Mercury(II) and cadmium(II) were separated from aqueous systems by a number of batch-type precipitate flotation and adsorbing colloid flotation techniques. HgS, CdS, and Cd(OH)2were removed by precipitate flotation; Fe(OH)3, Al(OH)3, FeS, and CuS were used as adsorbing colloids. Sodium lauryl sulfate and hexadecyltrimethylammonium bromide (HTA) were used as collectors. Dependence of separation efficiency on pH and ionic strength was investigated. Floc foam flotation of both metals with CuS and HTA was found to be quite effective, resulting in residual Hg(II) levels as low as 5 ppb and residual Cd(II) levels as low as 20 ppb. Floc foam flotation of Cd(II) with FeS and HTA yielded residual Cd(II) levels as low as 10 ppb.