Fluorination modifies the electronic properties of graphene, and thus it can be used to provide material with on-demand properties. However, the thermal stability of fluorinated graphene is crucial for any application in electronic devices. Herein, X-ray photoelectron spectroscopy (XPS), temperature-programmed desorption (TPD), and Raman spectroscopy were used to address the impact of the thermal treatment on fluorinated graphene. The annealing, at up to 700 K, caused gradual loss of fluorine and carbon, as was demonstrated by XPS. This loss was associated with broad desorption of CO and HF species, as monitored by TPD. The minor single desorption peak of CF species at 670 K is suggested to rationalize defect formation in the fluorinated graphene layer during the heating. However, fluorine removal from graphene was not complete, as some fraction of strongly bonded fluorine can persist despite heating to 1000 K. The role of intercalated H2 O and OH species in the defluorination process is emphasised.