Abstract: The invention provides a method of regenerating dithiophosphorus extractants such as dithiophosphoric acids, dithiophosphonic acids and dithiophosphinic acids from their sulfur-sulfur bonded oxidation products contained in an organic solution. The process generates active hydrogen for regenerating the spent dithiophosphorus extractants. Advantageously, this active hydrogen originates either from introducing a reactive metal into a liquid mixture containing the organic solution and an acidic aqueous solution to form nascent hydrogen or from using hydrogen gas in the presence of a catalyst in the organic solution. The active hydrogen generated in the process breaks the sulfur-sulfur bonds of the dithiophosphorus molecules to form the corresponding dithiophosphorus acids.