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In wastewater, sulfides are the primary culprit among malodorous compounds that are most complained about by the general public. A study is made to explore the oxidation process for remediating sulfide from refinery spent caustic solution by means of Fenton's Reagent i.e. ferrous ion, Fe2+ and hydrogen peroxide, H2O2 under acidic condition. The pH adjustment step also contributed towards the objective as 65-70% of sulfide removed in the form of hydrogen sulfide gas, H2S. Elevation in the operating temperature indicates no advantage in terms of sulfide removal percentage thus the process is best done in ambient conditions i.e. 30°C. The optimum Fe2+ and H2O2/COD obtained from this experimental work is 75mg/L and 1.1, respectively. Almost all of sulfide is believed to convert to sulfate within 30-minutes of reaction time. Complete sulfide removal also caused the COD to be reduced by 43% and formation of sulfate in the form of sulphuric acid may be the reason of pH reduction of final effluent from 3.5 to 2.8.