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Improving the sensitivity of J coupling measurements in solids with application to disordered materials

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Improving the sensitivity of J coupling measurements in solids with application to disordered materials. / Guerry, Paul; Brown, Steven P.; Smith, Mark Edmund.
In: AIP Advances, Vol. 6, No. 5, 055008, 05.2016.

Research output: Contribution to Journal/Magazine › Journal article › peer-review

Harvard

Guerry, P, Brown, SP & Smith, ME 2016, 'Improving the sensitivity of J coupling measurements in solids with application to disordered materials', AIP Advances, vol. 6, no. 5, 055008. https://doi.org/10.1063/1.4948965

APA

Guerry, P., Brown, S. P., & Smith, M. E. (2016). Improving the sensitivity of J coupling measurements in solids with application to disordered materials. AIP Advances, 6(5), Article 055008. https://doi.org/10.1063/1.4948965

Vancouver

Guerry P, Brown SP, Smith ME. Improving the sensitivity of J coupling measurements in solids with application to disordered materials. AIP Advances. 2016 May;6(5):055008. Epub 2016 May 4. doi: 10.1063/1.4948965

Author

Guerry, Paul ; Brown, Steven P. ; Smith, Mark Edmund. / Improving the sensitivity of J coupling measurements in solids with application to disordered materials. In: AIP Advances. 2016 ; Vol. 6, No. 5.

Bibtex

@article{86ab976b9800420e89e589a0faf4647f,
title = "Improving the sensitivity of J coupling measurements in solids with application to disordered materials",
abstract = "It has been shown previously that for magic angle spinning (MAS) solid state NMR the refocused INADEQUATE spin-echo (REINE) experiment can usefully quantify scalar (J) couplings in disordered solids. This paper focuses on the two z filter components in the original REINE pulse sequence, and investigates by means of a product operator analysis and fits to density matrix simulations the effects that their removal has on the sensitivity of the experiment and on the accuracy of the extracted J couplings. The first z filter proves unnecessary in all the cases investigated here and removing it increases the sensitivity of the experiment by a factor ∼1.1–2.0. Furthermore, for systems with broad isotropic chemical shift distributions (namely whose full widths at half maximum are greater than 30 times the mean J coupling strength), the second z filter can also be removed, thus allowing whole-echo acquisition and providing an additional √2 gain in sensitivity. Considering both random and systematic errors in the values obtained, J couplings determined by fitting the intensity modulations of REINE experiments carry an uncertainty of 0.2–1.0 Hz (∼1−10 %).",
author = "Paul Guerry and Brown, {Steven P.} and Smith, {Mark Edmund}",
year = "2016",
month = may,
doi = "10.1063/1.4948965",
language = "English",
volume = "6",
journal = "AIP Advances",
issn = "2158-3226",
publisher = "American Institute of Physics Publising LLC",
number = "5",

}

RIS

TY - JOUR

T1 - Improving the sensitivity of J coupling measurements in solids with application to disordered materials

AU - Guerry, Paul

AU - Brown, Steven P.

AU - Smith, Mark Edmund

PY - 2016/5

Y1 - 2016/5

N2 - It has been shown previously that for magic angle spinning (MAS) solid state NMR the refocused INADEQUATE spin-echo (REINE) experiment can usefully quantify scalar (J) couplings in disordered solids. This paper focuses on the two z filter components in the original REINE pulse sequence, and investigates by means of a product operator analysis and fits to density matrix simulations the effects that their removal has on the sensitivity of the experiment and on the accuracy of the extracted J couplings. The first z filter proves unnecessary in all the cases investigated here and removing it increases the sensitivity of the experiment by a factor ∼1.1–2.0. Furthermore, for systems with broad isotropic chemical shift distributions (namely whose full widths at half maximum are greater than 30 times the mean J coupling strength), the second z filter can also be removed, thus allowing whole-echo acquisition and providing an additional √2 gain in sensitivity. Considering both random and systematic errors in the values obtained, J couplings determined by fitting the intensity modulations of REINE experiments carry an uncertainty of 0.2–1.0 Hz (∼1−10 %).

AB - It has been shown previously that for magic angle spinning (MAS) solid state NMR the refocused INADEQUATE spin-echo (REINE) experiment can usefully quantify scalar (J) couplings in disordered solids. This paper focuses on the two z filter components in the original REINE pulse sequence, and investigates by means of a product operator analysis and fits to density matrix simulations the effects that their removal has on the sensitivity of the experiment and on the accuracy of the extracted J couplings. The first z filter proves unnecessary in all the cases investigated here and removing it increases the sensitivity of the experiment by a factor ∼1.1–2.0. Furthermore, for systems with broad isotropic chemical shift distributions (namely whose full widths at half maximum are greater than 30 times the mean J coupling strength), the second z filter can also be removed, thus allowing whole-echo acquisition and providing an additional √2 gain in sensitivity. Considering both random and systematic errors in the values obtained, J couplings determined by fitting the intensity modulations of REINE experiments carry an uncertainty of 0.2–1.0 Hz (∼1−10 %).

U2 - 10.1063/1.4948965

DO - 10.1063/1.4948965

M3 - Journal article

VL - 6

JO - AIP Advances

JF - AIP Advances

SN - 2158-3226

IS - 5

M1 - 055008

ER -