, or flibe, is the primary candidate coolant for the fluoride-salt-cooled high-temperature nuclear reactor (FHR). Kilogram quantities of pure flibe are required for repeatable corrosion tests of modern reactor materials. This paper details fluoride salt purification by the hydrofluorination–hydrogen process, which was used to regenerate 57.4 kg of flibe originating from the secondary loop of the molten salt reactor experiment (MSRE) at Oak Ridge National Laboratory (ORNL). Additionally, it expounds upon necessary handling precautions required to produce high-quality flibe and includes technological advancements which ease the purification and analysis process. Flibe batches produced at the University of Wisconsin are the largest since the MSRE program, enabling new corrosion, radiation, and thermal hydraulic testing around the United States.