scholarly journals Dipolar truncation in magic-angle spinning NMR recoupling experiments

2009 ◽  
Vol 130 (11) ◽  
pp. 114506 ◽  
Author(s):  
Marvin J. Bayro ◽  
Matthias Huber ◽  
Ramesh Ramachandran ◽  
Timothy C. Davenport ◽  
Beat H. Meier ◽  
...  
2020 ◽  
Author(s):  
Evgeny Nimerovsky ◽  
Kai Xue ◽  
Kumar Tekwani Movellan ◽  
Loren Andreas

Abstract. Homonuclear finite-pulse radio frequency driven recoupling (fp-RFDR) has been broadly used in multi-dimensional magic-angle spinning (MAS) solid-state NMR experiments over the past 20 years. The theoretical and the simulated descriptions of this method were presented during that time, resulting in an understanding of the influence of chemical shift offset, finite pulse effects, and dipolar truncation. Here we present an operator analysis of both heteronuclear and homonuclear fp-RFDR. By numerical simulation, we show which operators are involved in the longitudinal exchange for both heteronuclear and the well-known homonuclear sequences. This results in a better understanding of the influence of phase cycling of the fp-RFDR pulses, which is typically a variant of XY cycling. We investigate the heteronuclear and homonuclear fp-RFDR signals and evolution of the operators through the fp-RFDR block. We show the convergence of the evolutions of the heteronuclear and homonuclear fp-RFDR signals at even numbers of rotor periods and completely different evolution between them. We demonstrate heteronuclear 1H- 13C and 1H-15N fp-RFDR magnetization transfer using a microcrystalline SH3 sample at 100 kHz MAS.


Author(s):  
ASIF EQUBAL ◽  
Kan Tagami ◽  
Songi Han

In this paper, we report on an entirely novel way of improving the MAS-DNP efficiency by shaped μw pulse train irradiation for fast and broad-banded (FAB) saturation of the electron spin resonance. FAB-DNP achieved with Arbitrary Wave Generated shaped μw pulse trains facilitates effective and selective saturation of a defined fraction of the total electron spins, and provides superior control over the DNP efficiency under MAS. Experimental and quantum-mechanics based numerically simulated results together demonstrate that FAB-DNP significantly outperforms CW-DNP when the EPR-line of PAs is broadened by conformational distribution and exchange coupling. We demonstrate that the maximum benefit of FAB DNP is achieved when the electron spin-lattice relaxation is fast relative to the MAS frequency, i.e. at higher temperatures and/or when employing metals as PAs. Calculations predict that under short T<sub>1e </sub>conditions AWG-DNP can achieve as much as ~4-fold greater enhancement compared to CW-DNP.


2001 ◽  
Vol 4 (4) ◽  
pp. 333-351 ◽  
Author(s):  
G. Lippens ◽  
R. Warrass ◽  
J. Wieruszeski ◽  
P. Rousselot-Pailley ◽  
G. Chessari

1994 ◽  
Vol 49 (1-2) ◽  
pp. 19-26 ◽  
Author(s):  
B. Blümich

Abstract Recent developments, focussing on reduction of the rf excitation power by stochastic excitation, on improvements in sensitivity and excitation bandwidth by magic angle spinning, and on combining wideline spectroscopy with spatial resolution for investigations o f spatially inhomogeneous objects are reviewed.


2021 ◽  
Vol 2 (1) ◽  
pp. 39-48
Author(s):  
Nguyen H. H. Phuc ◽  
Takaki Maeda ◽  
Tokoharu Yamamoto ◽  
Hiroyuki Muto ◽  
Atsunori Matsuda

A solid solution of a 100Li3PS4·xLi3PO4 solid electrolyte was easily prepared by liquid-phase synthesis. Instead of the conventional solid-state synthesis methods, ethyl propionate was used as the reaction medium. The initial stage of the reaction among Li2S, P2S5 and Li3PO4 was proved by ultraviolet-visible spectroscopy. The powder X-ray diffraction (XRD) results showed that the solid solution was formed up to x = 6. At x = 20, XRD peaks of Li3PO4 were detected in the prepared sample after heat treatment at 170 °C. However, the samples obtained at room temperature showed no evidence of Li3PO4 remaining for x = 20. Solid phosphorus-31 magic angle spinning nuclear magnetic resonance spectroscopy results proved the formation of a POS33− unit in the sample with x = 6. Improvements of ionic conductivity at room temperature and activation energy were obtained with the formation of the solid solution. The sample with x = 6 exhibited a better stability against Li metal than that with x = 0. The all-solid-state half-cell employing the sample with x = 6 at the positive electrode exhibited a better charge–discharge capacity than that employing the sample with x = 0.


2018 ◽  
Vol 57 (14) ◽  
pp. 8390-8395 ◽  
Author(s):  
Bingtian Tu ◽  
He Zhang ◽  
Hao Wang ◽  
Weimin Wang ◽  
Zhengyi Fu

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