By means of thermal analysis,the thermogravimetry(TG) curves,derivative thermogravimetry(DTG) curves and differential thermal analysis(DTA) curves of the CaC2O4·H2O in different experimental conditions,including sample weight,grain size,heating rate and atmosphere are studied.The optimality thermal analysis of the CaC2O4·H2O by analyzing the TG-DTA comprehensive analysis is concluded in this paper.