Crystallization of glycine with ultrasound.

Sonocrystallization has proved to be an efficient tool to influence the external appearance and structure of a crystalline product obtained by various crystallization methods. The present work focuses on high intensity sonocrystallization of glycine by varying amplitude of ultrasound with an ultrasound frequency of 20kHz at two temperature ranges 40-50 and 20-30 degrees C in a jacketed 250-ml cooling crystallizer equipped with a stirrer. The polymorph composition of the obtained crystals was analyzed with a temperature variable X-ray powder diffractometer (XRPD). XRPD results showed that, besides the operating temperature, the glycine polymorphism was affected also by insonation. This was especially the case at the lower temperature range. Furthermore, based on the heat balance within the crystallizer, an increase in required cooling capacity was presented as a function of increasing ultrasound power. This study also showed, the higher the ultrasound amplitude the smaller the crystals obtained.

[1]  San Kiang,et al.  Crystallization Process Development of an Active Pharmaceutical Ingredient and Particle Engineering via the Use of Ultrasonics and Temperature Cycling , 2003 .

[2]  B. A. Garetz,et al.  Nonphotochemical, laser-induced nucleation of supersaturated aqueous glycine produces unexpected γ-polymorph , 2001 .

[3]  P. W. Cains,et al.  Use the power of sonocrystallization for improved properties , 2001 .

[4]  N. Kubota,et al.  Reliable and selective crystallization of the metastable α-form glycine by seeding , 2004 .

[5]  Allan S. Myerson,et al.  Impact of Ultrasonic Energy on the Crystallization of Dextrose Monohydrate , 2003 .

[6]  E. Ferrari,et al.  Crystallization in Polymorphic Systems: The Solution-Mediated Transformation of β to α Glycine , 2003 .

[7]  Gordon J. T. Tiddy,et al.  The Crystallization of Glycine Polymorphs from Emulsions, Microemulsions, and Lamellar Phases. , 2002 .

[8]  J. Rantanen,et al.  Characterization of polymorphic solid-state changes using variable temperature X-ray powder diffraction. , 2005, Journal of pharmaceutical and biomedical analysis.

[9]  Zhichao Guo,et al.  Rapid sonocrystallization in the salting-out process , 2003 .

[10]  James M. B. Evans,et al.  Determination of Solubility of Polymorphs Using Differential Scanning Calorimetry , 2003 .

[11]  R. Chivers,et al.  The microscopic visualisation of the sonocrystallisation of ice using a novel ultrasonic cold stage. , 2004, Ultrasonics sonochemistry.

[12]  Åke C. Rasmuson,et al.  Influence of Ultrasound on the Nucleation of Polymorphs of p-Aminobenzoic Acid , 2005 .

[13]  Guangyu Yang,et al.  The CFD simulation of temperature control in a batch mixing tank , 2003 .

[14]  Joel Bernstein,et al.  Polymorphism in Molecular Crystals , 2002 .

[15]  Olivier Louisnard,et al.  Effect of ultrasound on the induction time and the metastable zone widths of potassium sulphate , 2002 .