To provide a fluorine distillation apparatus for performing fluorine distillation work at the time of fluorine distillation analysis prescribed in JIS K 0102.

The fluorine distillation apparatus is equipped with a steam flask 12 into which water is introduced, a heater 11 for heating the steam flask 12, a distillation flask 14 into which a sample and a reagent are introduced, a heater 13 for heating the distillation flask 14, a solenoid valve 24 provided to a line 23 for sending steam generated in the steam flask 12 to the distillation flask 14, a temperature sensor 18 for detecting the liquid temperation in the steam flask 12, a beaker 17 for storing the distillate from the distillation flask 14 and a level sensor 19 for detecting the liquid level in the beaker 17. When the temperature detected by the temperature sensor 18 reaches a set value, the solenoid valve 24 is opened to send the steam of the steam flask 12 to the distillation flask 14 and the heater 13 is controlled to control the liquid temperature in the distillation flask 14 so as to hold the same to the set value and work is stopped on the basis of the detection value of the level sensor 19.