Department of Chemistry, University of Allahabad, Allahabad-211 002, Uttar Pradesh, India E-mail : mcc46@rediffmail.com, nnc2004200l@gmail.com Manuscript received 19 February 2010, revised 04 June 2010, accepted 21 June 2010 In this paper ultrafine powder of gadolinia doped ceria was prepared by a combustion synthesis method using metal nitrates, both as a precursor and oxidizer and glycine as fuel for combustion. The influence of glycine to metal molar ratio on the characteristics of the powders has been studied. Characterization of the powder samples was performed using, FTIR spectroscopy, TG/DTA analysis, X-ray diffractometry, Small angle X-ray scattcering (SAXS) technique and scanning electron microscopy. The ultrafine powders prepared by glycine to metal ratio 1.2 gives the best powder properties. The indexing or diffraction pattern shows that the gadolinia doped ceria powders have face centered cubic symmetry.