In Situ Monitoring of Cocrystallization Processes - Complementary Use of Sensing Technologies

E. Gagniere (1) , F. Puel (1) , D. Mangin (1) , J.-P. Valour (1) , A. Rivoire (1) , J.-M. Galvan (2) , O. Monnier (3) , J.-P. Klein (1)

1 LAGEP - Laboratoire d'automatique et de génie des procédés
2 INL - CSH - INL - Conception de Systèmes Hétérogènes
3 Sanofi-Aventis R&D

Two in situ process analytical technologies were used to investigate a cocrystallization process: a focused beam reflectance measurement probe and a video probe. The cocrystallizations were conducted batch-wise in a stirred thermostatted vessel with carbamazepine and nicotinamide. The experiments were started in three domains of the phase solubility diagram. When carbamazepine crystals were also formed, a solution mediated phase transition from carbamazepine crystals towards cocrystals was initiated by the addition of the cocrystallizing agent (nicotinamide crystals). As the carbamazepine crystals and the carbamazepine/nicotinamide cocrystals exhibit prism-like and needle-like habits, respectively, it was possible to discriminate between them with the two sensors. The mechanisms involved in the solution mediated phase transition were investigated.

Mots clés: Organic materials; Cocrystals; Phase diagram; Sensors

Domaines: Génie des procédés

E. Gagniere, F. Puel, D. Mangin, J.-P. Valour, A. Rivoire, et al.. In Situ Monitoring of Cocrystallization Processes - Complementary Use of Sensing Technologies. Chemical Engineering and Technology, 2012, 35 (SI) (6), pp.1039-1044. ⟨10.1002/ceat.201100711⟩. ⟨hal-01271824⟩