Abstract: A process for the recovery of rhodium and iodine values and the separation of rhodium from corrosion metal salts in the manufacture of acetic acid by the carbonylation of methanol wherein the reaction mixture contains from about none to about 20 wt % of water, from about 2 to about 20 wt % of alkali metal or alkaline earth metal iodide, methanol, acetic acid, methyl iodide, and carbon monoxide which comprises: (1) removing at least a portion of the reaction solution from the reactor, (2) removing at least a portion of the product acetic acid from the portion in (1) by distillation, (3) adding an excess of methyl acetate to the product depleted material in (2) and heating the resultant mixture to a sufficiently high temperature to convert the methyl acetate to methyl iodide (4) removing the resulting methyl iodide by distillation, (5) continuing to heat the resulting mixture at a temperature and time sufficient to precipitate the rhodium as rhodium iodide, and (6) separating the rhodium iodide and returning it