The multivessel batch distillation column, as well as conventional batch distillation, can be operated in a closed (total reflux) mode where the products are collected in vessels along the column. A previously proposed and simulated feedback control strategy for the closed operation is to indirectly adjust the vessel holdups by using the reflux flow out of the vessel to control the termperature at some location in the column section below. The feasibility of this scheme is demonstrated here experimentally on a laboratory-scale multivessel column. The experimental column consists of a reboiler, two intermediate vessels, and an accumulator, where a mixture of methanol–ethanol–propanol–butanol is separated into almost pure components. The first published experimental work on the closed operation of batch distillation is presented, as well as its results on the operation of a multivessel column.