Hydroxyl content of solution-precipitated calcium phosphates.

A method is described for determination of the titratable hydroxide ion in calcium phosphate precipitates. The procedure requires accurate analysis of the other titratable species in the crystal lattice but is unaffected by the presence of other lattice constituents or impurities. The method was applied to precipitates that had been previously analyzed by solution thermodynamic techniques, and the results were consistent with the earlier observations. The hydroxide content of the precipitates increased with crystal maturity and with increasing pH of the precipitation medium. The hydroxide content of the amorphous phase and the immediate postamorphous-crystalline transformation phase was shown to be nearly zero. After 3 to 4 days' maturation, the hydroxide content of precipitates prepared at pH values of 7, 8, and 9 was shown to increase to approximately 23, 40, 56% of that required for pure hydroxyapatite.