Quantitative determination of the phosphorus environment in lithium aluminosilicate glasses using solid-state NMR techniques

2019 ◽  
Vol 21 (33) ◽  
pp. 18370-18379
Author(s):  
Pauline Glatz ◽  
Monique Comte ◽  
Lionel Montagne ◽  
Bertrand Doumert ◽  
Laurent Cormier
Keyword(s):  
Solid State Nmr ◽  
Quantum Coherence ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Multiple Quantum ◽  
Aluminosilicate Glasses ◽  
Nmr Techniques ◽  
Angle Spinning ◽  
Multiple Quantum Coherence

The phosphorus environment is determined quantitatively using 31P Magic Angle Spinning NMR constrained by 31P–27Al Multiple-Quantum Coherence-based NMR techniques.

Determination of Phase Content in Multiphase Polymers by Solid-State NMR Techniques

2012 ◽  
Vol 714 ◽  
pp. 51-56 ◽  
Author(s):  
Antonio Martínez-Richa ◽  
Regan Silvestri
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Magic Angle Spinning ◽  
Polymer Chains ◽  
Magic Angle ◽  
Aliphatic Polyesters ◽  
Polymer Systems ◽  
Nmr Techniques ◽  
Angle Spinning

Solid-state nuclear magnetic resonance (NMR) spectroscopy has emerged as a relatively facile technique for the characterization of multi-component polymer systems. In particular, it has emerged to be a useful technique for probing the molecular structure, conformation and dynamics of polymer chains at interfaces between phases in various types of multi-component polymer systems including nanomaterials. The usefulness of solid-state NMR stems from its ability to non-destructively probe not only the bulk of the polymer, but moreover its ability to selectively probe the interface or interphase. As such, the technique has been extensively exploited in the study of multi-component polymer systems. To achieve13C spectral resolution in the solid-state magic angle spinning (MAS), dipolar decoupling and cross-polarization are applied which enables the study of individual carbon atoms directly with excellent resolution and sensitivity. Some examples of applications of this technique to the study of multiphase aliphatic polyesters are reviewed herein.

scholarly journals Combination of solid state NMR and DFT calculation to elucidate the state of sodium in hard carbon electrodes

2016 ◽  
Vol 4 (34) ◽  
pp. 13183-13193 ◽  
Author(s):  
Ryohei Morita ◽  
Kazuma Gotoh ◽  
Mika Fukunishi ◽  
Kei Kubota ◽  
Shinichi Komaba ◽  
...  
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Dft Calculation ◽  
Magic Angle Spinning ◽  
The State ◽  
Mas Nmr ◽  
Magic Angle ◽  
Multiple Quantum ◽  
Hard Carbon ◽  
Angle Spinning

We examined the state of sodium electrochemically inserted in HC prepared at 700–2000 °C using solid state Na magic angle spinning (MAS) NMR and multiple quantum (MQ) MAS NMR.

Determination of methyl order parameters using solid state NMR under off magic angle spinning

2019 ◽  
Vol 73 (8-9) ◽  
pp. 471-475 ◽  
Author(s):  
Kai Xue ◽  
Salvatore Mamone ◽  
Benita Koch ◽  
Riddhiman Sarkar ◽  
Bernd Reif
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Magic Angle Spinning ◽  
Order Parameters ◽  
Magic Angle ◽  
Angle Spinning

scholarly journals Materials Characterisation by Nuclear Quadrupole Interaction

1994 ◽  
Vol 49 (1-2) ◽  
pp. 320-328 ◽  
Author(s):  
T.J. Bastow
Keyword(s):  
Solid State Nmr ◽  
Materials Science ◽  
Spin Echo ◽  
Nuclear Quadrupole Interaction ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Quadrupole Coupling ◽  
Nmr Techniques ◽  
Nuclear Quadrupole ◽  
Angle Spinning

Abstract The power of solid state NMR to characterise solids by determining the nuclear quadrupole coupling of the constituent nuclei is demonstrated for a number of com pounds of current interest in a materials science laboratory. Recent results are presented for the nuclei 17O , 23Na, 27Al, 39K, 71Ga, 91Zr, 93Nb, and 139La. These were derived using a variety of FT NMR techniques including static, magic angle spinning and frequency stepped spin echo NMR spectroscopy.

High sensitivity and resolution in 43Ca solid-state NMR experiments

2015 ◽  
Vol 93 (8) ◽  
pp. 799-807 ◽  
Author(s):  
Kevin M.N. Burgess ◽  
Frédéric A. Perras ◽  
Igor L. Moudrakovski ◽  
Yijue Xu ◽  
David L. Bryce
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Nmr Spectra ◽  
High Sensitivity ◽  
Magic Angle Spinning ◽  
Signal Enhancement ◽  
Magic Angle ◽  
Multiple Quantum ◽  
Central Transition ◽  
Angle Spinning

A thorough investigation of solid-state NMR signal enhancement schemes and high-resolution techniques for application to the spin-7/2 43Ca nuclide are presented. Signal enhancement experiments employing double frequency sweeps, hyperbolic secant pulses, and rotor-assisted population transfer, which manipulate the satellite transitions of half-integer quadrupolar nuclei to polarize the central transition (m = + 1/2 ↔ –1/2), are carried out on four well-characterized 43Ca isotopically enriched calcium salts: Ca(NO3)2, Ca(OD)2, CaSO4·2H2O, and Ca(OAc)2·H2O. These results, in conjunction with numerical simulations of 43Ca NMR spectra under magic-angle spinning conditions, are used to identify the technique that provides the most uniform (or quantitative) polarization enhancement as well as the largest signal enhancement factors independent of size of the 43Ca quadrupolar coupling constant, which is the most significant source of resonance broadening in 43Ca NMR spectra. These samples are further investigated using 43Ca double-rotation NMR spectroscopy to yield isotropic, or solution-like, NMR spectra with exquisite resolution. In addition, three unique calcium sites are resolved for the hemihydrated form of calcium acetate (unknown structure), Ca(OAc)2·0.5H2O, with double-rotation NMR, whereas the more common, but more time-consuming, multiple quantum magic-angle spinning technique only clearly resolves two calcium sites. The results shown herein will be useful for other NMR spectroscopists attempting to acquire 43Ca solid-state NMR data for unknown and more complex materials with a higher degree of both sensitivity and resolution.

Sign in / Sign up

Export Citation Format

Share Document