Ultrafast Magic Angle Spinning Nuclear Magnetic Resonance

Deschamps, Michaël

doi:10.1016/b978-0-12-800185-1.00003-6

Cited by 44 publications

(25 citation statements)

References 145 publications

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“…In the strongly coupled homonuclear spin interactions, like 1 H spin network through 1 H-1 H dipolar couplings (120.1 kHz at 1Å), the situation is much more complicated. In such a case very fast MAS (> 60 kHz) is required to suppress the 1 H-1 H homonuclear dipolar broadenings which is inversely proportional to the MAS rate 5, 6,7,8,9,10 . Therefore, in the recent past, there has been a constant effort by several research groups including NMR spectrometer developers like JEOL and Bruker to develop fast MAS probes.…”

Section: Introductionmentioning

confidence: 99%

Fast magic-angle sample spinning solid-state NMR at 60–100 kHz for natural abundance samples

Nishiyama

2016

Solid State Nuclear Magnetic Resonance

126

239

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Section: Introductionmentioning

confidence: 99%

Fast magic-angle sample spinning solid-state NMR at 60–100 kHz for natural abundance samples

Nishiyama

2016

Solid State Nuclear Magnetic Resonance

126

239

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“…During the last 10-15 years there have been several encyclopedic and review articles covering MAS technology (see, e.g., [31][32][33][34]). The quest for increasing spinning speeds is also well documented, for example in Refs.…”

Section: Introductionmentioning

confidence: 99%

Fluid flow dynamics in MAS systems

Wilhelm

Purea

Engelke

2015

Journal of Magnetic Resonance

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“…In Figs.S2 to S9 (except Fig.S7), the MAS frequency was nR = 60 kHz for all recoupling sequences. This MAS frequency is accessible using rotor with an outer diameter of 1.3 mm and is generally required to achieve high resolution for the 1 H spectra without the use of 1 H-1 H dipolar decoupling sequence [71]. In Fig.7 27 Al CT-selective long pulses had to be used.…”

Section: Iii1 Simulation Parametersmentioning

confidence: 99%

“…Such decrease stems notably from the larger 1 H offset and CSA at high field. It can be desirable to transfer the magnetization of protons to half-integer spin quadrupolar nuclei at fast MAS, which improves the 1 H resolution by averaging out the 1 H-1 H dipolar couplings [71]. Fast MAS also enhances by a factor of 3 to 4 the spectral resolution of half-integer spin quadrupolar nuclei subject to large quadrupole interactions by separating the spinning sidebands from the center-band [87].…”

Section: R18 "mentioning

confidence: 99%

Magnetization transfer from protons to quadrupolar nuclei in solid-state NMR using PRESTO or dipolar-mediated refocused INEPT methods

Giovine

Trébosc

Pourpoint

et al. 2019

Journal of Magnetic Resonance

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In solid-state NMR spectroscopy, the through-space transfer of magnetization from protons to quadrupolar nuclei is employed to probe proximities between those isotopes. Furthermore, such transfer, in conjunction with Dynamic Nuclear Polarization (DNP), can enhance the NMR sensitivity of quadrupolar nuclei, as it allows the transfer of DNP-enhanced 1 H polarization to surrounding nuclei. We compare here the performances of two approaches to achieve such transfer: PRESTO (Phase-shifted Recoupling Effects a Smooth Transfer of Order), which is currently the method of choice to achieve the magnetization transfer from protons to quadrupolar nuclei and which has been shown to supersede Cross-Polarization under Magic-Angle Spinning (MAS) for quadrupolar nuclei and D-RINEPT (Dipolar-mediated Refocused Insensitive Nuclei Enhanced by Polarization Transfer) using symmetry-based SR4 ! " recoupling, which has already been employed to transfer the magnetization in the reverse way from half-integer quadrupolar spin to protons. We also test the PRESTO sequence with R16 # $ %recoupling using 270090180 composite π-pulses as inversion elements. This recoupling scheme, which has previously been proposed to reintroduce 1 H Chemical Shift Anisotropy (CSA) at high MAS frequencies with high robustness to rf-field inhomogeneity, has not so far been employed to reintroduce dipolar couplings with protons. These various techniques to transfer the magnetization from protons to quadrupolar nuclei are analyzed using (i) an average Hamiltonian theory, (ii) numerical simulations of spin dynamics, and (iii) experimental 1 H ® 27 Al and 1 H ® 17 O transfers in as-synthesized AlPO4-14 and 17 O-labelled fumed silica, respectively. The experiments and simulations are done at two magnetic fields (9.4 and 18.8 T) and several spinning speeds (15, 18-24 and 60 kHz). This analysis indicates that owing to its gencoded character, PRESTO yields the highest transfer efficiency at low magnetic fields and MAS frequencies, whereas owing to its higher robustness to rf-field inhomogeneity and chemical shifts, D-RINEPT is more sensitive at high fields and MAS frequencies, notably for protons exhibiting large offset or CSA, such as those involved in hydrogen bonds.

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Ultrafast Magic Angle Spinning Nuclear Magnetic Resonance

Cited by 44 publications

References 145 publications

Fast magic-angle sample spinning solid-state NMR at 60–100 kHz for natural abundance samples

Fast magic-angle sample spinning solid-state NMR at 60–100 kHz for natural abundance samples

Fluid flow dynamics in MAS systems

Magnetization transfer from protons to quadrupolar nuclei in solid-state NMR using PRESTO or dipolar-mediated refocused INEPT methods

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