Size‐exclusion chromatographic NMR under HR‐MAS

• Published in: Magnetic resonance in chemistry Vol. 55; no. 5; pp. 485 - 491
• Main Authors: Lucena Alcalde, Guillermo, Anderson, Natalie, Day, Iain J.
• Format: Journal Article
• Language: English
• Published: England Wiley Subscription Services, Inc 01.05.2017
• Subjects: Chromatography; Diffusion; Diffusion coefficient; Estimates; High resolution; HR‐MAS; Line broadening; Magnetic permeability; Molecular weight; NMR; Nuclear magnetic resonance; Phases; Rotors; Separation; size exclusion; Spectral resolution; diffusion; HR-MAS; size exclusion
• ISSN: 0749-1581; 1097-458X
• DOI: 10.1002/mrc.4464

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. Copyright © 2016 John Wiley & Sons, Ltd. 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 for static samples. Further investigation reveals that it is possible to obtain reasonably accurate estimates of diffusion coefficients under HR‐MAS, either using 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.