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Magic Angle (magic + angle)

Distribution by Scientific Domains
Chemistry55%
Medical Sciences22%

Terms modified by Magic Angle

  • magic angle spinning
    		•

    Selected Abstracts

    Structure and properties of regenerated Antheraea pernyi silk fibroin filaments

    JOURNAL OF APPLIED POLYMER SCIENCE, Issue 4 2009
    Baoqi Zuo
    Abstract Degummed Antheraeapernyi silk fibroin (APSF) fibers were dissolved in a lithium thiocyanate solution that was dialyzed against distilled water for 3 days. Solution-cast APSF films were dissolved in hexafluoroisopropanol to prepare a spinning solution. Wet spinning was employed to prepare APSF filaments. Scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, solid-state 13C cross-polarization/magic angle spinning nuclear magnetic resonance, and differential scanning calorimetry were employed to study the regenerated APSF filaments. The results showed a uniform distribution of molecular weights, and the largest one may have been greater than 200 kDa. The regenerated filaments contained ,-sheet, ,-helix, and random-coil conformations, and their breaking strength was 52.20% of the breaking strength of the native fibers. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009 [source]

    NMR chemical shift measurements revisited: High precision measurements

    CONCEPTS IN MAGNETIC RESONANCE, Issue 4 2007
    P. Granger
    Abstract Accurate chemical shifts are now accessible with high field NMR spectrometers. After the recall of the basic formulae, methods are proposed to measure chemical shifts with a high precision. Using two coaxial rotors at the magic angle, the necessary parameters used for correction are measured. The influence of different factors on the precision of the NMR measurements is discussed. Some proposals are given for MAS experiments used with solid-state samples. © 2007 Wiley Periodicals, Inc. Concepts Magn Reson Part A 30A: 184,193, 2007. [source]

    In Situ Synthesis, Characterization of SiPMo-X, and Different Catalytic Properties of SiPMo-X and SiPW-X

    EUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 15 2006
    Chunfeng Shi
    Abstract SBA-15 frameworks with encapsulated Keggin type heteropolyacids (HPAs) were synthesized in situ under strongly acidic conditions (pH,<,0). During the hydrolysis of tetraethyl orthosilicate (TEOS), a P- and a Mo source were added into the initial sol,gel system to form Keggin type HPAs. The texture of the final products was studied by the N2 adsorption,desorption isotherms and transmission electron microscopy (TEM), and their structure was systematically characterized by X-ray diffraction (XRD), UV/Vis diffuse reflectance- (DRS), infrared- (IR), and 31P magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy. Characterization results suggest that the samples show very ordered hexagonal mesostructure, and the HPAs that are incorporated into the framework of meso-silica are insoluble during catalysis. Results of catalytic tests indicate that the materials demonstrated catalytic activity comparable with or even surpassing those of the bulk HPAs in catalytic tests implementing chemical reactions of bulky molecules (1,3,5-triisopropylbenzene cracking, esterification of benzoic acid with tert -butyl alcohol, and 2,3,6-trimethylphenol hydroxylation with H2O2). Additionally, some other properties, such as easy separation and stability when recycled, ensure their potential applications in the chemical industries. Here, we report not only the in situ synthesis and characterization of SiPMo-X, but also the difference in the catalytic properties of SiPMo-X and SiPW-X. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2006) [source]

    Effect of long-term combined nitrogen and phosphorus fertilizer application on 13C CPMAS NMR spectra of humin in a Typic Hapludoll of northeast China

