The mass transfer characteristics of a pulsed disc and doughnut column with a 0.04 m internal diameter and 4.24 m active column length are investigated in order to evaluate its contacting efficiency for caprolactam extraction with toluene. Pilot plant experiments for both the forward and back-extraction process were performed in order to determine the concentration profile along the column length in both the extract and raffinate phase as a function of the operating conditions. The experimental conditions covered the industrial operating range. Furthermore the dispersed phase hold-up, average droplet diameter and operating regime were determined and compared with the results obtained for the equilibrium situation, as discussed in Part II. In the forward extraction process a significant influence of operating conditions was observed, where an increase in the flux decreased the separation efficiency, but an increase in pulsation intensity, temperature, or the addition of ammonium sulphate increased the separation efficiency. In the back-extraction all concentration profiles were comparable and all caprolactam was extracted after a column length of L/m=2. Compared to the equilibrium situation the drop diameter and pulsation intensity required for the transition of the mixer-settler to the dispersion operating regime were found to increase under mass transfer conditions, while the hold-up decreased. HETS values were determined for both the forward and back-extraction. For the latter HETS=0.28 to 0.41, whereas in the forward extraction HETS=0.32 to 0.67. The concentration profiles were described with the backflow model, using a constant backflow parameter for the continuous phase and a constant overall mass transfer coefficient. The interfacial area was correlated using drop diameter and hold-up expressions derived for the equilibrium situation, taking into account the relative effect of mass transfer. Using these expressions the measured data could be correlated and described well.