• Login
• Admin

Galtry, Elizabeth Sarah (2025) Development of segmented flow crystallisers for in situ X-ray diffraction analysis. PhD thesis, University of Nottingham.

Preview

PDF (Corrected thesis after viva) (Thesis - as examined) - Requires a PDF viewer such as GSview, Xpdf or Adobe Acrobat Reader Available under Licence Creative Commons Attribution. Download (9MB) | Preview

Abstract

The study of crystallisation through in situ analysis methods is key to elucidating the crystallisation processes of polymorphic materials. This thesis presents research on the development of in situ X-ray diffraction (XRD) techniques for the study of segmented flow crystallisation. This work was carried out as a joint studentship between University of Nottingham and Diamond Light Source, the UK’s national synchrotron research facility.

Chapter 5 describes the commissioning of a temperature-cycling segmented flow crystalliser, the KRAIC-T. Temperature-cycling during crystallisation enabled enhanced control over the crystallisation process of succinic acid. Integration of the KRAIC-T as a sample environment on Beamline I11 at Diamond Light Source involved the use of an upgraded data acquisition technique to improve the signal-to-noise of collected in situ powder X-ray diffraction data (PXRD). The study of the slurrying crystallisation of the polymorphic crystal system, ortho-aminobenzoic acid, was used to verify the improvement of the in situ technique. These data were also used for the development of enhanced data processing techniques.

In situ XRD analysis is largely limited to synchrotron facilities due to the high intensity, high energy X-rays required for XRD investigation of complex sample environments. Chapter 4 discusses the development of the KRAIC-Xl, a segmented flow crystalliser for lab-source PXRD analysis at the Flow-Xl facility, University of Leeds. Proof-of-principles studies found the lab-source system was able to achieve time-resolved PXRD studies of glycine (GLY) anti-solvent crystallisation, finding the initial crystallisation of the highly metastable β-GLY and rapid transformation to the more stable α-GLY polymorph.

Chapter 3 details the development of Python-based processing methodologies for PXRD data collected from the KRAIC-T and KRAIC-Xl systems. Existing processing techniques are often labour-intensive and time-consuming for processing of PXRD from complex environments; specialist Python modules were used to develop novel processing workflows in Chapter 3 maximise the diffraction signal extracted, whilst minimising data processing time.

Chapter 6 discusses the development of the KRAIC-S v2 and v3; upgraded crystalliser designs for serial crystallography during segmented flow at Beamline I19, Diamond Light Source. Beamtime with the KRAIC-S v2 on the cooling crystallisation of paracetamol assessed the system, showing an improved ease-of-use, but highlighted limitations of the serial crystallography technique. Chapter 7 uses the final KRAIC-S v3 design for the study of nonphotochemical laser induced nucleation of potassium chloride, achieving induced nucleation of a single particle per droplet and accompanying in situ XRD.

Item Type:	Thesis (University of Nottingham only) (PhD)
Supervisors:	Robertson, Karen Lester, Edward Allan, Dave Warren, Mark Day, Sarah
Keywords:	In situ X-ray diffraction techniques; Segmented flow crystallisation; Crystallisation; Polymorphic materials
Subjects:	T Technology > TP Chemical technology
Faculties/Schools:	UK Campuses > Faculty of Engineering > Department of Chemical and Environmental Engineering
Item ID:	80261
Depositing User:	Galtry, Elizabeth
Date Deposited:	31 Jul 2025 04:40
Last Modified:	31 Jul 2025 04:40
URI:	https://eprints.nottingham.ac.uk/id/eprint/80261

Actions (Archive Staff Only)

Edit View