Nanocrystalline Pr-doped ceria powders were prepared for the first time by a microwave-assisted hydrothermal route. The effect of the microwave treatment in relation to the conventional hydrothermal technique was evaluated. The samples prepared were characterized in terms of composition, crystalline structure, particle shape and size distribution by X-ray diffraction, transmission electron microscopy (TEM) and specific surface area analysis (BET). The color properties of these solid solutions were also evaluated as a function of synthesis conditions and composition. Finally the oxidation state of the Pr cations and the relative quantities of Pr(IV) and Pr( III) were investigated by X-ray absorption at the M-4,M-5 Pr absorption edge.