Azo dyes have been used in many industries (textile mill, printing and dyeing mill, paper and pulp mill) and have caused great environmental pollution due to complicated constitution and high chemical stability. The construction of azo dyes can be destroyed by ozonization, but not thoroughly when the ozone dosage is controlled to a certain extent and the operating cost is higher. Ozonization decomposed ability with ultrasonic enhancement on azo dyes has been demonstrated in the study. The conclusion derived from this investigation may be summarized as follows: (1) The decoloration rate of arsenazoⅠsolutions during sonozone treatment is more rapid than the rate obtained with ozone alone because the complicated constitution has been destroyed by the O free radical from ozone decomposition. (2) The destructing pathway of arsenazoⅠby ozone with ultrasound is identical with that of by ozone alone: the breakdown of -N== N- bonds, the conversion of benzene ring to carboxylic acid, and -HSO3 bonds to H2SO4. So, pH value of the arsenazo Ⅰ solution continuously drops down to 3.2.