Skip to content

Research at St Andrews

Investigating FAM-N pulses for signal enhancement in MQMAS NMR of quadrupolar nuclei

Research output: Contribution to journalArticle

Standard

Investigating FAM-N pulses for signal enhancement in MQMAS NMR of quadrupolar nuclei. / Colaux, Henri; Dawson, Daniel M.; Ashbrook, Sharon E.

In: Solid State Nuclear Magnetic Resonance, Vol. 84, 08.2017, p. 89-102.

Research output: Contribution to journalArticle

Harvard

Colaux, H, Dawson, DM & Ashbrook, SE 2017, 'Investigating FAM-N pulses for signal enhancement in MQMAS NMR of quadrupolar nuclei', Solid State Nuclear Magnetic Resonance, vol. 84, pp. 89-102. https://doi.org/10.1016/j.ssnmr.2017.01.001

APA

Colaux, H., Dawson, D. M., & Ashbrook, S. E. (2017). Investigating FAM-N pulses for signal enhancement in MQMAS NMR of quadrupolar nuclei. Solid State Nuclear Magnetic Resonance, 84, 89-102. https://doi.org/10.1016/j.ssnmr.2017.01.001

Vancouver

Colaux H, Dawson DM, Ashbrook SE. Investigating FAM-N pulses for signal enhancement in MQMAS NMR of quadrupolar nuclei. Solid State Nuclear Magnetic Resonance. 2017 Aug;84:89-102. https://doi.org/10.1016/j.ssnmr.2017.01.001

Author

Colaux, Henri ; Dawson, Daniel M. ; Ashbrook, Sharon E. / Investigating FAM-N pulses for signal enhancement in MQMAS NMR of quadrupolar nuclei. In: Solid State Nuclear Magnetic Resonance. 2017 ; Vol. 84. pp. 89-102.

Bibtex - Download

@article{680719e4023c4ab382c505f4f839b483,
title = "Investigating FAM-N pulses for signal enhancement in MQMAS NMR of quadrupolar nuclei",
abstract = "Although a popular choice for obtaining high-resolution solid-state NMR spectra of quadrupolar nuclei, the inherently low sensitivity of the multiple-quantum magic-angle spinning (MQMAS) experiment has limited its application for nuclei with low receptivity or when the available sample volume is limited. A number of methods have been introduced in the literature to attempt to address this problem. Recently, we have introduced an alternative, automated approach, based on numerical simulations, for generating amplitude-modulated pulses (termed FAM-N pulses) to enhance the efficiency of the triple- to single-quantum conversion step within MQMAS. This results in efficient pulses that can be used without experimental reoptimisation, ensuring that this method is particularly suitable for challenging nuclei and systems. In this work, we investigate the applicability of FAM-N pulses to a wider variety of systems, and their robustness under more challenging experimental conditions. These include experiments performed under fast MAS, nuclei with higher spin quantum numbers, samples with multiple distinct sites, low-γ nuclei and nuclei subject to large quadrupolar interactions.",
keywords = "Solid-state MAS NMR spectroscopy, MQMAS, Quadrupolar nuclei, Fast-amplitude modulation, FAM-N pulses, Challenging systems",
author = "Henri Colaux and Dawson, {Daniel M.} and Ashbrook, {Sharon E.}",
note = "The authors would like to thank EPSRC (EP/K503162/1) for the award of a studentship to HFC and the ERC (EU FP7 Consolidator Grant 614290 “EXONMR”) for support. SEA would also like to thank the Royal Society and Wolfson Foundation for a merit award. The UK 850 MHz solid-state NMR Facility used in this research was funded by EPSRC and BBSRC (contract reference PR140003), as well as the University of Warwick including via part funding through Birmingham Science City Advanced Materials Projects 1 and 2 supported by Advantage West Midlands (AWM) and the European Regional Development Fund (ERDF). Financial support from the TGIR-RMN-THC Fr3050 CNRS to access the 800 MHz spectrometer (Lille) is gratefully acknowledged.",
year = "2017",
month = aug,
doi = "10.1016/j.ssnmr.2017.01.001",
language = "English",
volume = "84",
pages = "89--102",
journal = "Solid State Nuclear Magnetic Resonance",
issn = "0926-2040",
publisher = "Elsevier",

}

RIS (suitable for import to EndNote) - Download

TY - JOUR

T1 - Investigating FAM-N pulses for signal enhancement in MQMAS NMR of quadrupolar nuclei

AU - Colaux, Henri

AU - Dawson, Daniel M.

AU - Ashbrook, Sharon E.

N1 - The authors would like to thank EPSRC (EP/K503162/1) for the award of a studentship to HFC and the ERC (EU FP7 Consolidator Grant 614290 “EXONMR”) for support. SEA would also like to thank the Royal Society and Wolfson Foundation for a merit award. The UK 850 MHz solid-state NMR Facility used in this research was funded by EPSRC and BBSRC (contract reference PR140003), as well as the University of Warwick including via part funding through Birmingham Science City Advanced Materials Projects 1 and 2 supported by Advantage West Midlands (AWM) and the European Regional Development Fund (ERDF). Financial support from the TGIR-RMN-THC Fr3050 CNRS to access the 800 MHz spectrometer (Lille) is gratefully acknowledged.

