The dynamics and control of a hydrogen isotope distillation column are discussed. The proportionalintegral (PI) controller parameter setting method previously reported by one of the authors is further investigated and extended by applying the method to two different experimental control modes. The method accounts for the nonlinearity of the column to some extent and allows us to predict the unstable region or the region of the proportional-only control behavior. The method can also be applied to the cases where the measurement of the controlled variable is accompanied by a significant time lag. The mean delay time depends greatly on the controlled variable and manipulated variable chosen and the upset condition assumed, varying by over two orders of magnitude. The PI control presents great stability, and a rather long time lag is permissible in the measurement of the controlled variable if the flow rate of the top product is chosen for the manipulated variable. On the other hand, if the reflux ratio is manipulated for controlling the lightest key element in the bottom product, the great stability is no longer present and the time lag must be adequately short. Once several response curves of the controlled variable are calculated for different magnitudes of the manipulated variable upset, the parameter setting method proposed makes it possible to study how long a time lag is allowable in the measurement of the controlled variable.