A Novel Batch Cooling Crystallizer for in Situ Monitoring of Solution Crystallization Using Energy Dispersive X-ray Diffraction
| Autor: | David J. Taylor, Roger Davey, Martin Song, Mike Quayle, Alfie Nield, Nicholas Blagden, Simon M. Clark |
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| Rok vydání: | 2003 |
| Předmět: |
Diffraction
Chemistry Scattering business.industry Synchrotron Radiation Source Analytical chemistry Synchrotron radiation General Chemistry Condensed Matter Physics law.invention Optics law Fluid dynamics General Materials Science Energy-dispersive X-ray diffraction Crystallization business Mass fraction |
| Zdroj: | Crystal Growth & Design. 3:197-201 |
| ISSN: | 1528-7505 1528-7483 |
| DOI: | 10.1021/cg020053n |
| Popis: | 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. |
| Databáze: | OpenAIRE |
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