Size-exclusion chromatographic NMR under HR-MAS

Lucena Alcalde, Guillermo, Anderson, Natalie and Day, Iain J (2016) Size-exclusion chromatographic NMR under HR-MAS. Magnetic Resonance in Chemistry, 55 (5). pp. 485-491. ISSN 0749-1581

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Abstract

The 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.

Item Type: Article
Keywords: Diffusion, Size exclusion, HR-MAS
Schools and Departments: School of Life Sciences > Chemistry
Subjects: Q Science > QD Chemistry > QD0071 Analytical chemistry
Q Science > QD Chemistry > QD0450 Physical and theoretical chemistry
Depositing User: Iain Day
Date Deposited: 20 Jun 2016 12:12
Last Modified: 20 Jun 2017 12:18
URI: http://sro.sussex.ac.uk/id/eprint/61595

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Project NameSussex Project NumberFunderFunder Ref
NMR Studies of the Early Stages of Aggregation PhenomenaG0186EPSRC-ENGINEERING & PHYSICAL SCIENCES RESEARCH COUNCILEP/H025367/1