The specific chemical, structural and morphological properties of calcium phosphates are highly sensitive to the changes of synthesis conditions. As many characteristics, e. g., purity, solubility, bioactivity, depend on chemical composition and crystal structure of synthesized calcium phosphates it has been studied extensively during last year. Influence of technological parameters on chemical composition of as-prepared and calcined calcium phosphates samples was investigated. Calcium phosphates powders have been synthesized by wet-chemical precipitation rout using CaCO3 and H3PO4 as starting materials. These synthesis series vary with following technological parameters: temperature of the suspension during the process of synthesis (T, °C), ending pH value, aging time of suspension (τ, h) and thermal processing (T, °C; τ, h). The identification and characterization of obtained calcium phosphates powders chemical composition has been made with Fourier Transform Infrared Spectroscopy method. FT-IR spectra of as-synthesized calcium phosphates powders showed characteristic chemical bands (PO4 3-, OH-, H2O absorbed, CO32- , HPO4 2-) at definite wave number ranges. The as-synthesized powders are non-stoichiometric hydroxylapatite (HAp) with the presence of CO3 2-, OH- and H2O absorbed bands. Carbonate and OH- absorbed bands can be perfectly removed after calcination above 900°C. The experimental results of X-ray diffraction and FT-IR spectra have shown the presence of biphasic mixtures containing HAp and β-tricalciumphosphate (β-TCP). The secondary phase of β-TCP was also formed after HAp samples heating at 1000°C and above.