Molecular distillation was studied for the separation of tocopherols from soya sludge, both experimentally and by simulation, under different operating conditions, with good agreement. Evaporator temperatures varied from 100 degrees C to 160 degrees C and feed flow rates ranged from 0.1 to 0.8 kg/h. The process pressure was maintained at 10(-6) bar, the feed temperature at 50 degrees C, the condenser temperature at 60 degrees C, and the stirring at 350 rpm. For each process condition, samples of both streams (distillate and residue) were collected and stored at -18 degrees C before tocopherols analyses. Owing to the differences between molecular weights and vapor pressures of free fatty acids and tocopherols, tocopherols preferentially remained in the residue at evaporator temperatures of 100 degrees C and 120 degrees C, whereas for higher temperatures (140 degrees C and 160 degrees C) and lower feed flow rate, tocopherols tended to migrate to the distillate stream.