Search results for "Magic angle"
showing 10 items of 57 documents
Gram-scale selective synthesis of WO3−x nanorods and (NH4)xWO3 ammonium tungsten bronzes with tunable plasmonic properties
2021
Localized surface plasmon resonance properties in unconventional materials like metal oxides or chalcogenide semiconductors have been studied for use in signal detection and analysis in biomedicine and photocatalysis. We devised a selective synthesis of the tungsten oxides WO3-x and (NH4)xWO3 with tunable plasmonic properties. We selectively synthesized WO3-x nanorods with different aspect ratios and hexagonal tungsten bronzes (NH4)xWO3 as truncated nanocubes starting from ammonium metatungstate (NH4)6H2W12O40·xH2O. Both particles form from the same nuclei at temperatures >200 °C; monomer concentration and surfactant ratio are essential variables for phase selection. (NH4)xWO3 was the prefe…
Influence of Whole-Body Dynamics on 15N PISEMA NMR Spectra of Membrane Proteins: A Theoretical Analysis
2009
AbstractMembrane proteins and peptides exhibit a preferred orientation in the lipid bilayer while fluctuating in an anisotropic manner. Both the orientation and the dynamics have direct functional implications, but motions are usually not accessible, and structural descriptions are generally static. Using simulated data, we analyze systematically the impact of whole-body motions on the peptide orientations calculated from two-dimensional polarization inversion spin exchange at the magic angle (PISEMA) NMR. Fluctuations are found to have a significant effect on the observed spectra. Nevertheless, wheel-like patterns are still preserved, and it is possible to determine the average peptide til…
Synthesis, structure and properties of N-acetylated derivatives of methyl 5-amino-1H-[1,2,4]triazole-3-carboxylate.
2004
Methyl 5-amino-1H-[1,2,4]triazole-3-carboxylate hydrochloride (1). and free ester (2). were obtained and 2 was reacted with Ac(2)O to give the acetylated products 3-6. Compounds 1-6 were studied using HPLC, GC-MS, FTIR and multinuclear NMR spectroscopy, including the cross-polarisation magic angle spinning (CPMAS) technique. The results of the acetylation of 2 were compared to those of the acetylation of 5-amino-1H-[1,2,4]triazole, and for 2 a significant decrease in the susceptibility to acetylation was found. The reaction of 2 with Ac(2)O at 20 degrees C, regardless of the amount and the concentration of the latter, including neat Ac(2)O, proceeds fully regioselectively and leads to one p…
Unraveling the packing pattern leading to gelation using SS NMR and X-ray diffraction: direct observation of the evolution of self-assembled fibers
2010
A detailed understanding of the mode of packing patterns that leads to the gelation of low molecular mass gelators derived from bile acid esters was carried out using solid state NMR along with complementary techniques such as powder X-ray diffraction (PXRD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and polarizing optical microscopy (POM). Solid state 13C{1H} cross polarization (CP) magic angle spinning (MAS) NMR of the low molecular mass gel in its native state was recorded for the first time. A close resemblance in the packing patterns of the gel, xerogel and bulk solid states was revealed upon comparing their 13C{1H}CPMAS NMR spectral pattern. A doublet r…
State of the art of CPMAS 13C-NMR spectroscopy applied to natural organic matter
2004
A number of different techniques are presently available for characterizing humified natural organic matter (NOM). Carbon-13 nuclear magnetic resonance spectroscopy (13C-NMR) in the solid state using cross-polarization (CP) and magic angle spinning (MAS) represents the most powerful experimental approach used to collect direct information on the structural and conformational characteristics of humic carbon backbones. Despite the problems due to the presence of paramagnetic impurities and the generally low organic matter concentration, cross-polarization magic angle spinning 13C-NMR spectroscopy (CPMAS 13C-NMR) is applied in soil chemistry and geochemistry mainly because of its relevance in …
N,N-Di-n-octyl-N,N-dimethyl and N,N-di-n-nonyl-N,N-dimethyl ammonium cholates: 13C and 15N CPMAS NMR, powder X-ray diffraction and thermoanalytical c…
2009
Abstract N,N-Di-n-octyl-N,N-dimethyl cholate (1) and N,N-di-n-nonyl-N,N-dimethyl ammonium cholate (2) have been prepared by crystallization from equimolar mixtures of sodium cholate and quaternary N,N-di-n-alkyl-N,N-dimethyl (n-octyl or n-nonyl) ammonium bromides. The formed crystalline materials have been structurally characterized by 13C and 15N cross polarization magic angle spinning (CPMAS) NMR, powder X-ray diffraction (PXRD) and thermoanalytical (TGA/DTA and DSC) methods and compared with each other. Powder X-ray diffraction patterns of 1 and 2 reveal clear similarities. Combined with the thermoanalytical data of these structures an existence of two hydrated polymorphs (most probably …
Static and MAS 35CI NMR and Molecular Motions of ClO −4 Ions in the Various Phases of Multimethylammonium Perchlorates
1986
Static and MAS*) 35CI NMR data of CIO−4 ions in the low-, intermediate- and high-temperature phases of trimethylammonium, dimethylammonium and monomethylammonium perchlorates are reported. The observed solid-solid phase transitions are interrelated with the motional state of the perchlorate ions. In the low-temperature phase III of trimethylammonium perchlorate there is an anisotropic motion of the ClO−4 ions with a constant quadrupole frequency of 185 kHz and an increasing value of the asymmetry parameter when approaching phase transition III-II. The activation energy for this motion is found to be 44.3 kj/mol. At the transition III-II the ClO−4 ions gain orientational degrees of freedom m…
Combining HR-MAS and In Vivo MRI and MRSI Information for Robust Brain Tumor Recognition
2009
In this study we propose to classify short echotime brain MRSI data by using multimodal information coming from magnetic resonance imaging (MRI), magnetic resonance spectroscopic imaging (MRSI) and high resolution magic angle spinning (HR-MAS), and to develop an advanced pattern recognition method that could help clinicians in diagnosing brain tumors. We study the impact of using HR-MAS information in combination with in vivo information for classifying brain tumors and we investigate which parameters influence our classification results.
Stabilization of the rhombohedral phase in LiZr2(PO4)3 by thermal quenching
1993
Abstract Two LiZr2(PO4)3 samples, which show rhombohedral and monoclinic symmetries, have been studied by powder XRD and MAS-NMR (31P and 7Li) techniques. In the monoclinic sample phosphorus occupies three crystallographic sites and lithium is preferentially placed in M2 environment. When the samples are subjected to successive heating-quenching treatments, the rhombohedral phase is not appreciably modified while the monoclinic phase is transformed into the rhombohedral one. In the quenched samples only one site for phosphorus has been detected and occupancy of lithium in the more symmetric M1 site is favoured. After the thermal treatments, when the samples are stored at room temperature fo…
Fast field cycling NMR relaxometry characterization of biochars obtained from an industrial thermochemical process
2012
Biochar has unique properties which make it a powerful tool to increase soil fertility and to contribute to the decrease of the amount of atmospheric carbon dioxide through the mechanisms of C sequestration in soils. Chemical and physical biochar characteristics depend upon the technique used for its production and the biomass nature. For this reason, biochar characterization is very important in order to address its use either for agricultural or environmental purposes. Three different biochars obtained from an industrial gasification process were selected in order to establish their chemical and physical peculiarities for a possible use in agronomical practices. They were obtained by char…