Disclosed herein is a process for the separation and recovery of Rhodium values from aqueous mineral acid solutions also containing Iridium and/or Ruthenium which comprises contacting the metal bearing aqueous solution with a water immiscible organic solvent containing an organically substituted quaternary amine salt to extract Iridium and Ruthenium into the solvent phase leaving Rhodium in the aqueous raffinate. The loaded organic phase is stripped of Iridium and Ruthenium in two sequential steps by contacting it first with an alkaline solution then redissolving the resulting precipitate in an acidified reducing solution.