Nanocrystalline CeO2 has been synthesized at room temperature using water-in-oil (w/o) microemulsion technique. The structure and properties of the nanocrystalline CeO2 were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), and gas adsorption desorption measurement. XRD results showed the synthesized CeO2 has a face centered cubic structure with crystallite size of about 5.2 nm. TEM observation also indicated the presence of nanometer sized particles of CeO2. Coarser particles were also observed due to agglomeration. Gas adsorption desorption isotherms showed the behavior of fine particles with mesoporous structure.