A method of separating 3,3,3-trifluoropropyne (TFPY) as an impurity from a first composition which includes hydrogen fluoride (HF), at least one primary compound selected from the group consisting of 2-chloro-3,3,3-trifluoropropene (1233xf), 2-chloro-1,1,1,2-tetrafluoropropane (HCFC-244bb), 2,3,3,3-tetrafluoropropene (HFO-1234yf), 1,1,1,2,3-pentafluoropropane (HFC-245eb), 1,3,3,3-tetrafluoropropene (HFO-1234ze), and 1,1,1,3,3-pentafluoropropane (HFC-245fa), and 3,3,3-trifluoropropyne (TFPY) as an impurity, comprising the steps of:
- subjecting the first composition to conditions effective to form a second, binary azeotrope or azeotrope-like composition consisting essentially of from about 71.5 wt. % to about 98.8 wt. % 3,3,3-trifluoropropyne (TFPY) and from about 1.2 wt. % to about 28.5 wt. % hydrogen fluoride (HF) at a boiling point between −10.0° C. and 25.0° C. at a pressure of between 61 psia and 166 psia, wherein the azeotrope-like composition is a composition which behaves substantially as an azeotrope composition;
- and
- separating the second, binary azeotrope or azeotrope-like composition consisting essentially of TFPY and HF by distillation from the first composition including the at least one primary compound, wherein the at least one primary compound remains in the first composition.