Abstract: The maximum-profit problem in the operation of a batch distillation column separating a binary mixture is studied. From the objective function made in this paper, such problem can be transformed under special condition, into either maximum-distillate or minimum-time problem. Reflux ratio is chosen as control variable. Digital method is worked out by using optimal control theory to find the condition of optimal operation. In deriving present mathematic model, the liquid hold-up in plates and in condenser as well as the plate efficiency are taken into account. The proposed optimal operation is compared theoretically with the conventional constant reflux ratio and constant overhead composition policies and the results show that the proposed optimal operation can lead to/nuch higher profits. To demonstrate the practical usefulness of the proposed optimal policy, experimental work is carried out in a 4 sieve trays 0.17M diameter batch distillation column with ethanolwater system. Agreement is found between the experimental data and the computed results from present model.