    EUROPEAN JOURNAL OF SOIL SCIENCE, Issue 6 2009
    J. J. Zhang
    Summary Because of its insolubility, heterogeneity and structural complexity, humin is the least understood among the three fractions of soil humic substances. This research aimed to evaluate the long-term effect of combined nitrogen and phosphorus (NP) fertilizer addition on the chemical structure of humin under maize (Zea mays L.) monoculture in a Typic Hapludoll of northeast China. Soil samples were collected 12 and 25 years after the initiation of the fertilizer treatment. Soil humin was isolated using NaOH-Na4P2O7 extraction to remove humic and fulvic acids, which was followed by HF-HCl treatment to remove most of the inorganic minerals. Solid-state 13C cross-polarization magic angle spinning nuclear magnetic resonance (13C CPMAS NMR) spectroscopy was used to characterize the chemical structure of the humin isolates. Results showed that the organic carbon (C) content of humin increased after NP fertilizer addition, compared with a no-fertilizer (CK) treatment. 13C CPMAS NMR indicated that O-alkyl C and aromatic C of humin decreased, while alkyl C and the ratios of alkyl C/O-alkyl C, aliphatic C/aromatic C and hydrophobic C/hydrophilic C all increased in the NP fertilizer treatment. The long-term application of NP fertilizer changed the molecular structure of soil humin to be more alkyl and hydrophobic, and was thus beneficial to the sequestration and stability of organic C in soil. [source]

    Epoxidation of allyl chloride and hydrogen peroxide over titanium silicalite-1 film on SiO2 pellet support

    JOURNAL OF CHEMICAL TECHNOLOGY & BIOTECHNOLOGY, Issue 4 2007
    Li Wang
    Abstract Titanium silicalite-1 (TS-1) films were prepared on SiO2 pellet supports via an in situ hydrothermal synthesis method and were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and 29Si magic angle spinning nuclear magnetic resonance (Si MAS NMR). The growth time of TS-1 film had a strong effect on its morphology and the thickness and size of the crystals. The uniformity and thickness of TS-1 films increased with increase of growth times. The epoxidation of allyl chloride (ACH) with dilute hydrogen peroxide to form epichlorohydrin (ECH) over the TS-1 films was carried out in a fixed bed reactor. The conversion of ACH and the selectivity to ECH over the TS-1 films of the second growth were higher than that of the first growth, the third and the fourth growth. And the conversion and selectivity as a function of time-on-stream gave a good stable performance in an extended test up to at least 19 h. The final steady-state conversion and selectivity were approximately 86% and 55%, respectively. Copyright © 2007 Society of Chemical Industry [source]

    Tailoring 13C labeling for triple-resonance solid-state NMR experiments on aligned samples of proteins

    MAGNETIC RESONANCE IN CHEMISTRY, Issue S1 2007
    Neeraj Sinha
    Abstract In order to develop triple-resonance solid-state NMR spectroscopy of membrane proteins, we have implemented several different 13C labeling schemes with the purpose of overcoming the interfering effects of 13C13C dipole,dipole couplings in stationary samples. The membrane-bound form of the major coat protein of the filamentous bacteriophage Pf1 was used as an example of a well-characterized helical membrane protein. Aligned protein samples randomly enriched to 35% 13C in all sites and metabolically labeled from bacterial growth on media containing [2- 13C]-glycerol or [1,3- 13C]-glycerol enables direct 13C detection in solid-state NMR experiments without the need for homonuclear 13C13C dipole,dipole decoupling. The 13C-detected NMR spectra of Pf1 coat protein show a substantial increase in sensitivity compared to the equivalent 15N-detected spectra. The isotopic labeling pattern was analyzed for [2- 13C]-glycerol and [1,3- 13C]-glycerol as metabolic precursors by solution-state NMR of micelle samples. Polarization inversion spin exchange at the magic angle (PISEMA) and other solid-state NMR experiments work well on 35% random fractionally and metabolically tailored 13C-labeled samples, in contrast to their failure with conventional 100% uniformly 13C-labeled samples. Copyright © 2007 John Wiley & Sons, Ltd. [source]

    29Si spin-lattice NMR relaxation in microporous silica-based materials with high Mn2+ concentrations

