Spherical, monosized gadolinium compound was prepared by the reaction of Gd(NO3)3 solution with decomposition products of urea in the solution at evaluated temperature. Chemical composition and calcination characteristics of spherical gadolinium compound prepared were investigated by X-ray IR and TG-DTA. The approximate chemical composition of the spherical particle precipitated was Gd(OH)CO3.1.5H2O. Gd(OH)CO3.1.5H2O was calcined to monoclinic type Gd2O3 at 115$0^{circ}C$ via cubic type Gd2O3 near $600^{circ}C$. The effects of various parameters such as pH, temperature, concentration ratio of urea to gadolinium precusor, ageing time, and others material (CCl3COOH and HOCNH2) in stead of urea as precipitating agent on the properties of the resulting precipitates were studied systematically.