Many techniques for separation and recovery of Rh(III) from aqueous solution have been studied. In this paper, Precipitation characteristics of rhodium [Rh(III)] from a simulated radwaste solution by the various reducing agents such as hydrazine and titanium chloride was investigated. When the nitric acid concentration at 2 (Rh, Ru) components system was 0,5 M, Rh over 98.2% was precipitated by adding the 0,1 M titanium chloride. However, Ru was co-precipitated with Rh(III).