The dispersed phase holdup and drop size in solvent extraction columns vary along the column height and this affects the mass transfer coefficient and interfacial area. In this article, mass transfer study was performed experimentally using a 25 mm diameter agitated pulsed column. The axial distribution of mass transfer coefficient was determined by coupling population balance equation and axial dispersion model by taking the longitudinal variation in hydrodynamic performance into consideration. Feasibility of different mass transfer models in predicting concentration profiles was evaluated and a novel correlation based on effective diffusivity was developed. The results showed that both overall and volumetric mass transfer coefficients have significant change along the column height and greatly depends on the agitation speed and pulsation intensity. Increasing dispersed phase velocity also augments the overall mass transfer coefficient. The maximum number of transfer unit was measured to be 10 m−1 at agitation speed of 1000 rpm.