. The study combined UV/TiO2 with ultrasonic procedure to degrade azo dye wastewater of Acid Yellow 17. The effects of factors including pH value, initial concentration of dye, and quantities of TiO2, Fe (II), and Fe (III) added on the removal efficiency of azo dye Acid Yellow 17 were investigated. Experimental results revealed significant additive effect attributed to the combination of two procedures under 13-watt UV irradiation and 10-watt ultrasound. Analysis of the catalyst properties indicated no evident changes in the appearance of crystal and TiO2 catalyst by UV/TiO2 combined with ultrasonic procedure. However, the specific surface area was increased by approximately 53%. No effective formation of hydrogen peroxide (ND 1 mg/L) proved that the addition of Fe (II) and Fe (III) failed to induce the Fenton-like reaction effectively. Nevertheless, the addition of Fe ions affected significantly the initial adsorption and the degradation rate of the dye. Moreover, the treatment efficiency of Fe (III) was found to be superior to that of Fe (II) under the same concentration.