Zirconium titanate and magnesium aluminate spinel precursors were prepared by non-hydrolytic sol-gel method using ethanol as oxygen donor. The gels and calcined powders were investigated by differential thermal analysis (DTA), thermogravimetry analysis (TG), X-ray diffraction (XRD). The results show that the ZrTiO4 and MgAl2O4 crystallized at low temperature of 550 °C and 700 °C, respectively. It indicated that the highly homogeneous zirconium titanate and magnesium aluminate gels were aslo obtained by nonhydrolytic sol-gel process using ethanol as oxygen donor. The particle size distribution measured by laser scattering exhibit that ZrTiO4 and MgAl2O4 powders were large soft agglomerates which could be broken through milling process.