A calorimetric, Differential Reaction Calorimetry (DRC), study of the thermochemical of the attack of a phosphate ore from Gafsa region (Tunisia) by a mixture of sulfuric and phosphoric acid is undertaken at different solid-liquid ratio and different temperature. The plot of the quantity of heat measured by integrating the raw signal as a function of the dissolved mass in the same volume solution at 25˚C presents three straight segments attributed at the formation of the hemihydrate (CaSO 4 •1/2H 2 O:HH), the dihydrate (CaSO 4 •2H 2 O:DH) or a mixture of these two products checked by X-ray diffraction, infrared spectroscopy and thermal analysis (Differential Scanning Calorimeter: DSC). The attack by the acid mixture was performed at higher temperature and showed in addition the formation of another form of calcium sulfate:anhydrous (CaSO 4 :AH). Moreover, the variation of mass enthalpy versus temperature presents a break at the T = 45˚C. According to our results, it seems that the effect of the temperature on the sulfo-phosphoric attack reaction on the natural phosphate (NP) generates a change of mechanism at around 45˚C.