In recent decades, advanced oxidation process employing sulfate radical has emerged as a very promising method to remove recalcitrant organic pollutant in water. One of the most efficient ways to generate sulfate radical is by heterogeneous transition metal activation of peroxymonosulfate (PMS, available commercially as Oxone ® ). To date, many studies employed cobalt oxide catalysts which can potentially lead to the cobalt pollution due to cobalt leaching during treatment. In order to eliminate the cobalt leaching problem, the main objective of this study is to fabricate other types of metal oxide catalysts to activate PMS for the degradation of recalcitrant organic contaminants.In the first part of the study, a novel dipicolinic acid−functionalized Fe2O3 (DPA−Fe2O3) with high surface area was prepared by co−precipitation of a Fe(III)-DPA complex. It was used as a catalyst to activate PMS for bisphenol A (BPA) detoxification. A higher catalytic activity of DPA−Fe2O3 over other Fe(III)−based catalysts was observed for BPA oxidation in the presence of Oxone ® . The performance of the catalyst was optimized with respect to the initial pH, Oxone ® dosage and catalyst loading. The acute toxicity of BPA solution over time was studied using Vibrio fischeri bacteria and the results indicated that the evolution of acute toxicity was highly dependent on the initial Oxone ® dosage.In the second part of the study, the catalytic activity of Fe2O3 catalyst was successfully improved by incorporating Cu(II) during the co−precipitation synthesis to produce a mixed metal CuFe2O4-Fe2O3 catalyst for BPA oxidation via PMS activation. The formation mechanism of CuFe2O4-Fe2O3 is proposed. The performance of CuFe2O4-Fe2O3 as a PMS activator was compared with those of other catalysts and the results indicated that the performance was in the following order: CuFe2O4-Fe2O3 > CuFe2O4 > CoFe2O4 > CuBi2O4 > CuAl2O4 > DPA−Fe2O3 > MnFe2O4. A kinetic model with II mechanistic consideration of the influence of pH, PMS dosage and catalyst loading is developed to describe the degradation of BPA. The intrinsic rate constant (ki) was obtained from the kinetic study and the relationship between the pseudo first−order rate constant and ki was successfully established. The influence of water matrix species (i.e.Cl − , NO3 − , HCO3 − , PO4 3− and humic acid) on the BPA degradation rate was also investigated and the results indicated that Cl − and humic acid exerted noticeable reduction in the BPA degradation rate. The CuFe2O4-Fe2O3 catalyst exhibited excellent stability and could be reused several times without significant deterioration in performance.The third phase of this study involved the fabrication of an efficient bi−functional CuBi2O4 catalyst via a facile hydrothermal method to activate PMS and persulfate (PS) for benzotriazole (BTZ) removal. Characterization of the CuBi2O4 catalyst using XRD, FESEM, FTIR, BET and XPS revealed that it has a unique 3−D hierarchical structure with molecular formula of Cu1.2Bi1.6O3.6 and 2.4% w/w of CuO. The perfo...