An amalgam exchange technique has been used for the rapid radiochemical separation of lead. A number of variables which affect the exchange were studied and a lead yield of 88.5 %was obtained. At room temperature the procedure requires about 13 min, whereas at 40 degrees it can be completed in about 9 min. Radioactive tracers of 16 different elements were used to check the selectivity of this procedure, which has also been applied for the separation of (212)Pb from thorium nitrate solution.