14N Quadrupole Interactions in Nitrogen-Containing Ceramics. Effects on 29Si NMR Line Shapes and Structural Implications

1992 ◽  
Vol 47 (1-2) ◽  
pp. 39-44 ◽  
Author(s):  
Alejandro Olivieri
Keyword(s):  
Solid State ◽  
Nmr Spectra ◽  
Dipolar Coupling ◽  
Coupling Constants ◽  
Simple Equation ◽  
29Si Nmr ◽  
Experimental Conditions ◽  
Line Shapes ◽  
Quadrupole Interactions ◽  
Quadrupole Coupling

AbstractSimulations of solid-state 29Si NMR spectra in nitrogen-containing silicon ceramics and glasses are described. The range of SiNxO4-x tetrahedra is covered, with emphasis on the experimental conditions needed to observe the effect of the incompletely averaged 29Si, 14N dipolar coupling. A simple equation is discussed concerning its use in the interpretation of these 29Si spectra, including the computation of 14N quadrupole coupling constants with its absolute sign.

scholarly journals High Resolution and Solid State NMR Investigations of Subvalent Gallium Compounds

1986 ◽  
Vol 41 (1-2) ◽  
pp. 315-318 ◽  
Author(s):  
Hubert Schmidbaur ◽  
Theodore Zafiropoulos ◽  
Wolfgang Bublak ◽  
Paul Burkert ◽  
Frank H. Köhler
Keyword(s):  
Solid State ◽  
Nmr Spectra ◽  
Quadrupole Coupling Constant ◽  
Coupling Constant ◽  
Gallium Atom ◽  
Line Shapes ◽  
Quadrupole Coupling ◽  
Structure Determinations ◽  
Constant E ◽  
Gallium Compounds

The 71Ga NMR spectra of Ga[GaX4] melts and of solutions in benzene and other hydrocarbons show discrete sharp GaI and broad GaIII resonances. In the light of recent structure determinations, the solution GaI signals must be attributed to bis(arene)Ga+ complexes in which the gallium atom is η6-bonded to the hydrocarbons. The low line widths and strong high field shifts are attributed to an almost spherical shielding of the metal nucleus by the 4 s2 electrons. Solid state 69Ga and 71Ga NMR spectra of Ga[GaCl4] crystalline powder show only Ga1 resonances. While the 71GaI line is rather narrow, the 69GaI line has a complex fine structure. Consistent with the crystal structure of Ga[GaCl4], the Ga1 ion is calculated to have a very low quadrupole coupling constant e2q Q/h = 1.7 ± 0.1 MHz and an asymmetry parameter η = 0.44. Experimental and simulated line shapes (using literature models) are in satisfactory agreement, implying that the 69Ga signal splitting is due to second order quadrupolar effects for the central m = + 1/2 ⇋ - 1/2 transition. The analogous splitting of the 71Ga NMR line is too small to be detected.

Line-Shape Analyses of Solid-state 17O NMR Spectra for Hexagonal Ice

2014 ◽  
Vol 69 (7) ◽  
pp. 786-792 ◽  
Author(s):  
Kazuhiko Yamada ◽  
Kenzo Deguchi ◽  
Tadashi Shimizu ◽  
Junji Watanabe
Keyword(s):  
Solid State ◽  
Nmr Spectra ◽  
17O Nmr ◽  
Line Shapes ◽  
Quadrupole Interactions ◽  
Isotropic Line ◽  
Hexagonal Ice ◽  
Theoretical Investigations ◽  
Proton Disorder ◽  
Shape Analyses

We present the results of experimental and theoretical investigations of line shapes in solid-state 17O NMR spectra of hexagonal ice, Ih. Stationary 17O NMR spectra of Ih at temperatures from 143 to 280 K were obtained at 11.7 and 16.4 T. Line shapes changed drastically as the temperature was increased from 143 to 243 K; at 253 K and above, pseudo-isotropic line shapes appear, indicating the presence of reorientational motions. We find that Ratcliffe’s model, which involves twelve orientations and four-step jumps for water reorientational motions, is effective for analyzing the NMR spectra at temperatures below 243 K. The present analysis demonstrates that the isotropic line shapes arise from proton disorder with respect to the solid-state 17O NMR time scale, producing pseudoicosahedral motional averaging that can completely average out second-order quadrupole interactions.

