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 ISSN 1090-7807.

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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
Subjects:	Q Science > QD Chemistry
Divisions:	Faculty of Science, Engineering and Medicine > Science > Chemistry Faculty of Science, Engineering and Medicine > Science > Physics
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:	Date Event November 2015 Published 16 September 2015 Available 1 September 2015 Accepted 27 May 2015 Submitted
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 (Creative Commons)
Date of first compliant deposit:	31 December 2015
Date of first compliant Open Access:	31 December 2015
RIOXX Funder/Project Grant:	Project/Grant ID RIOXX Funder Name Funder ID UNSPECIFIED [EPSRC] Engineering and Physical Sciences Research Council http://dx.doi.org/10.13039/501100000266
Related URLs:	Related dataset

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