Abstract: A process is described for the recovery of uranium values from phosphoric acid utilizing an alkyl pyrophosphoric acid (APPA) primary extractant. After extracting the uranium from the phosphoric acid, the APPA extractant is deactivated by heating and the uranium values stripped into a phosphoric acid strip solution containing ferric ion as a salting agent. The uranium values may then be re-extracted directly from this stripping solution without adjustment of its concentration into a dialkyl phosphoric acid trialkyl phosphine oxide synergistic extractant from which a relatively pure yellow cake is precipitated. A new procedure for preparing the requisite APPA primary extractants is also disclosed.