Diethyl ether is a common industrial reagent and medical anesthetic. It is necessary to carry out real-time monitoring of this molecule due to its harmful effects on human health. In this paper, a highly sensitive diethyl ether SnO 2 gas-sensing material has been prepared by a sol-gel method. The gas sensitivity was tested by a home-made gas-sensing equipment. The surface adsorption and reaction processes between the SnO 2 gas-sensing film and the diethyl ether have been studied by in situ diffuse-reflectance Fourier-transform infrared spectroscopy (DRFT-IR) at different temperatures. The results show that the SnO 2 gas-sensing material has high sensitivity to diethyl ether, and the lowest detection limit can reach 1 ppm. Furthermore, ethyl (CH 3 CH 2 •), oxoethyl (CH 3 CH 2 O•), ethanol (CH 3 CH 2 OH), formaldehyde (HCHO), acetaldehyde (CH 3 CHO), ethylene (C 2 H 4 ), H 2 O and CO 2 surface species are formed during diethyl ether adsorption at different temperatures. A possible mechanism of the reaction process is discussed.