In this contribution we present two cases of phase transitions,
in which the ability to control the reproducible formation of
the desired physical form requires a control of crystallization
parameters and a deep understanding of the phase diagram.
This paper presents and compares crystallization experiments
of an active pharmaceutical ingredient and a biological molecule
in the presence of a liquid−liquid phase separation monitored
by in situ video. The advantage of this setup is that it requires
a small quantity of these products to study the influence of the
physicochemical parameters on crystallization. Crystallization
mechanisms and kinetics are different depending on the starting
position in the phase diagram and on the temperature reduction,
when crystallization is temperature-induced. Liquid−liquid
phase separation changes the medium and the conditions of
crystallization, hinders both primary and secondary nucleation
for several hours, and consequently affects the process. For
great temperature reduction and, inside the spinodal zone,
namely high supersaturation (> 15), crystals nucleate inside
the droplets. Therefore, we take advantage of the formation of
droplets to propose a new approach to spherical crystallization.
The final products are quasi-spherical monodisperse agglomerated particles of about 500 μm made up of small crystals of a
few micrometers.
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