The thermogravimetry (TGA) and derivative thermogravimetry (DTG) methods have been used to measure the free water in low-moisture foods. In this study, the 2nd derivative thermogravimetry (2nd DTG) method distinguished the free and bound water based on the speed of moisture evaporation, which could be used for both low-moisture and high-moisture foods. First, the key factors related to moisture evaporation were optimized. Isothermal temperature of 30 ~ 50°C, dynamic temperature of 0.033 ~ 0.133°C/min, and flow rate of nitrogen of 20 ~ 40 mL/min were the optimal parameters for the 2nd DTG method. Under these conditions, the repeatability and reproducibility of the 2nd DTG method were enhanced, its applicability was expanded to high-moisture foods, and the accuracy was ± 4.0% of the nuclear magnetic resonance results. Hence, the 2nd DTG method is better suited for the measurement of free water in foods.