The optimum pretreatment method for a Pt-based spent catalyst for the removal of exhaust organic gases was examined. Two different pretreatment procedures with gas and aqueous solution were evaluated. Results obtained from the catalytic combustion of trace CH4 demonstrate that air pretreatment has a slightly positive effect. NaBH4 solution treatment leads to the highest initial activity. No pulverization of the granule size and sintering of the Pt nanoparticles happen after NaBH4 treatment. Results from the catalytic combustion of toluene indicate that the performance of the NaBH4-treated catalyst can be further improved by combination with air pretreatment.