    MAGNETIC RESONANCE IN CHEMISTRY, Issue 11 2006
    Vladimir I. Bakhmutov
    Abstract The 29Si T1 time measurements have been performed under magic angle spinning for supermicroporous Si/Mn materials 1,6 containing Mn2+ in concentrations of 0 (1), 1.2 (2), 2.5 (3), 3.8 (4), 15 (5) and 19.8 wt% (6). It has been found that the central lines, corresponding to isotropic chemical shifts, and their sidebands relax differently in samples 2,4 with relatively small Mn2+ contents. Because the relaxation curves for 1,6 are nonexponential and identical for 6 at spinning rates of 5, 10 and 12 kHz, dipolar relaxation via the paramagnetic centers is dominant. The relaxation data have been interpreted as a function of Mn2+ concentrations in terms of incorporation of the Mn2+ ions into the silica lattice when their concentration is small (,2.5 wt%). At higher concentrations, most of the manganese is located on the surface of the silica. Copyright © 2006 John Wiley & Sons, Ltd. [source]

    Preinvasive and invasive cervical cancer: an ex vivo proton magic angle spinning magnetic resonance spectroscopy study

    NMR IN BIOMEDICINE, Issue 3 2004
    Marrita M. Mahon
    Abstract The aim of this study was to obtain 1H MR spectra using magic angle spinning (MAS) techniques from punch biopsies (<20,mg) of preinvasive and invasive cervical disease and to correlate the spectral profiles with sample classification on the basis of histopathology. Tissue samples were obtained at colposcopic examination, during local treatment of cervical intraepithelial neoplasia (CIN) or at hysterectomy. 1H MAS MRS was performed at 25°C while spinning the sample at 4.5,kHz. After measurement, the tissue was immersed in formalin and the pathology determined. Histological examination after 1H MAS MRS defined 27 samples with squamous cell carcinoma (SCC), 12 with CIN and 39 with only normal tissue. The standardized integrals of the lipid, choline and creatine regions of the spectra were significantly higher in SCC than in normal or CIN tissue. There was no obvious difference in the standardized integral of the region 4.15,3.5,ppm. The acyl fatty acid side-chain length was longer or less unsaturated in SCC than in normal tissue. Normal tissue from patients with SCC showed significantly higher triglycerides than normal tissue from patients with benign uterine disease but significantly lower triglycerides than SCC tissue. 1H MAS MRS of the uterine cervix ex vivo may be used to differentiate non-invasive from invasive cervical lesions, increase interpretation of in vivo MRS and provide insights into tumor biology. Copyright © 2004 John Wiley & Sons, Ltd. [source]

    Simultaneous assignment and structure determination of a membrane protein from NMR orientational restraints

    PROTEIN SCIENCE, Issue 3 2003
    Francesca M. Marassi
    Abstract A solid-state NMR approach for simultaneous resonance assignment and three-dimensional structure determination of a membrane protein in lipid bilayers is described. The approach is based on the scattering, hence the descriptor "shotgun," of 15N-labeled amino acids throughout the protein sequence (and the resulting NMR spectra). The samples are obtained by protein expression in bacteria grown on media in which one type of amino acid is labeled and the others are not. Shotgun NMR short-circuits the laborious and time-consuming process of obtaining complete sequential assignments prior to the calculation of a protein structure from the NMR data by taking advantage of the orientational information inherent to the spectra of aligned proteins. As a result, it is possible to simultaneously assign resonances and measure orientational restraints for structure determination. A total of five two-dimensional 1H/15N PISEMA (polarization inversion spin exchange at the magic angle) spectra, from one uniformly and four selectively 15N-labeled samples, were sufficient to determine the structure of the membrane-bound form of the 50-residue major pVIII coat protein of fd filamentous bacteriophage. Pisa (polarity index slat angle) wheels are an essential element in the process, which starts with the simultaneous assignment of resonances and the assembly of isolated polypeptide segments, and culminates in the complete three-dimensional structure of the protein with atomic resolution. The principles are also applicable to weakly aligned proteins studied by solution NMR spectroscopy. [The structure we determined for the membrane-bound form of the Fd bacteriophage pVIII coat protein has been deposited in the Protein Data Bank as PDB file 1MZT.] [source]