A process to produce calcium phosphate biomaterial was done using an organic based diethylhexyl phosphoric acid (DEHPA) as its starting material. The gel obtained from this reaction was used to study calcium phosphate transformation using in-situ XRD with temperature ranges from room temperature to 1300 o C. The results obtained from this analysis show the following phase transformation sequence gel > β-Ca2P2O7 > β-TCP + HA > α-TCP + HA. β-Ca2P2O7 was formed at 400 o C and the sample when heated up to 1000 o C, peaks of β- TCP and HA appeared showing the transformation of the β-Ca2P2O7 phase. When the sample was heated up further to 1200 o C, β-TCP transformed into α-TCP.