Crystallization from Solutions Containing Multiple Conformers. 2. Experimental Study and Model Validation

• Published in: Crystal growth & design Vol. 12; no. 11; pp. 5188 - 5196
• Main Authors: Derdour, L, Sivakumar, C, Skliar, D, Pack, S. K, Lai, C. J, Vernille, J. P, Kiang, S
• Format: Journal Article
• Language: English
• Published: Washington,DC American Chemical Society 07.11.2012
• Subjects: Condensed matter: structure, mechanical and thermal properties; Cross-disciplinary physics: materials science; rheology; Crystalline state (including molecular motions in solids); Crystallographic aspects of phase transformations; pressure effects; Equations of state, phase equilibria, and phase transitions; Exact sciences and technology; General studies of phase transitions; Materials science; Methods of crystal growth; physics of crystal growth; Nucleation; Physics; Structure of solids and liquids; crystallography; Theory and models of crystal growth; physics of crystal growth, crystal morphology and orientation; Crystal growth; Temperature dependence; Fourier transform spectroscopy; Nucleation; Solid solutions; Growth rate; Solution crystallization; Attenuated total reflection; Experimental study
• DOI: 10.1021/cg300975s
• ISSN: 1528-7483

In this Article, the validity of a model derived for crystal growth rates and supersaturation for solids crystallized from solutions of materials containing multiple conformers is evaluated. A simple and straightforward method for determining crystal growth rates using FBRM and FTIR/ATR is utilized, which leads to a large amount of growth rate data from a single experiment. Supersaturation and crystal growth rate obtained experimentally were in good agreement with model predictions. In particular, data indicated that for the system at hand, crystal growth rate is inversely proportional to crystals size. Further, the solute integration coefficient determined from supersaturation measurements can be slightly overestimated due to surface nucleation and/or agglomeration that can result from supersaturation spikes during antisolvent addition. Last, crystal growth data obtained at different temperatures indicated that slow growth rate observed at low temperatures is likely to be due in part to surface poisoning by the wrong conformer.