PURPOSE: To separate and refine Rh with high purity and high yield from an aq. soln. containing Rh and at least one element selected from Pd, Pt, Au, Bi, Te, Pb and Cu.

CONSTITUTION: After the aq. soln. of Rh containing other impurity metals is adjusted to have radical hydrochloric acid concn. to ≥1mol/l, this soln. is then made to flow through a resin tower packed with a chelate resin to adsorb noble metals. Rh, Pd, Pt, Au, Bi, and Pb in the soln. are adsorbed by the chelate resin, while the soln. is continuously made to flow so that most of the Pd, Pt, Au, and Bi adsorbed by the resin are replaced by Rh to increase the proportion of Rh to the adsorbed metals to the resin. Then a sulfuric acid soln. of ≥1.0mol/l concn. at >25°C is made to flow through the resin tower to dissolve and elute Rh from the resin tower. By this method for refining, the used chelate resin can be again used, and this method can be applied for a Rh-contg. soln. produced by a treating process of slime in the electrolysis of silver or the like.