Abstract: A method for the removal and purification of substantially all of the fluoride ions contained in a solution containing greater than 10 parts per million (ppm) fluoride ion, a mixture of other anions, silicon in the form of a fluorosilicic acid, silicic acid, silicates, or silicon tetrafluoride, and optionally also containing complex metal fluorides, to produce an ultrapure hydrofluoric acid, comprising the steps of (a) adjusting the pH of the solution to an alkaline pH to hydrolyze the fluorosilicic acid and any complex metal fluorides; (b) removing the fluoride ions and other anions from the solution by passing the solution through an ion exchange resin, where the ion exchange resin is adapted to adsorb substantially all of the fluoride passed over the ion exchange resin; (c) displacing the fluoride ions and other anions bound to the ion exchange resin, thereby forming a mixture of anions in an effluent emanating from resin; (d) optionally concentrating the effluent at a high pH and then lowering the pH; and