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Simultaneous differential scanning calorimetry – synchrotron X-ray powder diffraction : a powerful technique for physical form characterisation in pharmaceutical materials

Clout, Alexander; Buanz, Asma B. M.; Prior, Timothy J.; Reinhard, Christina; Wu, Yue; O'Hare, Dermot; Williams, Gareth R.; Gaisford, Simon

Authors

Alexander Clout

Asma B. M. Buanz

Christina Reinhard

Yue Wu

Dermot O'Hare

Gareth R. Williams

Simon Gaisford



Abstract

© 2016 American Chemical Society. We report a powerful new technique: hyphenating synchrotron X-ray powder diffraction (XRD) with differential scanning calorimetry (DSC). This is achieved with a simple modification to a standard laboratory DSC instrument, in contrast to previous reports which have involved extensive and complex modifications to a DSC to mount it in the synchrotron beam. The high-energy X-rays of the synchrotron permit the recording of powder diffraction patterns in as little as 2 s, meaning that thermally induced phase changes can be accurately quantified and additional insight on the nature of phase transitions obtained. Such detailed knowledge cannot be gained from existing laboratory XRD instruments, since much longer collection times are required. We demonstrate the power of our approach with two model systems, glutaric acid and sulfathiazole, both of which show enantiotropic polymorphism. The phase transformations between the low and high temperature polymorphs are revealed to be direct solid-solid processes, and sequential refinement against the diffraction patterns obtained permits phase fractions at each temperature to be calculated and unit cell parameters to be accurately quantified as a function of temperature. The combination of XRD and DSC has further allowed us to identify mixtures of phases which appeared phase-pure by DSC.

Citation

Clout, A., Buanz, A. B. M., Prior, T. J., Reinhard, C., Wu, Y., O'Hare, D., …Gaisford, S. (2016). Simultaneous differential scanning calorimetry – synchrotron X-ray powder diffraction : a powerful technique for physical form characterisation in pharmaceutical materials. Analytical chemistry, 88(20), 10111-10117. https://doi.org/10.1021/acs.analchem.6b02549

Journal Article Type Article
Acceptance Date Sep 19, 2016
Online Publication Date Sep 30, 2016
Publication Date Oct 18, 2016
Deposit Date Oct 25, 2016
Publicly Available Date Oct 25, 2016
Journal Analytical chemistry
Print ISSN 0003-2700
Electronic ISSN 1520-6882
Publisher American Chemical Society
Peer Reviewed Peer Reviewed
Volume 88
Issue 20
Pages 10111-10117
DOI https://doi.org/10.1021/acs.analchem.6b02549
Keywords Hyphenating synchrotron X-ray powder diffraction (XRD)
Public URL https://hull-repository.worktribe.com/output/444520
Publisher URL http://pubs.acs.org/doi/abs/10.1021/acs.analchem.6b02549
Copyright Statement ACS AuthorChoice - This is an open access article published under an ACS AuthorChoice License, which permits copying and redistribution of the article or any adaptations for non-commercial purposes.
Additional Information Copy of an article published in: Analytical chemistry, v.88, issue 20.

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Copyright Statement
ACS AuthorChoice - This is an open access article published under an ACS AuthorChoice License, which permits copying and redistribution of the article or any adaptations for non-commercial purposes.



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