Optimization of the freeze-drying cycle: adaptation of the pressure rise analysis model to non-instantaneous isolation valves

Abstract

The principal aim of this study is to extend to a pilot freeze-dryer equipped with a non-instantaneous isolation valve the previously presented pressure rise analysis (PRA) model for monitoring the product temperature and the resistance to mass transfer of the dried layer during primary drying. This method, derived from the original MTM method previously published, consists of interrupting rapidly (a few seconds) the water vapour flow from the sublimation chamber to the condenser and analysing the resulting dynamics of the total chamber pressure increase. The valve effect on the pressure rise profile observed during the isolation valve closing period was corrected by introducing in the initial PRA model a valve characteristic function factor which turned out to be independent of the operating conditions. This new extended PRA model was validated by implementing successively the two types of valves and by analysing the pressure rise kinetics data with the corresponding PRA models in the same operating conditions. The coherence and consistency shown on the identified parameter values (sublimation front temperature, dried layer mass transfer resistance) allowed validation of this extended PRA model with a non-instantaneous isolation valve. These results confirm that the PRA method, with or without an instantaneous isolation valve, is appropriate for on-line monitoring of product characteristics during freeze-drying. The advantages of PRA are that the method is rapid, non-invasive, and global. Consequently, PRA might become a powerful and promising tool not only for the control of pilot freeze-dryers but also for industrial freeze-dryers equipped with external condensers.