Abstract: A process for the separation of hydrogen fluoride (HF) and of difluoromethane (F32) by fractional distillation and/or condensation, in at least one stage, including in at least one stage obtaining a stream whose HF and F32 contents correspond.

Abstract: The invention relates to the separation of hydrogen fluoride (HF) from its mixtures with 1,1,1-trifluoro-2-chloroethane (F133a).By settling of the mixture of HF and F133a in the presence of trichloroethylene at a temperature below 0.degree. C., a lower organic phase which is poor in HF and an upper phase which is rich in HF are obtained. The latter can be directly recycled to the fluorination reactor or subjected to a distillation in order to separate, at the head, the HF/F133a azeotrope which is returned to the settler, and to recover, at the foot, practically pure HF. By distillation of the lower phase, the HF/F133a azeotrope which is returned to the settler is separated at the head and a mixture of F133a and trichloroethylene is recovered at the foot. The latter mixture is subjected to a distillation which makes it possible to separate, at the head, pure F133a from trichloroethylene at the foot.