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The use of a selective saturation pulse to suppress t1 noise in two-dimensional 1H fast magic angle spinning solid-state NMR spectroscopy
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Robertson, Aiden, Pandey, Manoj, Marsh, Andrew, Nishiyama, Yusuke and Brown, Steven P. (2015) The use of a selective saturation pulse to suppress t1 noise in two-dimensional 1H fast magic angle spinning solid-state NMR spectroscopy. Journal of Magnetic Resonance, 260 . pp. 89-97. doi:10.1016/j.jmr.2015.09.005
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Official URL: http://dx.doi.org/10.1016/j.jmr.2015.09.005
Abstract
A selective saturation pulse at fast magic angle spinning (MAS) frequencies (60+ kHz) suppresses t1 noise in the indirect dimension of two-dimensional 1H MAS NMR spectra. The method is applied to a synthetic nucleoside with an intense methyl 1H signal due to triisopropylsilyl (TIPS) protecting groups. Enhanced performance in terms of suppressing the methyl signal while minimising the loss of signal intensity of nearby resonances of interest relies on reducing spin diffusion – this is quantified by comparing two-dimensional 1H NOESY-like spin diffusion spectra recorded at 30 to 70 kHz MAS. For a saturation pulse centred at the methyl resonance, the effect of changing the nutation frequency at different MAS frequencies as well as the effect of changing the pulse duration is investigated. By applying a pulse of duration 30 ms and nutation frequency 725 Hz at 70 kHz MAS, a good compromise of significant suppression of the methyl resonance combined with the signal intensity of resonances greater than 5 ppm away from the methyl resonance being largely unaffected is achieved. The effectiveness of using a selective saturation pulse is demonstrated for both homonuclear 1H – 1H double quantum (DQ)/ single quantum (SQ) MAS and 14N – 1H heteronuclear multiple quantum coherence (HMQC) two-dimensional solid-state NMR experiments.
| Item Type: | Journal Article | ||||||||||
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| Subjects: | Q Science > QD Chemistry | ||||||||||
| Divisions: | Faculty of Science > Chemistry Faculty of Science > Physics |
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| Library of Congress Subject Headings (LCSH): | Nuclear magnetic resonance -- Research, Crystallography | ||||||||||
| Journal or Publication Title: | Journal of Magnetic Resonance | ||||||||||
| Publisher: | Academic Press | ||||||||||
| ISSN: | 1090-7807 | ||||||||||
| Official Date: | November 2015 | ||||||||||
| Dates: |
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| Date of first compliant deposit: | 31 December 2015 | ||||||||||
| Volume: | 260 | ||||||||||
| Page Range: | pp. 89-97 | ||||||||||
| DOI: | 10.1016/j.jmr.2015.09.005 | ||||||||||
| Status: | Peer Reviewed | ||||||||||
| Publication Status: | Published | ||||||||||
| Access rights to Published version: | Open Access | ||||||||||
| RIOXX Funder/Project Grant: |
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