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The article focuses on a laboratory course in unit operations and process control for chemical engineering students at the Instituto Superior de Engenharia de Coimbra in Portugal which covers topics such as distillation and the control of variables often found in industrial units. The course provides students with experience in operating and controlling complex units. For the study of distillation, the students are asked to validate the steady-state behavior of a laboratory unit used for segregating an azeotropic mixture of aniline and water.