Exploiting solid-state dynamic nuclear polarization NMR spectroscopy to establish the spatial distribution of polymorphic phases in a solid material

Cousin, Samuel François, Hughes, Colan E., Ziarelli, Fabio, Viel, Stéphane, Mollica, Giulia, Harris, Kenneth D. M. ORCID: https://orcid.org/0000-0001-7855-8598, Pinon, Arthur C. and Thureau, Pierre 2023. Exploiting solid-state dynamic nuclear polarization NMR spectroscopy to establish the spatial distribution of polymorphic phases in a solid material. Chemical Science 14 , pp. 10121-10128. 10.1039/D3SC02063K

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Abstract

Solid-state DNP NMR can enhance the ability to detect minor amounts of solid phases within heterogenous materials. Here we demonstrate that NMR contrast based on transport of DNP-enhanced polarization can be exploited in the challenging case of early detection of a small amount of a minor polymorphic phase within a major polymorph, and we show that this approach can yield quantitative information on the spatial distribution of the two polymorphs. We focus on the detection of a minor amount (<4%) of polymorph III of m-aminobenzoic acid within a powder sample of polymorph I at natural isotopic abundance. Based on proposed models of the spatial distribution of the two polymorphs, simulations of 1H spin diffusion allow NMR data to be calculated for each model as a function of particle size and the relative amounts of the polymorphs. Comparison between simulated and experimental NMR data allows the model(s) best representing the spatial distribution of the polymorphs in the system to be established.

Item Type:	Article
Date Type:	Published Online
Status:	Published
Schools:	Advanced Research Computing @ Cardiff (ARCCA) Chemistry
Publisher:	Royal Society of Chemistry
ISSN:	2041-6520
Funders:	European Union Horizon 2020
Date of First Compliant Deposit:	29 June 2023
Date of Acceptance:	22 June 2023
Last Modified:	12 Jun 2024 12:31
URI:	https://orca.cardiff.ac.uk/id/eprint/160707

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