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Practical considerations for the acquisition of ultra-wideline 14 N NMR spectra
Several considerations for the acquisition, processing, and analysis of high quality ultra-wideline (UW) N solid-state NMR (SSNMR) powder patterns under static conditions are discussed. It is shown that the N quadrupolar parameters may be determined accurately using the frequencies of only two disco...
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Published in: | Solid state nuclear magnetic resonance 2017-07, Vol.84, p.45 |
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Main Authors: | , , , |
Format: | Article |
Language: | English |
Online Access: | Get full text |
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Summary: | Several considerations for the acquisition, processing, and analysis of high quality ultra-wideline (UW)
N solid-state NMR (SSNMR) powder patterns under static conditions are discussed. It is shown that the
N quadrupolar parameters may be determined accurately using the frequencies of only two discontinuities in
N NMR powder patterns that are dominated by the first-order quadrupolar interaction, thereby eliminating the need for the acquisition of the entire pattern and concomitantly reducing experimental time. A framework for utilizing the WURST-CPMG pulse sequence to improve the efficiency of UW
N SSNMR experiments is explored in two parts: (i) a systematic investigation of the design and parameterization of the WURST pulse is presented, and (ii) the development of the practical aspects of CPMG refocusing for the acquisition of UW
N SSNMR powder patterns is discussed, with a focus on maximizing both signal-to-noise and resolution, and minimizing spectral distortions. Finally, a strategy is demonstrated that allows for the measurement of the
N quadrupolar parameters for any nitrogen moiety whose quadrupolar coupling constant falls within the range 0.8≤|C
|≤1.5MHz, by acquiring only two
N NMR sub-spectra at strategically located transmitter frequencies; these results are compared to full powder patterns which are acquired using frequency-stepped methods. The methodologies and practical considerations outlined herein are not only useful for the rapid acquisition of UW
N NMR spectra, but may also be modified and applied for UW NMR of a plethora of quadrupolar and spin-1/2 nuclides. |
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ISSN: | 1527-3326 |