A rapid, selective, and highly sensitive froth flotation method for the separation and enrichment of ultra trace amounts of bismuth is developed. The bismuth-Arsenazo III complex is concentrated from 1000mL of aqueous solution into the scum in the presence of cetyltrimethylammonium bromide (CTAB) as a cationic surfactant. The proposed procedure of pre-concentration is applied prior to the determination of bismuth using inductively coupled plasma-atomic emission spectrometry (ICP-AES). Effects of Arsenazo III concentration, pH, CTAB concentration, and foreign ions have been studied. The proposed method possesses a pre-concentration factor of 500 and a detection limit of 0.28ngmL-1.