In the present work, hydrodynamics and mass transfer performance of the asymmetric rotating impeller column (ARIC) of different scales, that is, ARIC 1 (I.D. = 0.1 m), ARIC 2 (I.D. = 0.22 m), and ARIC 3 (I.D. = 0.3 m), have been investigated. The liquid−liquid system used in the present study is phosphoric acid containing metal ions and the organo-phosphorous solvent. The effect of different operating conditions on regime transition in ARIC of different scales has been analyzed. Correlations have been developed for the prediction of holdup and drop size in the ARIC of different scales. The average absolute relative error values in the prediction of holdup and drop size using these correlations are 10 and 9%, respectively. An increase in the height of transfer unit is observed with an increase in throughput and column diameter. The results indicate that adequate design and scale-up of extraction columns can be carried out based on geometric similarity.