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The thermokinetic mathematical models for consecutive first-order reactions in titration period and the stopped-titration reaction period were proposed for titration calorimetry, based on which, thermodynamic parameters (reaction enthalpies, Δ r H m1 and Δ r H m2 ) and kinetic parameters (rate constants, k 1 and k 2 ) of the consecutive first-order reactions could be obtained by directly simulating the calorimetric curve from a single experiment with the method of nonlinear least squares regression (NLLS). The reliability of the model has been verified by investigating the reaction of the saponification of diethyl succinate in an aqueous ethanol solvent.