Dataset for "Continuous flow for materials synthesis, assembly and crystallisation at Diamond: discovery and delivery of high value materials"

Continuous crystallisation of the model system Carbamazepine (CBZ) in ethanol in the KRAIC-D (Kinetically Regulated Automated Input Crystalliser - Diffraction) platform on beamline I11 (high resolution powder diffraction) is presented. The effect of introducing a controlled solid interface into the crystallisation process is investigated, where CBZ form III seeds are introduced in polymorphic purity at different seeding positions (pre- and post-nucleation) throughout the length of the KRAIC-D. The video associated with Chapter 4 corresponds with a post-nucleation CBZ form III experiment where a separation of crystal habit is observed as a result of the different interaction with the flow paths in the solution slugs with the segmented flow.

The second device is the KRAIC-S (Kinetically Regulated Automated Input Crystalliser - Single Crystal) platform installed at I19 (small molecule single crystal beamline) employed to investigate the continuous crystallisation of paracetamol (PCM) in 60:40 water:isopropanol via a range of experiments including unseeded and seeded cooling crystallisations. The unseeded experiments also looked at the crystallisation at different set points along the KRAIC-S (6.7 m and 8.7 m) to investigate crystal growth and crystal rotation at different length scales. The videos associated with Chapter 5 include single crystals produced from the range of experiments investigated. Each video tracks a different single crystal in a solution slug, where through use of the slug triggering mechanism, whereby an optical trigger prompts translation of the motorised stage to artificially suspend the single crystal in the X-ray beam during data collection. These videos complement the diffraction data and can provide explanation for data collections, which do not achieve cell indexation as the single crystal is shown to move in and out of the X-ray beam in these videos.

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Cite this dataset as:
Wayment, L., 2020. Dataset for "Continuous flow for materials synthesis, assembly and crystallisation at Diamond: discovery and delivery of high value materials". Bath: University of Bath Research Data Archive. Available from: https://doi.org/10.15125/BATH-00779.

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Data

CBZ form III … Chapter 4.MOV
video/quicktime (13MB)
Creative Commons: Attribution 4.0

Carbamazepine (CBZ) is well known to typically present as needles for CBZ form II and as blocks for CBZ form III. However, in spite of only detecting CBZ III in the in situ Powder X-ray Diffraction data after post-nucleation seeding, aggregated needles were the main habit observed, in addition to a low proportion of small blocks. This is an unusual case of crystallising CBZ form III needles. The two habits are shown to separate as a result of their different interaction with the flow paths.

Chapter 5 - KRAIC-S.zip
application/zip (35MB)
Creative Commons: Attribution 4.0

Videos of single crystals tracked by the slug triggering mechanism comprising an optical trigger and translation of the motorised stage to artificially suspend the single crystal in the X-ray beam during data collection. Videos are categorised into unseeded and seeded crystallisations of paracetamol (PCM). The unseeded cooling crystallisation are further segmented into 6.7 m and 8.7 m crystalliser length. N.B videos are rotated by 180° and thus is observed as residing in the top of solution slug

Slug Triggering Mechanism.3gp
video/3gpp (145MB)
Creative Commons: Attribution 4.0

Slug Triggering Mechanism comprising the optical trigger and motorised stage translation to artificially suspend the solution slugs in the X-ray beam.

Creators

Lois Wayment
University of Bath; Diamond Light Source Ltd

Contributors

Chick Wilson
Supervisor
University of Bath

Karen Robertson
Supervisor
University of Nottingham

Mark R Warren
Supervisor
Diamond Light Source Ltd

David R. Allan
Supervisor
Diamond Light Source Ltd

Chiu Tang
Supervisor
Diamond Light Source Ltd

Daniel Scott
Contributor
University of Bath

Mark Levenstein
Contributor
University of Illinois at Urbana-Champaign

Pollyanna Payne
Contributor
University of Bath

Ruth Lunt
Contributor
University of Bath

Pierre-Baptiste Flandrin
Contributor
University of Bath

University of Bath
Rights Holder

Diamond Light Source Ltd
Rights Holder

Documentation

Data collection method:

Videos obtained using Camera positioned by X-ray beam on beamline I19, the small molecule single crystal beamline at Diamond Light Source.

Documentation Files

ESI Details … - KRAIC-S.docx
application/vnd.openxmlformats-officedocument.wordprocessingml.document (21kB)
Creative Commons: Attribution 4.0

Details of videos of single crystals tracked in solution slugs, including experiment type and run number. The Paracetamol (PCM) form II videos also state the polymorphic outcome as PCM form II was not produced in each case, in some instances the thermodynamically stable PCM form I polymorph was crystallised instead.

Context of Research.docx
application/vnd.openxmlformats-officedocument.wordprocessingml.document (25kB)
Creative Commons: Attribution 4.0

Context of Research

Funders

Engineering and Physical Sciences Research Council (EPSRC)
https://doi.org/10.13039/501100000266

Future Continuous Manufacturing and Advanced Crystallisation Research Hub
EP/P006965/1

Diamond Light Source
https://doi.org/10.13039/100011889

Diamond Light Source studentship

Publication details

Publication date: 1 June 2020
by: University of Bath

Version: 1

DOI: https://doi.org/10.15125/BATH-00779

URL for this record: https://researchdata.bath.ac.uk/id/eprint/779

Related articles

Levenstein, M. A., Wayment, L., Scott, C. D., Lunt, R., Flandrin, P.-B., Day, S. J., Tang, C. C., Wilson, C. C., Meldrum, F. C., Kapur, N. and Robertson, K., 2020. Dynamic Crystallization Pathways of Polymorphic Pharmaceuticals Revealed in Segmented Flow with Inline Powder X-ray Diffraction. Analytical Chemistry, 92(11), pp.7754-7761. Available from: https://doi.org/10.1021/acs.analchem.0c00860.

Contact information

Please contact the Research Data Service in the first instance for all matters concerning this item.

Contact person: Lois Wayment

Departments:

Faculty of Science
Chemistry