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Size-exclusion chromatographic NMR under HR-MAS
journal contribution
posted on 2023-06-09, 01:45 authored by Guillermo Lucena Alcalde, Natalie Anderson, Iain DayThe addition of stationary phases or sample modifiers can be used to modify the separation achievable in the diffusion domain of diffusion NMR experiments or provide information on the nature of the analyte–sample modifier interaction. Unfortunately, the addition of insoluble chromatographic stationary phases can lead to line broadening and degradation in spectral resolution, largely because of differences in magnetic susceptibility between the sample and the stationary phase. High-resolution magic angle spinning (HR-MAS) techniques can be used to remove this broadening. Here, we attempt the application of HR-MAS to size-exclusion chromatographic NMR with limited success. Observed diffusion coefficients for polymer molecular weight reference standards are shown to be larger than those obtained on static samples. Further investigation reveals that under HR-MAS it is possible to obtain reasonably accurate estimates of diffusion coefficients, using either full rotor synchronisation or sophisticated pulse sequences. The requirement for restricting the sample to the centre of the MAS rotor to ensure homogeneous magnetic and RF fields is also tested.
Funding
NMR Studies of the Early Stages of Aggregation Phenomena; G0186; EPSRC-ENGINEERING & PHYSICAL SCIENCES RESEARCH COUNCIL; EP/H025367/1
History
Publication status
- Published
File Version
- Accepted version
Journal
Magnetic Resonance in ChemistryISSN
0749-1581Publisher
WileyExternal DOI
Issue
5Volume
55Page range
485-491Department affiliated with
- Chemistry Publications
Full text available
- Yes
Peer reviewed?
- Yes
Legacy Posted Date
2016-06-20First Open Access (FOA) Date
2017-06-16First Compliant Deposit (FCD) Date
2016-06-20Usage metrics
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