In recent years the utility of extended x-ray absorption fine structure (EXAFS) as a probe for the study of catalysts has been clearly demonstrated [1–13]. Measurements of EXAFS are particularly valuable for very highly dispersed catalysts. Supported metal systems, in which small metal clusters or crystallites are commonly dispersed on a refractory oxide such as alumina or silica, are good examples of such catalysts. The rätio of surface atoms to total atoms in the metal clusters is generally high and may even approach unity in some cases. With such catalysts it is difficult or impossible to obtain structural information by conventional x-ray diffraction methods [14].