The metallic semiconductor of TiO2 was immobilized in thin-film during UV photodegradation of AY-36. Immobilizing the catalyst allowed H2O2 to be present at the start of photodegradation without fear of recombination, electron band competition, and destruction of immobilized photocatalyst. The photodegradation of AY-36 was improved by 90%. Decolorization in the present method was begun more slowly but by 75 min, no difference was observed. An enzymatic method has been conducted to accurately measure the formation of extra-H2O2 concentration and its decomposition. The pH needed no adjustments; it increased slightly instead of decreasing as was seen in the previously tried AOP methods. This method has the potential of both increasing degradation and slightly reducing costs in practice.