Structural and Catalytic Properties of the Alkali Metal Ion-Exchanged Y-Zeolites by 29Si and 27Al Solid-State NMR and FT-IR Spectroscopy

2005 ◽  
Vol 277-279 ◽  
pp. 708-719
Author(s):  
Chang Seop Lee ◽  
Hee Jung Lee ◽  
Sung Woo Choi ◽  
Jahun Kwak ◽  
Charles H.F. Peden
Keyword(s):  
Solid State ◽  
Alkali Metal ◽  
Photoelectron Spectroscopy ◽  
Metal Ion ◽  
Nmr Spectra ◽  
Catalytic Properties ◽  
Nox Reduction ◽  
29Si Nmr ◽  
Y Zeolites ◽  
X Ray

A series of cation exchanged Y-zeolites were prepared by exchanging cations with various alkali (M+, M= Li, Na, K, Cs) metals. The structural and catalytic properties of the alkali metal exchanged Y-zeolites have been investigated by a number of analytical techniques. Comparative elemental analyses were determined by an Energy Dispersive Spectroscopy X-ray (EDS), X-ray Photoelectron Spectroscopy (XPS), Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) and X-ray Fluorescence (XRF) before and after cation substitution. The framework and non-framework Al coordination and the Si/Al ratios of the Y-zeolites were investigated by MAS Solid-State Nuclear Magnetic Resonance (NMR) spectroscopy. The Al NMR spectra were characterized by two 27Al resonance signals at 12 and 59 ppm, indicating the presence of the non-framework and framework Al respectively. The intensities of these resonances were used to monitor the amount of the framework and non-framework Al species in the series of exchanged zeolites. The 29Si NMR spectra were characterized by four resonance signals at -79, -84, -90, and -95 ppm. Changing the alkali metal cations in the exchanged Y-zeolites significantly altered the extent of the octahedral/tetrahedral coordination and the Si/Al ratio. The Fourier Transform Infrared spectra of the CO2 adsorbed on to the exchanged Y-zeolites showed a low frequency shift, as the atomic number of the exchanged alkali metal increased. In addition, the catalytic activity of these samples for NOx reduction were tested in combination with a non-thermal plasma technique and interpreted based on the above structural and spectroscopic information.

NQR Studies of the Structure of Glasses and Crystalline Compounds

1992 ◽  
Vol 47 (1-2) ◽  
pp. 30-38 ◽  
Author(s):  
P. J. Bray ◽  
DongHoon Lee ◽  
De Gen Mao ◽  
G. L. Petersen ◽  
S. A. Feller ◽  
...  
Keyword(s):  
Nuclear Quadrupole Resonance ◽  
Nmr Spectra ◽  
Coupling Constants ◽  
Borate Glasses ◽  
Low Frequencies ◽  
Structure Of Glasses ◽  
Quadrupole Coupling ◽  
Quadrupole Resonance ◽  
Nuclear Quadrupole ◽  
Asymmetry Parameters

AbstractPure nuclear quadrupole resonance (NQR) spectroscopy at low frequencies (down to 275 kHz) has been used to investigate a number of borate, aluminate, and vanadate crystalline compounds and borate glasses. The values of the quadrupole coupling constants (Qcc) and asymmetry parameters (η) are obtained with error limits that are one or two orders of magnitude less than those for values obtained from NMR spectra. New sites, not resolved in NMR spectra, have been detected for boron in borate glasses.

scholarly journals NMR Detection of Oxygen Isotopes in TiO2 Single Crystal

1998 ◽  
Vol 53 (6-7) ◽  
pp. 305-308
Author(s):  
M. Tanigaki ◽  
S. Takeda ◽  
K. Matsuta ◽  
Y. Matsumoto ◽  
T. Minamisono ◽  
...  
Keyword(s):  
Single Crystal ◽  
Quadrupole Moment ◽  
Oxygen Isotopes ◽  
Electric Quadrupole ◽  
Coupling Constants ◽  
Quadrupole Moments ◽  
Quadrupole Interactions ◽  
Quadrupole Coupling ◽  
Nmr Signals

Abstract We studied the electric quadrupole interactions of Oxygen isotopes in a TiO2 single crystal. For 13O and 19O nuclei, quadrupole coupling constants were measured by the β-NMR technique, and for the 17O nucleus the FT-NMR technique was utilized. We synthesized a TiO2 single crystal which was enriched in 17O up to 5 atom % to observe NMR signals without any perturbations from impurities. Using the known quadrupole moment of 17O, EFGs at an O site in TiO2 and the quadrupole moments of 13O and 19O were determined.

The fine structure of high-resolution solid state 29Si NMR spectra of zeolites X and Y

1986 ◽  
Vol 127 (6) ◽  
pp. 563-565 ◽  
Author(s):  
Xinsheng Liu ◽  
Jacek Klinowski ◽  
J.M. Thomas
Keyword(s):  
Fine Structure ◽  
Solid State ◽  
High Resolution ◽  
Nmr Spectra ◽  
29Si Nmr ◽  
29Si Nmr Spectra
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