Plate shape NaZnPO4·H2O was synthesized by solid-state reaction at low temperature and characterized by X-Ray Diffraction, Scanning electron microscope and elemental analysis. Thermochemical study was performed with an isoperibol solution calorimeter. Based on Hess’s law, thermochemical cycl was designed to determine the dissolution enthalpies of reactants and products using a solution-reaction isoperibol calorimeter at 298.15 K, and the molar reaction enthalpy was calculated on the basis of above dissolution enthalpies. The results show that the obtained product is plate shape NaZnPO4·H2O. The standard molar formation enthalpy of the NaZnPO4·H2O is ΔfHm [NaZnPO4·H2O,s]= -1967.18 ± 0.69 kJ•mol-1.