A very rapid method of separation of Bi by amalgamation in a fine mercury drop is proposed. The principle of the method consists in finding agents that form much more stable complexes with Hg²⁺ than with Bi³⁺ so that the Hg²⁺/Hg potential becomes lower than that of Bi²⁺/Bi. Iodide was found to be most convenient. In an aqueous solution of 10⁻¹ M concentration in I⁻, traces of bismuth difuse into mercury in about one minute with a yield of more than 99%. Studies on the extraction of the amalgamated bismuth into an aqueous solution are in progress.