화학공학소재연구정보센터
Journal of Crystal Growth, Vol.311, No.14, 3640-3650, 2009
Determination of metastable zone width for combined anti-solvent/cooling crystallization
The metastable zone width (MSZW), induction time and primary nucleation kinetics have been measured and estimated for simultaneous anti-solvent and cooling crystallization of paracetamol in isopropanol/water solution. ATR-FTIR spectroscopy and laser back-scattering are used to measure the solute concentration and primary nucleation event, respectively. Response surface analysis was applied to find the contribution of the crystallization mechanism on the MSZW and obtain a statistical model for quick estimation of the MSZW. Two theoretical approaches for the estimation of nucleation rate kinetic parameters from experimental data are presented. The methods are obtained by modifying the classical Nyvlt's correlation for simultaneous cooling/anti-solvent crystallizations. The nucleation order n for primary nucleation was deduced from the slope of a linear plot of log(MSZW) vs. log(cooling and anti-solvent rates). The induction time was also estimated by changing the classical methods for combined cooling and anti-solvent crystallization. (C) 2009 Elsevier B.V. All rights reserved.