An original procedure has been established for estimating the overall volumetric mass transfer coefficient using the oxygen concentration curves resulting from the usual gassing-in and gassing-out method. This procedure was applied to experimental data obtained in a small scale bubble column using both tap water and a coalescence-inhibiting liquid mixture that represents the coalescence behavior of biological media. It is based on the analysis of the characteristics times of the system, including those of the hydrodynamics of the two phases, the sensor dynamics and the system inertia when the gas composition is modified. A numerical procedure was developed to estimate the characteristic time of the system inertia ti, using the assumption that this inertia is nearly independent of superficial gas velocity UG. The calculations confirmed that the optimized ti value was nearly independent of UG and of the coalescence behavior of the liquid phase. Additionally, the resulting KLaL values for tap water were closer to the correlation of Shah et al. [1982. Design parameters estimations for bubble column reactors. A.I.Ch.E. Journal 28, 353–379] than those of other conventional models. Finally, the original procedure was also reported to reduce significantly the square sum deviation between the predicted and the measured oxygen response curves.