Molecular Mechanism of Crystalline-to-Amorphous Conversion of Pharmaceutical Solids from 19F Magic Angle Spinning NMR

2020 ◽  
Vol 124 (25) ◽  
pp. 5271-5283 ◽  
Author(s):  
Xingyu Lu ◽  
Chengbin Huang ◽  
Mingyue Li ◽  
Daniel Skomski ◽  
Wei Xu ◽  
...  
Keyword(s):  
Molecular Mechanism ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Pharmaceutical Solids ◽  
Angle Spinning

Three-Dimensional NMR Spectroscopy of Fluorinated Pharmaceutical Solids under Ultrafast Magic Angle Spinning

2019 ◽  
Vol 91 (9) ◽  
pp. 6217-6224 ◽  
Author(s):  
Xingyu Lu ◽  
Daniel Skomski ◽  
Karen C. Thompson ◽  
Michael J. McNevin ◽  
Wei Xu ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Three Dimensional ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Pharmaceutical Solids ◽  
Angle Spinning

Pulse Shaped Dynamic Nuclear Polarization Under Magic Angle Spinning

2019 ◽  
Author(s):  
ASIF EQUBAL ◽  
Kan Tagami ◽  
Songi Han
Keyword(s):  
Electron Spin ◽  
Lattice Relaxation ◽  
Magic Angle Spinning ◽  
Spin Lattice Relaxation ◽  
Magic Angle ◽  
Total Electron ◽  
Spin Lattice ◽  
Maximum Benefit ◽  
Selective Saturation ◽  
Angle Spinning

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.

High Resolution Magic Angle Spinning NMR in Combinatorial Chemistry

2001 ◽  
Vol 4 (4) ◽  
pp. 333-351 ◽  
Author(s):  
G. Lippens ◽  
R. Warrass ◽  
J. Wieruszeski ◽  
P. Rousselot-Pailley ◽  
G. Chessari
Keyword(s):  
High Resolution ◽  
Combinatorial Chemistry ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Angle Spinning

Wideline 2H -NMR Spectroscopy and Imaging of Solids

1994 ◽  
Vol 49 (1-2) ◽  
pp. 19-26 ◽  
Author(s):  
B. Blümich
Keyword(s):  
Nmr Spectroscopy ◽  
Excitation Power ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
2H Nmr ◽  
Stochastic Excitation ◽  
2H Nmr Spectroscopy ◽  
Spatially Inhomogeneous ◽  
Recent Developments ◽  
Angle Spinning

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.

scholarly journals Preparation of Li3PS4–Li3PO4 Solid Electrolytes by Liquid-Phase Shaking for All-Solid-State Batteries

2021 ◽  
Vol 2 (1) ◽  
pp. 39-48
Author(s):  
Nguyen H. H. Phuc ◽  
Takaki Maeda ◽  
Tokoharu Yamamoto ◽  
Hiroyuki Muto ◽  
Atsunori Matsuda
Keyword(s):  
Solid Solution ◽  
Solid State ◽  
Liquid Phase ◽  
Room Temperature ◽  
Reaction Medium ◽  
Magic Angle Spinning ◽  
Resonance Spectroscopy ◽  
Synthesis Methods ◽  
Magic Angle ◽  
Angle Spinning

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.

Magic Angle Spinning NMR Study on Inversion Behavior and Vacancy Disorder in Alumina-Rich Spinel

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