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Solid State Nuclear Magnetic Resonance

Nghia Tuan Duong, Yusuke Nishiyama
Recent study has demonstrated the application of the proton-detected heteronuclear multi-quantum coherence (HMQC) at ultrafast Magic Angle Spinning (MAS) to probe quadrupolar nuclei including (14)N and (35)Cl. In addition, for half-integer quadrupolar nucleus like (35)Cl, the quadrupolar product can be calculated based on the shift difference between the center band of satellite transition (ST) and the central transition (CT) peaks. The applicability of this technique is further investigated on spin I=5/2, namely (27)Al nucleus, and kaolin is chosen as the testing sample...
January 4, 2017: Solid State Nuclear Magnetic Resonance
Christophe Odin
The aim of this work is to generalize the Ernst-Anderson model developed to account of the steady-state regime of isolated spins I=1/2 subject to a train of strictly identical pulse sequences separated by free evolution periods of same duration. We generalize this model to the general case of spins I≥1 and general pulse sequence within the framework of the Liouville space. In particular, it is proved that under reasonable assumptions, a well defined steady-state regime is reached which is independent of the initial conditions...
December 29, 2016: Solid State Nuclear Magnetic Resonance
Charlotte Martineau-Corcos, Jiri Dědeček, Francis Taulelle
In this paper, we review and illustrate applications, reported in the literature or used in our group, of (27)Al-(27)Al double-quantum single-quantum (DQ-SQ) MAS NMR experiments for the structural characterization of Al-containing microporous solids, namely zeolites, aluminophosphates and metal-organic frameworks. Information regarding the periodic frameworks or the localization of the various aluminum species in the materials are obtained from the analysis of the two-dimensional NMR spectra, which allows getting local structural details sometimes inaccessible from other characterization technique...
December 28, 2016: Solid State Nuclear Magnetic Resonance
Xianqi Kong, Yizhe Dai, Gang Wu
We report synthesis and solid-state (17)O NMR characterization of four site-specifically (17)O-labeled 2-acylbenzoic acids (2-RC(O)C6H4COOH) where R=H and CH3): 2-[3-(17)O]formylbenzoic acid, 2-[1,2-(17)O2]formylbenzoic acid, 2-[3-(17)O]acetylbenzoic acid, and 2-[1,2,3-(17)O3]acetylbenzoic acid. In the solid state, both 2-formyl- and 2-acetyl-benzoic acids exist as the cyclic phthalide form each containing a five-membered lactone ring and a cyclic hemiacetal/hemiketal group. Static and magic-angle-spinning (17)O NMR spectra were recorded at 14...
December 27, 2016: Solid State Nuclear Magnetic Resonance
M Bashi, H A Rahnamaye Aliabad, A A Mowlavi, Iftikhar Ahmad
We have calculated Nuclear Magnetic Resonance (NMR) spectroscopy for (127)I (quadrupolar nuclei I=5/2) in binary metal iodides XI (X=Li, Na, K, Rb and Cs) by using PBE- GGA, YS- PBE0 and mBJ exchange correlation potentials. The results show that the nature of bonds between Iodine and metal atoms are ionic. The main contribution in NMR spectroscopy is related to the induced current inside the atomic sphere and the remainder of the unit cell volume contributes only a few ppm. Obtained NMR shifts are compared with the NMR shielding data and the NMR shielding for metal-p band varies across the series about 221ppm...
December 23, 2016: Solid State Nuclear Magnetic Resonance
Baudouin Dillmann, Luc Dubois, Erick Paleczny, Julien Trébosc, Jean-Paul Amoureux, Frédérique Pourpoint, Olivier Lafon
The development of probes for Nuclear Magnetic Resonance (NMR) spectroscopy of metabolites, biomolecules or materials requires the accurate determination of the radio-frequency (RF) magnetic field strength, B1, at the position of the sample since this RF-field strength is related to the signal sensitivity and the excitation bandwidth. The Ball Shift (BS) technique is a commonly employed test bench method to measure the B1 value. Nevertheless, the influence of the RF electric field, E1, on BS is often overlooked...
December 18, 2016: Solid State Nuclear Magnetic Resonance
Sarra Aissani, Laouès Guendouz, Pierre-Louis Marande, Daniel Canet
Until now, NQR imaging has been considered mainly in the case of Chlorine-35. This is a spin 3/2 resonating at relatively high frequency (around 30MHz) thus affording a favorable sensitivity. Conversely, Nitrogen-14 (spin 1) NQR is much less sensitive because its resonances frequencies are below 6MHz. In contrast to already existing methodologies for object localization by (14)N NQR, we present here a new, more straightforward, approach and the principles of space dependent (14)N Quadrupole Resonance are laid down...
