▎ 摘　　要

Nanoscale pores in graphene oxide (GO) control various important functions. The nanoporosity of GO is sensitive to low-temperature heating. Therefore, it is important to carefully process GO and GO-based materials to achieve superior functions. Optimum pretreatment conditions, such as the pre-evacuation temperature and time, are important during gas adsorption in GO to obtain accurate pore structure information. This study demonstrated that the pre-evacuation temperature and time for gas adsorption in GO must be approximately 333-353 K and 4 h, respectively, to avoid the irreversible alteration of nanoporosity. In situ temperature-dependent Fourier-transform infrared spectra and thermogravimetric analysis-mass spectrometry suggested significant structural changes in GO above the pre-evacuation temperature (353 K) through the desorption of "physically adsorbed water" and decomposition of unstable surface functional groups. The nanoporosity of GO significantly changed above the aforementioned pre-evacuation temperature and time. Thus, standard pretreatment is indispensable for understanding the intrinsic interface properties of GO.