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Structural Elucidation of Amorphous Photocatalytic Polymers from Dynamic Nuclear Polarization Enhanced Solid State NMR

Brownbill, NJ, Sprick, RS, Bonillo, B, Pawsey, S, Aussenac, F, Fielding, AJ, Cooper, AI and Blanc, F (2018) Structural Elucidation of Amorphous Photocatalytic Polymers from Dynamic Nuclear Polarization Enhanced Solid State NMR. Macromolecules, 51 (8). pp. 3088-3096. ISSN 0024-9297

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Abstract

Dynamic nuclear polarization (DNP) solid-state nuclear magnetic resonance (NMR) offers a recent approach to dramatically enhance NMR signals and has enabled detailed structural information to be obtained in a series of amorphous photocatalytic copolymers of alternating pyrene and benzene monomer units, the structures of which cannot be reliably established by other spectroscopic or analytical techniques. Large 13C cross-polarization (CP) magic angle spinning (MAS) signal enhancements were obtained at high magnetic fields (9.4–14.1 T) and low temperature (110–120 K), permitting the acquisition of a 13C INADEQUATE spectrum at natural abundance and facilitating complete spectral assignments, including when small amounts of specific monomers are present. The high 13C signal-to-noise ratios obtained are harnessed to record quantitative multiple contact CP NMR data, used to determine the polymers’ composition. This correlates well with the putative pyrene:benzene stoichiometry from the monomer feed ratio, enabling their structures to be understood.

Item Type: Article
Uncontrolled Keywords: 03 Chemical Sciences, 09 Engineering
Subjects: Q Science > QD Chemistry
Divisions: Pharmacy & Biomolecular Sciences
Publisher: American Chemical Society
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Date Deposited: 27 Jun 2018 10:15
Last Modified: 04 Sep 2021 10:22
DOI or ID number: 10.1021/acs.macromol.7b02544
URI: https://researchonline.ljmu.ac.uk/id/eprint/8900
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