The investigation of the thermal behavior of calcium fructoborate samples of composition Ca(C<SUB>6</SUB>H<SUB>10</SUB>O<SUB>6</SUB>BO)<SUB>2</SUB>.3.5H<SUB>2</SUB>O showed that CaB<SUB>2</SUB>O<SUB>4</SUB> is generated as the final solid pyrolysis residue. On the basis of these observations a new, very easy, synthetic procedure for the preparation of high purity samples of this calcium borate is proposed. The material was characterized by X ray powder diffractometry and IR spectroscopy.Facultad de Ingeniería