The extent of phenol degradation by the advanced oxidation process in the presence of zero valent iron (ZVI) and zero valent copper (ZVC) was studied using 20, 300 and 520 kHz ultrasonic (US) reactors. Quantification of hydrogen peroxide has also been performed with an aim of investigating the efficacy of different sonochemical reactors for hydroxyl radical production. It has been observed that the 300 kHz sonochemical reactor has the maximum efficacy for hydroxyl radical production. Phenol degradation studies clearly indicate that degradation of phenol is intensified in the presence of the catalyst and hydrogen peroxide, which can be attributed to enhanced production of hydroxyl radicals in the system. Experimental data shows that with ZVI, when the reaction was subjected to 300 kHz, complete phenol removal and 37% TOC mineralization was achieved within 25 min, whereas, in the case of 20 kHz US treatment no phenol was detected after 45 min and 39% TOC mineralization was observed. This novel study also investigated the use of zero valent copper (ZVC) and results showed that with 20, 300 and 520 kHz ultrasonic rectors, phenol removal was 10–98%, however, the maximum TOC mineralization achieved was only 26%. A comparative study between hydrogen peroxide and ozone as a suitable oxidant for Fenton-like reactions in conjunction with zero valent catalysts showed that an integrated approach of US/Air/ZVC/H2O2 system works better than US/ZVC/O3 (the ZOO process).