In this investigation, a crystalline metaboric acid (HBO 2 ) powder was subjected to a dehydration process to transform it into boron oxide (B 2 O 3 ) using thermogravimetry (TG) technique in an argon atmosphere under non-isothermal conditions at different heating rates (3, 5, 10, and 15 °C min −1 ). The results of kinetic analysis revealed that the dehydration process was a complex one comprising a consecutive region (region I) followed by a parallel one (region II). Using the relevant kinetic models, the mechanisms involved in each region were analyzed by a proposed method for the complex reactions separately and find that the dehydration mechanism in the region I consisted of the kinetic models R 4 : g(α) = [1 − (1 − α) 2/3 ] (the chemical reaction at the HBO 2 /H 2 B 4 O 7 interface) and D 3 : g(α) = [1 − (1 − α) 1/3 ] 2 (the diffusion of H 2 O (g) in the H 2 B 4 O 7 layer), while that in the region II was parallel and consisted of the models D 3 (the diffusion of H 2 O (g) in the H 2 B 4 O 7 layer) and R 4 (the chemical reaction at the of H 2 B 4 O 7 /B 2 O 3 interface). Therefore, based on the kinetic results, the mechanisms of complex processes could be determined by the method.