Search results for "Magic angle spinning"
showing 10 items of 48 documents
Effects of nucleotide binding to LmrA: A combined MAS-NMR and solution NMR study
2015
ABC transporters are fascinating examples of fine-tuned molecular machines that use the energy from ATP hydrolysis to translocate a multitude of substrates across biological membranes. While structural details have emerged on many members of this large protein superfamily, a number of functional details are still under debate. High resolution structures yield valuable insights into protein function, but it is the combination of structural, functional and dynamic insights that facilitates a complete understanding of the workings of their complex molecular mechanisms. NMR is a technique well-suited to investigate proteins in atomic resolution while taking their dynamic properties into account…
Non-negative blind source separation techniques for tumor tissue typing using HR-MAS signals.
2010
Given High Resolution Magic Angle Spinning (HR-MAS) signals from several glioblastoma tumor subjects, the goal is to differentiate between tumor tissue types by separating the different sources that contribute to the profile of each spectrum. Blind source separation techniques are applied for obtaining characteristic profiles for necrosis, high cellular tumor and border tumor tissue, and providing the contribution (abundance) of each tumor tissue to the profile of the spectra. The problem is formulated as a non-negative source separation problem. We illustrate the effectiveness of the proposed methods and we analyze to which extent the dimension of the input space could influence the perfor…
Precise measurement of 1H 90° pulse in solid-state NMR spectroscopy for complex and heterogeneous molecular systems
2007
The 90 degrees pulse calibration is essential in NMR spectroscopy to prevent artefacts in the liquid state or to enhance cross-polarization efficiency in the solid state. We verified pulse-angle (PA) errors due to circuit impedances in solid-state NMR and suggested a possible solution to prevent the inconvenience of PA errors. The classic pulse sequences used to calibrate (1)H 90 degrees pulse lengths by direct detection of protons or by cross-polarization were modified in order to replace single (1)H pulses with (1)H pulse trains. Pulse trains were found to decrease the effect of PA imperfections in the calibration of basic pulses (i.e. 90 degrees and 180 degrees ) for a number of organic …
Quantification and classification of high-resolution magic angle spinning data for brain tumor diagnosis.
2007
The goal of this work is to propose a complete protocol (preprocessing, processing and classification) for classifying brain tumors with proton high-resolution magic-angle spinning ((1)H HR-MAS) data. The different steps of the procedure are detailed and discussed. Feature extraction techniques such as peak integration, including also the automated quantitation method AQSES, were combined with linear (LDA) and non-linear (least-squares support vector machine or LS-SVM) classifiers. Classification accuracy was assessed using a stratified random sampling scheme. The results suggest that LS-SVM performs better than LDA while AQSES performs better than the standard peak integration feature extr…
H3PW12O40 supported on mesoporous MCM-41 and Al-MCM-41 materials: preparation and characterisation
2011
MCM-41 and Al–MCM-41 has been synthesized using cetyl-trimethylammonium bromide (CTAB) surfactant as template and adding the silica precursor to aqueous solutions containing CTAB. The obtained solids were calcined at 600 °C for 4 h. HPW heteropolyacid supported on the mesoporous were prepared using the incipient wetness method. The characterization of materials was performed by X-ray diffraction, Transmission Electron Microscopy, N2 adsorption, 29Si Cross Polarization–Magic Angle Spinning and 27Al MAS NMR. Results showed that the hexagonal structure is obtained in both cases. The Aluminium species are located inside an extra-framework. The impregnation reduces the surface area of the mesopo…
Low-temperature Ti-containing 3:2 and 2:1 mullite nanocrystals from single-phase gels
2007
Abstract TiO 2 -containig single-phase gels with (Al 2 O 3 + TiO 2 )/(SiO 2 ) molar ratios 3/2 and 2/1 were prepared by gelling mixtures of aluminium nitrate, tetraethylorthosilicate and titanium isopropoxide. Gels were fast heated at several temperatures up to 1100 °C. Dried and heated gels were characterized by differential thermal analysis (DTA), magic angle spinning nuclear magnetic resonance (MAS-NMR), X-ray powder diffraction (XRD), and scanning and transmission electron microscopies (SEM and TEM). Coupled DTA and XRD results of gels fast heated at 900 °C showed the crystallisation of two mullites as well as a small amount of alumina-silica spinel. 27 Al NMR spectra showed the format…
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…
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 …