In situ non-invasive Raman spectroscopic characterisation of succinic acid polymorphism during segmented flow crystallisation

    • Anuradha R. Pallipuratha
    • Pierre-Baptiste Flandrina
    • Lois E. Waymenta, b, c
    • Chick C. Wilsona, b
    • Karen Robertsona
    • aDepartment of Chemistry, University of Bath, Claverton Down, BA2 7AY, UK
    • bCMAC Future Manufacturing Hub, University of Bath, Claverton Down, Bath BA2 7AY, UK
    • c.Diamond Light Source, Harwell Campus, Didcot, Oxfordshire OX11 0DE, UK

    The kinetically regulated automated input crystalliser for Raman spectroscopy (KRAIC-R) combines highly controlled crystallisation environments, via tri segmented flow, with non-invasive confocal Raman spectroscopy. Taking advantage of the highly reproducible crystallisation environment within a segmented flow crystalliser and the non-invasive nature of confocal spectroscopy, we are able to shine light on the nucleation and growth of Raman active polymorphic materials without inducing unrepresentative crystallisation events through our analysis technique. Using the KRAIC-R we have probed the nucleation and subsequent growth of succinic acid. Succinic acid typically crystallises as β-SA from solution-based crystallisation although some examples of a small proportion of α-SA have been reported in the β-SA product. Here we show that α-SA and β-SA nucleate concomitantly but undergo Ostwald ripening to a predominantly β-SA product.

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