Abstract: Acidic impurity, such as HCl, is removed from chlorofluoromethanes of the formula CHCl.sub.n F.sub.3-n, where n is 1 or 2, by scrubbing the contaminated fluorocarbon with an aqueous solution made from a mixture of trisodium phosphate and sodium hydroxide. Use of this solution as scrubbing medium allows purification of the contaminated fluorocarbon without appreciable decomposition and also without generation of a significant quantity of environmentally objectionable waste stream of high phosphate content. The presence of NaOH in the scrubbing medium provides in situ regeneration of mono and disodium phosphates to trisodium phosphate.