This research investigates the potential for zeolites containing transition metals to act as solid-phase-advanced oxidation catalysts in the destruction of chlorinated phenols in aqueous waste. Advanced oxidation processes utilize hydroxyl radicals to destroy organic micropollutants. The lack of selectivity of hydroxyl radicals leads to their loss from the system by reaction with other less toxic species ('scavengers'). The efficient use of the expensive hydroxyl radicals requires a solution to this problem. This work overcomes this difficulty by the selective adsorption of the target micropollutant onto an iron-loaded zeolite. The zeolite is then regenerated through the destruction of the adsorbed organics by in-situ Fenton oxidation. The iron-loaded zeolite acts as a catalyst in the advanced oxidation process. In control experiments, the effect of pH and contact time on the decomposition of hydrogen peroxide was studied using zeolites Beta and 4A, which contained iron (2+). The stability of the transition metal zeolites in terms of the leachability of the transition metal was determined by atomic absorption spectroscopy. Breakthrough experiments are reported for the removal of 2,4-dichlorophenol from aqueous solution at a concentration of 1.0 x 10(-3) M onto zeolite Fe-Beta in a 10 mm diameter x 125 mm adsorption column at a flow rate of 3 ml min(-1). Three regenerations of the column were achieved by the use of hydrogen peroxide solution (5 x 10(-2) M) at pH 3.5. The zeolite Fe-Beta successfully catalysed the decomposition of the hydrogen peroxide to hydroxyl radicals, which then degraded the adsorbed organics. No significant deterioration in crystallinity due to the regeneration cycles was detectable by X-ray diffraction.