An experimental study of ethanol dehydration with cyclohexane as the entrainer has been carried out in order to verify the existence of multiple steady states in heterogeneous azeotropic distillation. As a basis, the bifurcation diagram for the ethanol product purity is determined from thermodynamic considerations using the distillate now rate as the bifurcation parameter. The predicted multiple steady states are then verified by rigorous simulation and by experiments on a laboratory tray column with a decanter. The hysteresis behavior due to multiple steady states is also verified in a dynamic experiment.