Dissolved-air flotation has been investigated in the present paper as a suitable solid/liquid separation technique, applied downstream for hydroxyapatite ultrafine particles which were used in a preliminary stage for the removal by sorption of toxic cadmium cations. The main parameters affecting this process were evaluated, including the necessary quantity of sorbent material in the dispersion, the proper pH values of Cd solutions, the type and concentration of supplementary inorganic flocculant agents (ferric chloride and aluminum sulfate), and the presence of additional surfactant added. The results obtained were considered to be promising. Under optimum conditions, over 95% of Cd-loaded hydroxyapatite particles were separated in a very short retention time.