Application of in-process X-ray powder diffraction for the identification of polymorphic forms during batch crystallization reactions

Robert B. Hammond, Xiaojun Lai, Kevin J. Roberts, Alistair Thomas, Graeme White

Research output: Contribution to journalArticle

11 Citations (Scopus)

Abstract

An on-line X-ray diffraction system capable of monitoring and identifying the polymorphic form of organic materials crystallized during batch crystallization processes is described. The overall system comprises a conventional X-ray source, monochromator, collimator, slits, curved position sensitive detector, and a flow-through analysis cell together with the electronics and the data acquisition software. The cell enables X-ray diffraction data to be recorded from crystals suspended within a slurry pumped to and from a batch crystallizer via an external temperature controlled sampling loop. The system is validated via benchmark crystallization studies of urea, L-glutamic acid and monosodium glutamate. The system was found to have a performance consistent with a lower detection limit of ca. 1% wt % of crystals and to be able to follow polymorphic transformation during representative crystallization processes. A forward look to the further development of the system is provided.

Original languageEnglish
Pages (from-to)943-948
Number of pages6
JournalCrystal Growth and Design
Volume4
Issue number5
DOIs
Publication statusPublished - Sep 2004

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