Abstract The influence of temperature and sulfuric acid concentration on the enthalpy and the rate of heat release during the reaction of Norwegian and Australian ilmenites with sulfuric acid was determined. The experimental results obtained from calorimetric measurements were compared with theoretical calculations based on the oxide composition and the phase composition of the raw material. Experimentally determined heat of reaction for Norwegian ilmenite (900–940 kJ/kg) and Australian ilmenite (800–840 kJ/kg) showed good agreement with theoretical calculations based on the phase composition of the raw material. It was found that the enthalpy of ilmenites decomposition reaction does not depend on the concentration of sulfuric acid in the concentration range from 83% to 93%. It was also demonstrated that the temperature and concentration of sulfuric acid have a significant impact on the thermokinetics of the decomposition process, increasing the value of the average rate of temperature change.