In the recycle process of organic solvent, the atmospheric oxygen can cause autoxidation and product peroxide. The time-saving method to evaluate the hazards has been required. In this study, oxygen pressure monitoring experiment was proposed as a new method to evaluate autoxidative resistances of solvents. Some of organic solvents were pressurized by oxygen and kept under isothermal condition. At the same time, the pressure in the vessel tracked. Iodometrical titration, thermal analysis and spectroscopic analysis were performed to measure peroxide concentration, the heat of reaction and chemical bonding change. From the results that THF has larger oxygen consumption rate than CPME, it is considered that autoxidative resistance of THF is lower than that of CPME. This method enables to obtain results in shorter time than other methods. These experimental results were consistent with the previous research with longer test durations [1-2].