Chemical preparation, thermal behavior, kinetic and IR studies are given for the cyclotriphosphate Ca 3 (P 3 O 9 ) 2 . 10H 2 O. Ca 3 (P 3 O 9 ) 2 . 10H 2 O is monoclinic P2 1 /n with the following unit-cell dimensions : a = 9.332(7)Å, b = 18.13(1)Å, c = 7.841(5), β = 106.69(5)° and Z = 2. Ca 3 (P 3 O 9 ) 2 . 10H 2 O has never been studied except for its crystallographic characterization. The thermal behavior of Ca 3 (P 3 O 9 ) 2 .10H 2 O has been studied and interpreted by comparison with IR absorption spectrometry, X-ray diffraction experiments, chemical analyses, thermal analyses (TGA-DTA) and differential scanning calorimetry (DSC).