PY - 2017/8

Y1 - 2017/8

N2 - Although a popular choice for obtaining high-resolution solid-state NMR spectra of quadrupolar nuclei, the inherently low sensitivity of the multiple-quantum magic-angle spinning (MQMAS) experiment has limited its application for nuclei with low receptivity or when the available sample volume is limited. A number of methods have been introduced in the literature to attempt to address this problem. Recently, we have introduced an alternative, automated approach, based on numerical simulations, for generating amplitude-modulated pulses (termed FAM-N pulses) to enhance the efficiency of the triple- to single-quantum conversion step within MQMAS. This results in efficient pulses that can be used without experimental reoptimisation, ensuring that this method is particularly suitable for challenging nuclei and systems. In this work, we investigate the applicability of FAM-N pulses to a wider variety of systems, and their robustness under more challenging experimental conditions. These include experiments performed under fast MAS, nuclei with higher spin quantum numbers, samples with multiple distinct sites, low-γ nuclei and nuclei subject to large quadrupolar interactions.

AB - Although a popular choice for obtaining high-resolution solid-state NMR spectra of quadrupolar nuclei, the inherently low sensitivity of the multiple-quantum magic-angle spinning (MQMAS) experiment has limited its application for nuclei with low receptivity or when the available sample volume is limited. A number of methods have been introduced in the literature to attempt to address this problem. Recently, we have introduced an alternative, automated approach, based on numerical simulations, for generating amplitude-modulated pulses (termed FAM-N pulses) to enhance the efficiency of the triple- to single-quantum conversion step within MQMAS. This results in efficient pulses that can be used without experimental reoptimisation, ensuring that this method is particularly suitable for challenging nuclei and systems. In this work, we investigate the applicability of FAM-N pulses to a wider variety of systems, and their robustness under more challenging experimental conditions. These include experiments performed under fast MAS, nuclei with higher spin quantum numbers, samples with multiple distinct sites, low-γ nuclei and nuclei subject to large quadrupolar interactions.

KW - Solid-state MAS NMR spectroscopy

KW - MQMAS

KW - Quadrupolar nuclei

KW - Fast-amplitude modulation

KW - FAM-N pulses

KW - Challenging systems

U2 - 10.1016/j.ssnmr.2017.01.001

DO - 10.1016/j.ssnmr.2017.01.001

M3 - Article

VL - 84

SP - 89

EP - 102

JO - Solid State Nuclear Magnetic Resonance

JF - Solid State Nuclear Magnetic Resonance

SN - 0926-2040

ER -

Related by author

  1. Application of NMR crystallography to highly disordered templated materials: extensive local structural disorder in the gallophosphate GaPO-34A

    Ashbrook, S. E., Dawson, D. M., Gan, Z., Hooper, J. E., Hung, I., Macfarlane, L. E., McKay, D., McLeod, L. K. & Walton, R. I., 4 Aug 2020, In : Inorganic Chemistry. Article ASAP

    Research output: Contribution to journalArticle

  2. Solid-state host-guest influences on a BODIPY dye hosted within a crystalline sponge

    Gee, W. J., Shepherd, H. J., Dawson, D. M., Ashbrook, S. E., Raithby, P. R. & Burrows, A. D., 30 Jul 2020, In : New Journal of Chemistry. Advance Article, 8 p.

    Research output: Contribution to journalArticle

  3. Phase distribution, composition and disorder in Y2(Hf,Sn)2O7 ceramics: insights from solid-state NMR spectroscopy and first-principles calculations

    Moran, R. F., Fernandes, A., Dawson, D. M., Sneddon, S., Gandy, A. S., Reeves-McLaren, N., Whittle, K. R. & Ashbrook, S. E., 9 Jul 2020, In : Journal of Physical Chemistry C. In press

    Research output: Contribution to journalArticle

  4. Following the unusual breathing behaviour of 17O-enriched mixed-metal (Al,Ga)-MIL-53 using NMR crystallography

    Rice, C. M., Davis, Z. H., McKay, D., Bignami, G. P. M., Chitac, R. G., Dawson, D. M., Morris, R. E. & Ashbrook, S. E., 16 Jun 2020, In : Physical Chemistry Chemical Physics. Advance Article, 13 p.

    Research output: Contribution to journalArticle

  5. Site-specific iron substitution in STA-28, a large pore aluminophosphate zeotype prepared using 1,10-phenanthrolines as framework-bound templates

    Watts, A. E., Lozinska, M. M., Slawin, A. M. Z., Mayoral, A., Dawson, D. M., Ashbrook, S. E., Bode, B. E., Dugulan, I., Shannon, M., Cox, P., Turrina, A. & Wright, P. A., 8 Jun 2020, In : Angewandte Chemie International Edition. Early View, 6 p.

    Research output: Contribution to journalArticle

Related by journal

  1. 13C pNMR of “crumple zone” Cu(II) isophthalate metal-organic frameworks

    Dawson, D. M., Sansome, C. E. F., McHugh, L. N., McPherson, M. J., McCormick McPherson, L. J., Morris, R. E. & Ashbrook, S. E., 14 May 2019, In : Solid State Nuclear Magnetic Resonance. In press

    Research output: Contribution to journalArticle

  2. NMR chemical shifts of urea loaded copper benzoate. A joint solid-state NMR and DFT study

    Ke, Z., Jamieson, L., Dawson, D. M., Ashbrook, S. E. & Buehl, M., 20 Apr 2019, In : Solid State Nuclear Magnetic Resonance. In press

    Research output: Contribution to journalSpecial issue

  3. NMR spectroscopy of paramagnetic solids

    Ashbrook, S. E. & Jaroniec, C. P., Dec 2019, In : Solid State Nuclear Magnetic Resonance. 104, 1 p., 101625.

    Research output: Contribution to journalEditorial

  4. Sensitivity improvement in 5QMAS NMR Experiments Using FAM-N Pulses

    Kanwal, N., Colaux, H., Dawson, D. M., Nishyama, Y. & Ashbrook, S. E., Aug 2019, In : Solid State Nuclear Magnetic Resonance. 100, p. 1-10 10 p.

    Research output: Contribution to journalArticle

ID: 248478677

Top