Metastable crystalline phase formation in deep eutectic systems revealed by simultaneous synchrotron XRD and DSC

The phase behaviour of various deep eutectic systems was analysed using concurrent synchrotron powder X-ray diffraction and differential scanning calorimetry. Deep eutectic systems containing the pharmaceuticals metacetamol, 2-ethoxybenzamide or benzamide as binary mixtures with phenol revealed new...

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Bibliographic Details
Published in:Chemical communications (Cambridge, England) England), 2020-09, Vol.56 (73), p.1726-1729
Main Authors: Hall, Charlie L, Potticary, Jason, Hamilton, Victoria, Gaisford, Simon, Buanz, Asma, Hall, Simon R
Format: Article
Language:English
Subjects:
Benzamide
Binary mixtures
Crystal structure
Crystallinity
Crystals
Eutectic temperature
Materials science
Metastable phases
Phenols
Synchrotrons
X ray powder diffraction
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Summary:The phase behaviour of various deep eutectic systems was analysed using concurrent synchrotron powder X-ray diffraction and differential scanning calorimetry. Deep eutectic systems containing the pharmaceuticals metacetamol, 2-ethoxybenzamide or benzamide as binary mixtures with phenol revealed new crystalline phases melting either before or with crystals of phenol, highlighting their lower stabilities. Furthermore, in the phenol : 2-ethoxybenzamide system it was shown that multiple metastable phases can form, highlighting the potential for the separation of a hierarchy of crystal structures with differing stabilities from eutectic systems. Through these experiments, we strengthen the idea that eutectic systems can be described by understanding the formation and stabilities of metastable co-crystalline structures. These novel results lead to a deeper understanding of the structure and thermodynamics of deep eutectic solvents, with relevance for analagous systems across materials science. For the first time, simultaneous pXRD and DSC is used to investigate the crystallinity of deep eutectic solvents upon cooling.
ISSN:1359-7345
1364-548X
DOI:10.1039/d0cc04696e