The structure of carbon supported platinum electrocatalysts for the direct methanol fuel cell has been studied using extended X-ray absorption fine structure (EXAFS) in both gas treatment and electrochemical environments. The EXAFS of the as prepared catalyst indicates that the preparation of the dispersed Pt by the oxidation of Pt(SO3)(4)(6-) forms dispersed PtOx species. After reduction by either flowing hydrogen in the gas treatment cell or potentiostatically in the electrochemical cell small Pt particles are formed as indicated by the presence of Pt neighbours in the first coordination shell. Carbon neighbours from the support are also evident in the first coordination shell. at 2.6 and 3.6 Angstrom.