The standard enthalpy of formation ( Δ \-f H\+\+ \-\-m[K\-2Zn(IO\-3)\-4·2H\-2O,s,298.2K]=-2210.68 kJ·mol\+\{-1\}) of a double salt K\-2Zn(IO\-3)\-4·2H\-2O is determined by solution calorimetry in a isoperibel reaction calorimeter. The calorimetric solvent is an acid solution consisting of 3 mol·L\+\{-1\} HNO\-3. Accoding to the HESS Law, we designed a rational thermochemical cycle. Simultaneously, the Δ \-f H\+\+ \-\-\{m 298.2K\} was calculated from the data of the DSC curve. The values obtained by the two methods were compared.