Flow‐Xl : a new facility for the analysis of crystallization in flow systems
Turner, T. D. and O'Shaughnessy, C. and He, X. and Levenstein, M. A. and Hunter, L. and Wojciechowski, J. and Bristowe, H. and Stone, R. and Wilson, C. C. and Florence, A. and Robertson, K. and Kapur, N. and Meldrum, F. C. (2024) Flow‐Xl : a new facility for the analysis of crystallization in flow systems. Journal of Applied Crystallography, 57 (5). pp. 1299-1310. ISSN 0021-8898 (https://doi.org/10.1107/s1600576724006113)
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Abstract
Characterization of crystallization processes in situ is of great importance to furthering knowledge of how nucleation and growth processes direct the assembly of organic and inorganic materials in solution and, critically, understanding the influence that these processes have on the final physico‐chemical properties of the resulting solid form. With careful specification and design, as demonstrated here, it is now possible to bring combined X‐ray diffraction and Raman spectroscopy, coupled to a range of fully integrated segmented and continuous flow platforms, to the laboratory environment for in situ data acquisition for timescales of the order of seconds. The facility used here (Flow‐Xl) houses a diffractometer with a micro‐focus Cu Kα rotating anode X‐ray source and a 2D hybrid photon‐counting detector, together with a Raman spectrometer with 532 and 785 nm lasers. An overview of the diffractometer and spectrometer setup is given, and current sample environments for flow crystallization are described. Commissioning experiments highlight the sensitivity of the two instruments for time‐resolved in situ data collection of samples in flow. Finally, an example case study to monitor the batch crystallization of sodium sulfate from aqueous solution, by tracking both the solute and solution phase species as a function of time, highlights the applicability of such measurements in determining the kinetics associated with crystallization processes. This work illustrates that the Flow‐Xl facility provides high‐resolution time‐resolved in situ structural phase information through diffraction data together with molecular‐scale solution data through spectroscopy, which allows crystallization mechanisms and their associated kinetics to be analysed in a laboratory setting.
ORCID iDs
Turner, T. D., O'Shaughnessy, C., He, X., Levenstein, M. A., Hunter, L., Wojciechowski, J., Bristowe, H., Stone, R., Wilson, C. C., Florence, A. ORCID: https://orcid.org/0000-0002-9706-8364, Robertson, K., Kapur, N. and Meldrum, F. C.;-
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Item type: Article ID code: 90328 Dates: DateEvent1 October 2024Published19 August 2024Published Online23 June 2024Accepted4 August 2023SubmittedSubjects: Science > Chemistry > Crystallography Department: Strategic Research Themes > Advanced Manufacturing and Materials
Technology and Innovation Centre > Continuous Manufacturing and Crystallisation (CMAC)
Faculty of Science > Strathclyde Institute of Pharmacy and Biomedical SciencesDepositing user: Pure Administrator Date deposited: 23 Aug 2024 11:39 Last modified: 28 Oct 2024 08:59 URI: https://strathprints.strath.ac.uk/id/eprint/90328