December 16, 2016: Solid State Nuclear Magnetic Resonance
Ivan Hung, Gang Wu, Zhehong Gan
NMR spectroscopy is a powerful tool for probing molecular dynamics. For the classic case of two-site exchange, NMR spectra go through the transition from exchange broadening through coalescence and then motional narrowing as the exchange rate increases passing through the difference between the resonance frequencies of the two sites. For central-transition spectra of half-integer quadrupolar nuclei in solids, line shape change due to molecular dynamics occurs in two stages. The first stage occurs when the exchange rate is comparable to the second-order quadrupolar interaction...
December 10, 2016: Solid State Nuclear Magnetic Resonance
Rupal Gupta, Wenlin Huang, Lynn C Francesconi, Tatyana Polenova
We examined the positional isomerism and vanadium substitution on the (51)V magic angle spinning NMR spectra of potassium salts of vanadium-substituted polyoxotungstates of the Wells-Dawson series. NMR parameters of this class of catalytically active polyoxotungstates effect of are reported. Multiple species, indicative of differences in the local environment at the substitution sites, are observed in solid-state NMR spectra of the di- and tri- substituted complexes in contrast to solution NMR spectra, where single average chemical shift was observed...
December 10, 2016: Solid State Nuclear Magnetic Resonance
Andreas Brinkmann, Luke A O'Dell
Numerically exact simulations of the (14)N overtone ((14)N(OT)) MAS NMR experiment are used to investigate the effects of the applied magnetic field strength as well as three types of excitation pulse. The results show that both the resolution and sensitivity of (14)N(OT) MAS NMR increase linearly with the applied static magnetic field strength. Standard RF excitation pulses are compared with frequency-swept WURST pulses as well as several composite pulses. WURST pulses are demonstrated to provide the largest bandwidths, while the direction of the frequency sweep is shown to be important when these pulses are used for the direct observation of (14)N(OT) signals...
December 10, 2016: Solid State Nuclear Magnetic Resonance
Libor Kobera, Scott A Southern, Jamie M Frost, David L Bryce
Carboxylate paddlewheels and their oxo-bridged analogues constitute ideal building blocks for the assembly of two- and three-dimensional framework materials. Here, we present a multinuclear ((1)H, (13)C, (93)Nb, (95)Mo) magnetic resonance study of solid samples of Nb2OCl6(O2Ph)2 (1), Mo2(O2CMe)4 (2), and Mo2(O2CCHF2)4 (3). High-resolution proton and (13)C CP/MAS NMR spectra provide valuable information on structure and crystal symmetry and on cocrystallized solvent. (93)Nb solid-state NMR spectra of 1 provide quadrupolar coupling constants and chemical shift tensors which are characteristic of the axially asymmetric Nb-O-Nb bridging environment...
December 7, 2016: Solid State Nuclear Magnetic Resonance
Smita Odedra, Stephen Wimperis
Spin-locking of spin I=3/2 and I=5/2 nuclei in the presence of large resonance offsets has been studied using both approximate and exact theoretical approaches and, in the case of I=3/2, experimentally. We show the variety of coherences and population states produced in a far off-resonance spin-locking NMR experiment (one consisting solely of a spin-locking pulse) and how these vary with the radiofrequency field strength and offset frequency. Under magic angle spinning (MAS) conditions and in the "adiabatic limit", these spin-locked states acquire a time dependence...
November 30, 2016: Solid State Nuclear Magnetic Resonance
Aneta Woźniak-Braszak
Molecular dynamics of the solid 3-(trifluoromethyl) benzoic acid containing proton (1)H and fluorine (19)F nuclei was explored by the solid-state NMR off - resonance technique. Contrary to the previous experiments the proton nuclei system I relaxed in the off - resonance effective field B→e while fluorine nuclei system S was saturated for short time in comparison to the relaxation time T1I. New cross - relaxation solid - state NMR off - resonance experiments were conducted on a homebuilt pulse spectrometer operating at the on-resonance frequency of 30...
