A novel pretreatment technique was applied to the conventional Pt/alumina catalyst to prepare for the highly efficient catalyst for the preferential oxidation of carbon monoxide in hydrogen-rich condition. Their performance was investigated by selective CO oxidation reaction. CO conversion with the oxygen-treated Pt/Alumina catalyst increased remarkably especially at the low temperature below 100℃. This result is promising for the normal operation of the proton exchange membrane fuel cell (PEMFC) without CO poisoning of the anode catalyst. XRD analysis results showed that metallic Pt peaks were not observed for the oxygen-treated catalyst. This implies that well dispersed small Pt particles exist on the catalyst. This result was confirmed by high resolution transmission electron microscopy (HRTEM) analysis. Consequently, it can be concluded that highly dispersed Pt nanoparticles could be prepared by the novel pretreatment technique and thus, CO conversion could be increased considerably especially at the low temperatures below 100℃.