A novel approach using a semipermeable Teflon AF-2400 tube-in-tube membrane contactor was developed for the measurement of gas solubility in organic solvents. This membrane ensures gas saturation of liquids in continuous flow at a specific pressure and temperature. After liquid decompression, the amount of gas outgassed was measured with a bubble meter and used for solubility calculation. The proposed method was applied to the measurement of oxygen solubility in toluene and benzyl alcohol. Validation experiments were initially performed by comparing the obtained oxygen solubility in toluene with literature data. With higher temperature, the solubility of oxygen in benzyl alcohol was found to increase, indicating that the oxygen-dissolving process is endothermic. Finally, an empirical correlation of Henry's law constant as a function of temperature was determined.