Abstract: Trivalent thallium values are extractively recovered from aqueous media containing dissolved trivalent and monovalent thallium values by contacting the aqueous medium in the presence of an alkanoic acid, having from 2 to 4 carbon atoms per molecule and having a molecular weight of at least 74 grams per gram-mol of acid, with an inert, organic, non-acidic solvent for the alkanoic acid, said solvent having limited solubility in water, to preferentially extract at least a portion of the dissolved trivalent thallium values into the organic solvent extractant and recovering an extract comprising the organic solvent containing the extracted trivalent thallium values.