The process of fractional distillation has been performed for many years but has only within the past half century become a true science. However, because of the many variables involved and the uncertainty of their effect upon fractionating column efficiency, the design of columns has long been a major engineering problem. Plate and column efficiencies, as given in the literature, vary widely and it was thought possible that the inconsistencies of the results reported might be due to poor equilibrium within the column, caused in part by faulty sampling. In order to determine the operating characteristics of a fifteen plate bubble-cap column (8-3/8" I.D., one 3-7/8" bubble-cap per plate, and plate spacing of 5-7/8"), the effects of the operating variables, and the distillation characteristics of two different types of binary mixtures, the column assembly was redesigned for continuous distillation and provisions made for the introduction of feed at its boiling point to any one of the bottom eight plates. The binary — mixtures distilled were isopropyl alcohol — water (distillation rates 157 - 376 gms./min., feed concentrations 3.1 - 10.8 mol per cent isopropyl alcohol, reflux ratio 3:1, and feed rate of 330 gms./min.), and toluene - ethylene dichloride (distillation rates 203 and 196 gms./min., feed concentrations 41.4 and 39.7 mol percent ethylene dichloride, reflux ratio 4:1, and feed rate of 138 gms./min.) In order to reduce the possibility of disturbances within the column by removal of large plate samples, the refractive index method of analysis was used which required maximum samples of only 4 ml. Results of the experiments made indicated that the assumption of the McCabe - Thiele operating line is probably incorrect. In the case of the isopropyl alcohol — water fractionation, a considerable divergence (largest between 10 and 40 mol per cent isopropyl alcohol) between the McCabe - Thiele and the actual operating line was noted, the actual operating line being a curve approximately the shape of the equilibrium curve. Murphree Plate Efficiencies for the mixture varied from 0 to 100 per cent, depending primarily on the relative deviations of the two operating lines from the equilibrium curve. The McCabe - Thiele operating line for the system toluene — ethylene dichloride closely approximated the actual operating line. Murphree Plate Efficiencies varied from 44.5 to 121 percent, but the individual plate efficiencies were more consistent with the average efficiency. The rate of distillation over the range of 157 to 376 gms./min. and feed concentration over the range of 3.1 to 10.8 mol percent isopropyl alc1ohol, at a reflux ratio of 3:1 had negligible effect on product purity which ranged from approximately 62 to 67 mol per cent isopropyl alcohol. / Master of Science