Evidence of transient amorphization during the polymorphic transformation of sorbitol induced by milling.

In this paper, we show that the polymorphic transformation γ → α of sorbitol upon milling involves a transient amorphization of the material. This could be done by comilling sorbitol with a high Tg amorphous material (Hydrochlorothiazide, Tg = 115 °C) to stabilize any transient amorphous fractions of sorbitol through the formation of a molecular alloy. The results indicate that for large sorbitol concentration (50%), the comilling leads to a heterogeneous mixture made of sorbitol crystallites in the form α embedded into an amorphous molecular alloy sorbitol / HCT. Interestingly, the kinetic investigation of this transformation reveals that these two components are not produced simultaneously. On the contrary, they are produced one after the other, during two distinct consecutive stages. The first stage concerns the formation of the amorphous alloy while the second one concerns the polymorphic transformation γ → α of the fraction of crystalline sorbitol not involved in the alloy. These results clearly indicate that the polymorphic transformation of sorbitol upon milling results from the recrystallization of a transient amorphous state generated by the mechanical shocks. The investigations were mainly performed by calorimetry and powder X-ray diffraction.