dye have been evaluated. A strongly absorbing solution was completely decolorized after 35 min of treatment, and after 60 min an 82% reduction of the total organic carbon (TOC) was obtained. It has been found that the degradation rate increased until an optimum value, beyond which the reagent exerted an inhibitory effect. The degradation rate was also function of pH.