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Extraction of rhodium(III) from hydrochloric acid solutions with bisacylated triethylenetetramine dihydrochloride has been studied. The optimal extraction conditions have been elaborated. At the phase contact time of 5 min rhodium(III) is extracted via the interphase anionic exchange mechanism. Concentration constants of extraction have been calculated, and thermodynamic parameters of extraction have been estimated. The extracted ion associate has been isolated and characterized by means of electronic, IR, and 13 C NMR spectroscopy.