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This study focused on a detailed examination of the thermal behavior of Brushite-based calcium phosphate (CaHPO 4 .2H 2 O, DCPD) to identify and characterize the intermediate phases which have been the subject of previous several controversies. For that, in situ high-temperature X-ray diffraction supported by infrared spectroscopy, thermal analysis, and scanning electron microscopy analysis were used and the results showed that the progressive thermal stress of DCPD in air resulted in a heterogeneous formulation consisting of dibasic calcium phosphate anhydrous (CaHPO 4 , DCPA) and an amorphous phase, which appears at low temperatures (~160 °C) and persists up to 375 °C. The deep examination of the amorphous phase by infrared spectroscopy revealed that its chemical composition is similar to that of disordered calcium pyrophosphate (Ca 2 P 2 O 7 , CPP) with the appearance of a characteristic band δ(P-O-P), located at 740 cm -1 . This IR band is shifted to low frequencies (725 cm -1 ) as the temperature is increased, indicating the crystallization of the amorphous phase into γ-CPP. The high temperature treatment (≥ 375 °C) leads to b-CPP polymorph. According to the present characterization results, obtaining pure DCPA from the thermal dehydration of DCPD is not effective and leads to biphasic materials including an amorphous phase.