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A series of graphite oxide samples were prepared using the modified Hummers method. Flake graphite was used as the raw material and the reaction temperature of the aqueous solution was changed (0 °C, 30 °C, 50 °C, 60 °C, 70 °C, 80 °C, and 100 °C). X-ray diffraction, Fourier-transform infrared spectroscopy, Raman spectral analysis, X-ray photoelectron spectroscopy, and contact angle tests were performed to characterize the structure, chemical bonding, type, and content of oxygen-containing functional groups of the graphite oxide samples. The results showed that the type and content of each oxygen-containing functional group could be controlled by changing the reaction temperature with the addition of water. As the temperature of the system increased, the degree of oxidation of the graphite oxide samples first increased and then decreased. Too high a temperature (100 °C) of the system led to the formation of epoxy groups by the decomposition of some hydroxyl groups in the samples, causing the reduction of oxygen-containing functional groups between the graphite layers, poor hydrophilic properties, and low moisture content. When the system temperature was 50 °C, the interlayer spacing of the graphite oxide samples was at its highest, the graphite was completely oxidized (C/O = 1.85), and the oxygen-containing functional groups were mainly composed of hydroxyl groups (accounting for approximately 28.88% of the total oxygen-containing functional groups). The high content of hydroxyl and carboxyl groups had good hydrophilic ability and showed the highest moisture content. The sample at 50 °C had better sensitivity to ammonia because of its high hydroxyl group and carboxyl group content, with the sample showing an excellent profile when the ammonia concentration was 20–60 ppm.

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