Gypsum is a dihydrated calcium sulfate, with the composition of CaSO 4 ⋅2H 2 O, with large application interest in ceramic industry, odontology, sulfuric acid production, cement, paints, etc. During calcination, a phase transformation is observed associated to the loss of water, leading to the formation of gypsum or anhydrite, which may present different phases. The identification of the phases is not so easy since their infrared spectra and their X-ray diffraction patterns are quite similar. Thus, in this work, temperature modulated differential scanning calorimetry (TMDSC) was used to identify the different gypsum phases, which can be recognized by their different profiles.