A systematic procedure is presented to assist the calibration of tray distillation column models over plant data. Practical suggestions are provided that contribute to reduce the time needed to check the closure of the experimental material and energy balances. Typical modeling inaccuracies that may have a strong impact in the model performance are highlighted. A set of "cold" and "hot" test runs is suggested to minimize the time that is needed to reliably tune the model in view of using it for control system design and testing. The procedure is discussed with reference to the experimental results obtained in a pilot-plant column.