Nanocrystalline ceria has been synthesized by a non-hydrolytic method using organic solvent and precipitant. The effect of the source compound on final nanocrystalline powder was investigated. The cerium nitrate hexahydrate subjected to different vacuum/thermal treatments to get cetium source compound having different extent of water of crystallization. The nanoceria, synthesized from these compounds was characterized by TGA-MS, XRD, HR-TEM and AFM. (C) 2005 Elsevier B.V. All rights reserved.