scholarly journals Solid State NMR: A Powerful Tool for the Characterization of Borophosphate Glasses

Molecules ◽  
2020 ◽  
Vol 25 (2) ◽  
pp. 428 ◽  
Author(s):  
Grégory Tricot ◽  
Lazzat Alpysbay ◽  
Bertrand Doumert
Keyword(s):  
Solid State ◽  
Quantum Coherence ◽  
Glass Structure ◽  
Magic Angle Spinning ◽  
Mas Nmr ◽  
Local Order ◽  
Magic Angle ◽  
Multiple Quantum ◽  
Borophosphate Glasses ◽  
Heteronuclear Multiple Quantum Coherence

This review will show how solid state nuclear magnetic resonance (NMR) has contributed to a better understanding of the borophosphate glass structure. Over the last fifteen years, 1D and 2D magic angle spinning (MAS)-NMR has been used to produce key information about both local and medium range organization in this type of glass. After a brief presentation on borophosphate glasses, the paper will focus on the description of the local order of phosphate and borate species obtained by 1D 31P-and 11B-MAS-NMR experiments, with a special emphasis on the improvements obtained at high magnetic fields on the borate speciation description. The last part of this review will show how correlation NMR provided new insights into the intermediate length scale order. Special attention will be paid to the quantitative data retrieved from 11B/31P REDOR-based NMR sequences and to the qualitative connectivity schemes observed on the 2D 11B/31P maps edited with the heteronuclear multiple quantum coherence (HMQC) NMR techniques.

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.

Investigation of Lead Borosilicate Glass Structure With 207Pb and 11B Solid-State NMR

2000 ◽  
Vol 658 ◽  
Author(s):  
James M. Gibson ◽  
Frederick G. Vogt ◽  
Amy S. Barnes ◽  
Karl T. Mueller
Keyword(s):  
Solid State ◽  
Structural Information ◽  
Structural Parameters ◽  
Glass Structure ◽  
Active Role ◽  
Magic Angle Spinning ◽  
Lead Content ◽  
Magic Angle ◽  
Multiple Quantum ◽  
Borosilicate Glasses

ABSTRACTA series of three lead borosilicate glasses were synthesized and analyzed for structural information with both 11B and 207Pb solid-state nuclear magnetic resonance (NMR) spectroscopic methods. Results showed that increasing lead content caused lead to take a more active role in the network as a former and that the populations in these sites can be approximately quantified. 207Pb phase-adjusted-spinning sidebands (PASS), 11B magic-angle spinning (MAS), and 11B multiple-quantum MAS (MQMAS) experiments were used to determine structural parameters for the two nuclei. The 207Pb PASS experiment showed that at higher lead content, more covalent bonding was present. This principle was demonstrated in both an overall shift of the spectral resonances and a quantitative change in site ratios. The 11B MAS experiment showed that the ratio of BO3 to BO4 units was dependent on the amount of lead and boron, consistent with previous studies. Preliminary 11B MQMAS experiments failed to detect any BO3– units, previously hypothesized to exist in this system.

Solid-state 17O NMR Study of Small Biological Compounds

2007 ◽  
Vol 62 (11) ◽  
pp. 1422-1432 ◽  
Author(s):  
Kazuhiko Yamada ◽  
Tadashi Shimizu ◽  
Yoshida Mitsuru ◽  
Miwako Asanuma ◽  
Masataka Tansho ◽  
...  
Keyword(s):  
Solid State ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Multiple Quantum ◽  
Peptide Analysis ◽  
17O Nmr ◽  
Nmr Study ◽  
Biological Compounds ◽  
Nmr Tensors ◽  
Angle Spinning

We present a systematic experimental and theoretical investigation of the oxygen chemical shielding and electric-field-gradient tensors in polycrystalline amino acids and a peptide. Analysis of the 17O magic-angle-spinning (MAS), multiple-quantum MAS, and stationary nuclear magnetic resonance (NMR) spectra yield the magnitudes and the relative orientations between the two NMR tensors. The obtained 17O NMR parameters are sensitive to the hydrogen bond environments. We also demonstrate that solid-state 17O NMR is potentially useful for studying the secondary structures of peptides and proteins.

X-ray diffraction and solid-state 119Sn CP-MAS NMR studies of some triaryltin(IV) chlorides

2003 ◽  
Vol 81 (11) ◽  
pp. 1187-1195 ◽  
Author(s):  
Jordan M Geller ◽  
Ian S Butler ◽  
Denis FR Gilson ◽  
Frederick G Morin ◽  
Ivor Wharf ◽  
...  
Keyword(s):  
Solid State ◽  
Chemical Shift ◽  
Magic Angle Spinning ◽  
Mas Nmr ◽  
Spin Coupling ◽  
Magic Angle ◽  
X Ray ◽  
Tin Chloride ◽  
Angle Spinning ◽  
Spin Spin Coupling

The solid-state 119Sn cross-polarization (CP) magic angle spinning (MAS) NMR spectra of a series of triaryltin chlorides of the form Ar3SnCl have been acquired. The indirect spin-spin coupling constants (J(119Sn-35Cl)), quadrupolar-dipolar shifts (d(119Sn-35Cl)), and the 119Sn chemical shift tensors were extracted. For the spectrum of triphenyltin chloride (I) the validity of the first-order perturbation approximation was tested by comparing results of both the perturbation and cubic-equation approaches and a variable-temperature NMR study undertaken to investigate the influence of the previously reported molecular motion in the solid. The X-ray crystal structures of the tris(o-tolyl)tin chloride (II) and tris(p-tolyl)tin chloride (IV) complexes have been examined. They belong to the monoclinic and triclinic space groups P21/n and P[Formula: see text], respectively, which are different from the previously reported tris(m-tolyl)tin chloride (III) complex, which crystallizes in the space group R3 and has threefold molecular symmetry. The structures and NMR properties of the complexes with meta-substituents are quite different from those with ortho- or para-substituents having axially symmetric shift tensors with small spans and larger J values.Key words: aryltin chlorides, magic angle spinning NMR, tin-chlorine spin-spin coupling, 119Sn chemical shift tensor, crystal structure.

