This paper on the dynamics of multicomponent distillation is based on experimental investigations in a laboratory-scale distillation column. The concentration and temperature profiles are obtained at the steady-state operating point, and the transition behavior is observed by systematically changing the relevant operating variables. The general scope of these experiments is to evaluate and study the concentration and temperature profiles measured along the column height. The developed methodology for sampling at vacuum is explained. The experimental results are compared with theoretical calculations obtained by means of steady-state and dynamic simulation. The influence and the importance of heat losses on the steady-state and dynamic behavior at high temperature levels are investigated and discussed. The aim of these studies is to prove the steady-state and dynamic simulation tool on the basis of the equilibrium stage model. It is found that the simulation results agree closely with those obtained experimentally. This refers to the concentration and temperature profiles as well as to the calculated and the experimentally used reboiler heat input. In order to achieve this good agreement, heat losses along the column height have to be taken into account in the simulation. Consequently, the consideration of heat losses is of great importance for the determination of HETP values in packed columns.