A novel batch cooling crystallizer for in situ monitoring of solution crystallization using energy dispersive X-ray diffraction

Blagden, Nicholas and Davey, R. and Song, M. and Quayle, M. and Clark, S. and Taylor, D. and Nield, A. (2003) A novel batch cooling crystallizer for in situ monitoring of solution crystallization using energy dispersive X-ray diffraction. Crystal Growth and Design, 3 (2). pp. 197-201. ISSN 1528-7483

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Item Type:Article
Item Status:Live Archive

Abstract

In situ X-ray diffraction monitoring of crystallization from solution is often hampered by a combination of the rather low levels of crystallized solid (typically 5 to 20 wt ) and the large background scattering that arises from the solution phase. In this work, we have attempted to overcome these limitations, first, by using high intensity dispersive X-rays available at the Synchrotron Radiation Source, Daresbury Laboratory, UK, and second by designing a novel batch classifying crystallizer. This crystallizer was designed to maximize the weight fraction of solid presented to the probe beam. In this configuration, solution crystallizations generating between 2 and 30 wt of solids were monitored successfully. Three preliminary studies describe the application of this equipment to the simple real time monitoring of a crystallization event, the interconversion of two polymorphic crystalline forms, and the orientation of crystals in the fluid flow of the crystallizer.

Keywords:article, chemical modification, crystallization, energy, fluid flow, hydrodynamics, laboratory, monitoring, radiation scattering, solid, synchrotron, United Kingdom, X ray diffraction
Subjects:B Subjects allied to Medicine > B230 Pharmacy
F Physical Sciences > F100 Chemistry
Divisions:College of Science > School of Pharmacy
ID Code:8772
Deposited On:04 Apr 2013 11:25

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