As a part of a research program on the treatment of radioactive process waste waters, sorbent macroflotation was tested to remove Co(II) from dilute aqueous solutions. Activated charcoal was used as the sorbent, and gelatin, cetylpyridinium chloride, dodecylamine or N-dodecylpyridinium chloride (NDPC) as the collector. In addition to the effect of the collector type on the percent removal, the effects of the pH, the charcoal and collector doses, the metal ion concentration, the ionic strength and the use of combinations of NDPC with other reagents have been investigated. At the optimum conditions removals better then 97% could be achieved in the pH range of 7.5–10.0 with NDPC plus a low concentration of a low-molecular-weight polyacrylamide. The results obtained are discussed in terms of hydrolysis of the metal ion and the electric state of both the charcoal and collector.