Electrodialysis in an ion-exchange membrane cell was shown to be technically feasible for the concentration of an azeotropic mixture of HF and water. A flowsheet is presented for recovery of anhydrous HF by distillation and electrodialysis of the azeotropic residue. In the electrodialysis step, 2.6 kwhr of energy per pound of anhydrous product was consumed, with electricity at 1¢ per kilowatt-hour, the total operating cost of the electrodialysis equipment alone, including amortization, would be 6¢ per pound of HF.