Molten alkali metal nitrites or nitrates and co-precipitation methods were used to prepare CeO2, SnO2 and Ce0.5Sn0.5O2 solid solutions with high surface areas. In the case of the single oxides prepared by the molten salt method, the use of KNO3 leads to better crystallised solids than with KNO2, but on the opposite with higher particle sizes and lower BET surface areas. The same effect was observed for the preparation of the mixed oxides with different resulting structures. With KNO3, the mixed oxide appears as a mechanical mixture of the single oxides, whereas with KNO2, a mixture of amorphous SnO2 and of solid solution with a specific surface area (SSA) of 100 m(2) g(-1) has been synthesised, but without evidence Of Ce2Sn2O8 pyrochlore formation. The solid prepared by co-precipitation is also well dispersed. Its amorphous structure by X-ray diffraction (XRD) analysis does not allow to conclude to the formation of a solid solution.TPR experiments with hydrogen have shown a beginning of reduction at lower temperature in presence of the solid solution compared to the mechanical mixture of the single oxides. An improved reducibility was also observed with the oxide prepared by co-precipitation, which is in favour of a solid solution formation also in this case. Therefore, the resulting hydrogen consumption obtained when reducing the solid solutions at 450degreesC is very high and the oxygen storage capacities (OSCs) reach about 1 mmol O-2 g(-1), value higher than those obtained with ceria-zirconia solid solutions. The OSC values were confirmed by oxygen chemisorption on the reduced solid between 25 and 450degreesC. The full recovery of the initial solid solution was shown by XRD analysis and a second redox cycle has demonstrated the reversibility of the redox properties at this temperature. (C) 2003 Elsevier B.V. All rights reserved.