23Na magic-angle spinning and double-rotation NMR study of solid forms of sodium valproate

2014 ◽  
Vol 92 (1) ◽  
pp. 9-15 ◽  
Author(s):  
Nuiok M. Dicaire ◽  
Frédéric A. Perras ◽  
David L. Bryce
Keyword(s):  
Solid State ◽  
Sodium Valproate ◽  
Nmr Spectra ◽  
Structural Information ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Multiple Quantum ◽  
Asymmetric Unit ◽  
Nmr Study ◽  
Angle Spinning

Sodium valproate is a pharmaceutical with applications in the treatment of epilepsy, bipolar disorder, and other ailments. Sodium valproate can exist in many hydrated and acid-stabilized forms in the solid state, and it can be difficult to obtain precise structural information about many of these. Here, we present a 13C and 23Na solid-state NMR study of several forms of sodium valproate, only one of which has been previously structurally characterized by single-crystal X-ray diffraction. 23Na magic-angle spinning (MAS), double-rotation (DOR), and multiple-quantum magic-angle spinning (MQMAS) NMR spectra are shown to provide useful information on the number of molecules in the asymmetric unit, the local coordination geometry of the sodium cations, and the presence of amorphous phases. Two previously identified forms are shown to be highly similar, or identical, according to the 23Na NMR data. The utility of carrying out both DOR and MQMAS NMR experiments to identify all crystallographically unique sites is demonstrated. 13C cross-polarization MAS NMR spectra also provide complementary information on the number of molecules in the asymmetric unit and the crystallinity of the sample.

scholarly journals A novel multinuclear solid-state NMR approach for the characterization of kidney stones

2021 ◽  
Vol 2 (2) ◽  
pp. 653-671
Author(s):  
César Leroy ◽  
Laure Bonhomme-Coury ◽  
Christel Gervais ◽  
Frederik Tielens ◽  
Florence Babonneau ◽  
...  
Keyword(s):  
Solid State ◽  
Kidney Stones ◽  
Solid State Nmr ◽  
Magic Angle Spinning ◽  
Mas Nmr ◽  
Magic Angle ◽  
Nmr Studies ◽  
Stone Composition ◽  
Analytical Technique ◽  
Nmr Data

Abstract. The spectroscopic study of pathological calcifications (including kidney stones) is extremely rich and helps to improve the understanding of the physical and chemical processes associated with their formation. While Fourier transform infrared (FTIR) imaging and optical/electron microscopies are routine techniques in hospitals, there has been a dearth of solid-state NMR studies introduced into this area of medical research, probably due to the scarcity of this analytical technique in hospital facilities. This work introduces effective multinuclear and multidimensional solid-state NMR methodologies to study the complex chemical and structural properties characterizing kidney stone composition. As a basis for comparison, three hydrates (n=1, 2 and 3) of calcium oxalate are examined along with nine representative kidney stones. The multinuclear magic angle spinning (MAS) NMR approach adopted investigates the 1H, 13C, 31P and 31P nuclei, with the 1H and 13C MAS NMR data able to be readily deconvoluted into the constituent elements associated with the different oxalates and organics present. For the first time, the full interpretation of highly resolved 1H NMR spectra is presented for the three hydrates, based on the structure and local dynamics. The corresponding 31P MAS NMR data indicates the presence of low-level inorganic phosphate species; however, the complexity of these data make the precise identification of the phases difficult to assign. This work provides physicians, urologists and nephrologists with additional avenues of spectroscopic investigation to interrogate this complex medical dilemma that requires real, multitechnique approaches to generate effective outcomes.

scholarly journals t1-Noise eliminated dipolar heteronuclear multiple-quantum coherence solid-state NMR spectroscopy

2020 ◽  
Vol 22 (36) ◽  
pp. 20815-20828 ◽  
Author(s):  
Amrit Venkatesh ◽  
Xuechen Luan ◽  
Frédéric A. Perras ◽  
Ivan Hung ◽  
Wenyu Huang ◽  
...  
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Quantum Correlation ◽  
Quantum Coherence ◽  
Pulse Sequences ◽  
Multiple Quantum ◽  
Heteronuclear Correlation ◽  
Heteronuclear Multiple Quantum Coherence ◽  
Multiple Quantum Coherence ◽  
Nuclear Magnetic Resonance Pulse

t1-Noise eliminated (TONE) heteronuclear multiple quantum correlation (HMQC) solid-state nuclear magnetic resonance pulse sequences improve the sensitivity of 2D 1H{X} heteronuclear correlation experiments with X = 17O, 25Mg, 27Al and 35Cl.

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