The effect of an anodic treatment on the methanol oxidation activity of PtRu/C (50:50at.%) and PtNiCr/C (Pt:Ni:Cr=28:36:36at.%) catalysts was investigated for various potential limits of 0.9, 1.1, 1.3 and 1.4V (vs. reference hydrogen electrode, RHE). NaBH4 reduced catalysts were further reduced at 900°C for 5min in an argon balanced hydrogen flow stream. Improved alloying was obtained by the hydrogen reduction procedure as confirmed by X-ray diffraction results. In the PtRu/C catalyst, a decrease of irreversible Ru (hydrous) oxide formation was observed when the anodic treatment was performed at 1.1V (vs. RHE) or higher potentials. In chronoamperometry testing performed for 60min at 0.6V (vs. RHE), the highest activity of the PtRu/C catalyst was observed when anodic treatment was performed at 1.3V (vs. RHE). The current density increased from 1.71 to 4.06Agcat. −1 after the anodic treatment. In the PtNiCr/C catalyst, dissolution of Ni and Cr was observed when potentials ≥1.3V (vs. RHE) were applied during the anodic treatment. In MOR activity tests, the current density of the PtNiCr/C catalyst dramatically increased by more than 13.5 times (from 0.182 to 2.47Agcat. −1) when an anodic treatment was performed at 1.4V. On an Agnoble metal −1 basis, the current density of PtNiCr-1.4V is slightly higher than the best anodically treated PtRu-1.3V catalyst, suggesting the PtNiCr catalyst is a promising candidate to replace the PtRu catalysts.