Reduction of graphene oxide is primarily important because different reduction methods may result in graphene with totally different properties. For systematically exploring the reduction of graphene oxide, studies of the temperature-dependent electrical properties of graphene oxide (GO) are urgently required. In this work, for the first time, broadband dielectric spectroscopy was used to carry out an in situ investigation on the transition of the electrical properties of GO paper from -40 to 150 °C. The results clearly reveal a very interesting four-stage transition of electrical properties of GO paper with increasing temperature: insulator below 10 °C (stage 1), semiconductor at between 10 and 90 °C (stage 2), insulator at between 90 and 100 °C (stage 3), and semiconductor again at above 100 °C (stage 4). Subsequently, the transition mechanism was discussed in combination with detailed dielectric properties, microstructure and thermogravimetric analyses. It is suggested that the temperature-dependent transition of electronic properties of GO is closely associated with the ion mobility, water molecules removal and the reduction of GO in the GO paper. Most importantly, the present work clearly demonstrates the reduction of GO paper starts at above 100 °C.