CeO₂–γ-Al₂O₃ mixed oxides have been prepared by using both co-precipitation and impregnation methods followed by calcination at 650 1C and investigated by ²⁷Al MAS NMR, powder X-ray diffraction and temperature programmed reduction techniques to understand the nature of chemical interaction existing between CeO₂ and γ-Al₂O₃. The ²⁷Al NM Rspectra of CeO_2- containing samples showed an additional peak placed at 40ppm along with the two peaks at 68 and 6ppm which originate from the tetrahedrally and octahedrally coordinated Al³⁺ ions present in g-Al₂O₃. As the concentration of CeO₂ in the mixed oxide increased, the intensity of the 40ppm peak increased and this was the prominent peak for CeO_2- rich mixed oxide samples. The origin of this 40ppm peak is discussed and it is inferred that this peak is due to Al³⁺ ions, which are present in CeO₂ lattice, forming a solid solution.