February 2017: Solid State Nuclear Magnetic Resonance
Marko Bertmer
Solid-state NMR (SSNMR) experiments are mainly performed on diamagnetic materials. However, the study of paramagnetic materials offers access to additional information in combination with the unpaired electron. This article discusses the experimental complications arising when considering paramagnetic materials such as large shift effects and large linewidths. A look at the theoretical description as well as experimental methods are shown and accompanied by techniques for signal assignment, also with the help of quantum-chemical calculations...
February 2017: Solid State Nuclear Magnetic Resonance
Colan E Hughes, Kenneth D M Harris
Two new methods for calculating lineshapes in solid-state NMR spectra are described. The first method, which we refer to as semi-analytical, allows the rapid calculation of quadrupolar central-transition lineshapes in both static and magic-angle spinning cases. The second method, which is fully numerical, allows the calculation of lineshapes resulting from any combination of interactions, including quadrupolar, dipolar and chemical shift anisotropy, and is not restricted to cases in which the principal axis systems for the different interactions are aligned...
November 2016: Solid State Nuclear Magnetic Resonance
J W Zwanziger
The assumptions underlying the popular projector-augmented wave (PAW) method of computing electronic structure in solids are examined, with primary attention to the computation of NMR observables. In particular, the assumption of non-overlapping PAW spheres is studied, and it is shown that when the spheres do overlap, the errors may be significant and furthermore are of unpredictable sign. Examples are provided by comparing PAW-based calculations with and without overlapping spheres, with the highly accurate all-electron linear augmented wave method...
November 2016: Solid State Nuclear Magnetic Resonance
Lei Zhou, Shenhui Li, Guodong Qi, Yongchao Su, Jing Li, Anmin Zheng, Xianfeng Yi, Qiang Wang, Feng Deng
The carbonylation of methanol with carbon monoxide to generate methyl acetate over Cu-H-MOR and H-MOR zeolites is studied using solid-state NMR spectroscopy. It is found that the catalytic activity of Cu-H-MOR zeolite is much higher than that of H-MOR zeolite. The presence of Cu(+) species enables the stabilization of dimethyl ether, which efficiently suppresses the hydrocarbon formation during carbonylation process over Cu-H-MOR zeolite. In addition, the carbon monoxide adsorbed on Cu(+) site is not an active species to produce either methyl acetate or acetic acid...
November 2016: Solid State Nuclear Magnetic Resonance
S Greiser, M Hunger, C Jäger
(29)Si{(27)Al} TRAPDOR MAS NMR was applied to two faujasite-type zeolites with Si/Al ratios of 1.3 (Na-X) and 2.7 (Na-Y). The aim of this test study is to show that different Q(4)(mAl) sites (m =4, 3, 2, 1) can be distinguished by differently strong TRAPDOR effects (ΔS/S0). Indeed, it was found that the TRAPDOR effect depends on the number m of AlO4 units connected to the Q(4) silicon tetrahedrons. For Na-X, the measured ΔS/S0 values are 1 : 0.81 : 0.56 for Q(4)(4Al), Q(4)(3Al) and Q(4)(2Al), respectively (normalized to Q(4)(4Al))...
October 8, 2016: Solid State Nuclear Magnetic Resonance
Ryan J McCarty, Jonathan F Stebbins
This paper demonstrates the approach of using paramagnetic effects observed in NMR spectra to investigate the distribution of lanthanide dopant cations in YAG (yttrium aluminum garnet, Y3Al5O12) optical materials, as a complimentary technique to optical spectroscopy and other standard methods of characterization. We investigate the effects of Ce(3+), Nd(3+), Yb(3+), Tm(3+), and Tm(3+)-Cr(3+) on (27)Al and (89)Y NMR spectra. We note shifted resonances for both AlO4 and AlO6 sites. In some cases, multiple shifted peaks are observable, and some of these can be empirically assigned to dopant cations in known configurations to the observed nuclides...
October 6, 2016: Solid State Nuclear Magnetic Resonance
Brendan W Wilson, Arlo A Parker, Terry Gullion
The measurement of the dipolar interaction between two spins provides the distance between nuclei. A better structural picture emerges when the distance is combined with the orientation of the internuclear vector in the principal axis system of the chemical shift anisotropy tensor. The SEDOR experiment is used on a static sample of alanine to show that the orientation of the vector connecting the nitrogen and carboxylate carbon nuclei can be accurately determined in the CSA PAS of the (13)C carboxylate spin...
September 20, 2016: Solid State Nuclear Magnetic Resonance
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