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Sample records for 6li mas nmr

  1. Investigating sorption on iron-oxyhydroxide soil minerals by solid-state NMR spectroscopy: a 6Li MAS NMR study of adsorption and absorption on goethite

    DEFF Research Database (Denmark)

    Nielsen, Ulla Gro; Paik, Younkee; Julmis, Keinia;

    2005-01-01

    High-resolution 2H MAS NMR spectra can be obtained for nanocrystalline particles of goethite (alpha-FeOOH, particle size approximately 4-10 nm) at room temperature, facilitating NMR studies of sorption under environmentally relevant conditions. Li sorption was investigated as a function of pH, th...

  2. MAS NMR of HIV-1 protein assemblies

    Science.gov (United States)

    Suiter, Christopher L.; Quinn, Caitlin M.; Lu, Manman; Hou, Guangjin; Zhang, Huilan; Polenova, Tatyana

    2015-04-01

    The negative global impact of the AIDS pandemic is well known. In this perspective article, the utility of magic angle spinning (MAS) NMR spectroscopy to answer pressing questions related to the structure and dynamics of HIV-1 protein assemblies is examined. In recent years, MAS NMR has undergone major technological developments enabling studies of large viral assemblies. We discuss some of these evolving methods and technologies and provide a perspective on the current state of MAS NMR as applied to the investigations into structure and dynamics of HIV-1 assemblies of CA capsid protein and of Gag maturation intermediates.

  3. High resolution MAS-NMR in combinatorial chemistry.

    Science.gov (United States)

    Shapiro, M J; Gounarides, J S

    High-resolution magic angle spinning (hr-MAS) NMR is a powerful tool for characterizing organic reactions on solid support. Because magic angle spinning reduces the line-broadening due to dipolar coupling and variations in bulk magnetic susceptibility, line widths approaching those obtained in solution-phase NMR can be obtained. The magic angle spinning method is amenable for use in conjunction with a variety of NMR-pulse sequences, making it possible to perform full-structure determinations and conformational analysis on compounds attached to a polymer support. Diffusion-weighted MAS-NMR methods such as SPEEDY (Spin-Echo-Enhanced Diffusion-Filtered Spectroscopy) can be used to remove unwanted signals from the solvent, residual reactants, and the polymer support from the MAS-NMR spectrum, leaving only those signals arising from the resin-bound product. This review will present the applications of high-resolution magic angle spinning NMR for use in combinatorial chemistry research.

  4. Structural biology applications of solid state MAS DNP NMR

    Science.gov (United States)

    Akbey, Ümit; Oschkinat, Hartmut

    2016-08-01

    Dynamic Nuclear Polarization (DNP) has long been an aim for increasing sensitivity of nuclear magnetic resonance (NMR) spectroscopy, delivering spectra in shorter experiment times or of smaller sample amounts. In recent years, it has been applied in magic angle spinning (MAS) solid-state NMR to a large range of samples, including biological macromolecules and functional materials. New research directions in structural biology can be envisaged by DNP, facilitating investigations on very large complexes or very heterogeneous samples. Here we present a summary of state of the art DNP MAS NMR spectroscopy and its applications to structural biology, discussing the technical challenges and factors affecting DNP performance.

  5. High-temperature MAS-NMR at high spinning speeds.

    Science.gov (United States)

    Kirchhain, Holger; Holzinger, Julian; Mainka, Adrian; Spörhase, Andreas; Venkatachalam, Sabarinathan; Wixforth, Achim; van Wüllen, Leo

    2016-09-01

    A low cost version to enable high temperature MAS NMR experiments at temperatures of up to 700°C and spinning speeds of up to 10kHz is presented. The method relies on inductive heating using a metal coated rotor insert. The metal coating is accomplished via a two step process involving physical vapor deposition and galvanization.

  6. Size-exclusion chromatographic NMR under HR-MAS.

    Science.gov (United States)

    Lucena Alcalde, Guillermo; Anderson, Natalie; Day, Iain J

    2017-05-01

    The addition of stationary phases or sample modifiers can be used to modify the separation achievable in the diffusion domain of diffusion NMR experiments or provide information on the nature of the analyte-sample modifier interaction. Unfortunately, the addition of insoluble chromatographic stationary phases can lead to line broadening and degradation in spectral resolution, largely because of differences in magnetic susceptibility between the sample and the stationary phase. High-resolution magic angle spinning (HR-MAS) techniques can be used to remove this broadening. Here, we attempt the application of HR-MAS to size-exclusion chromatographic NMR with limited success. Observed diffusion coefficients for polymer molecular weight reference standards are shown to be larger than those obtained on static samples. Further investigation reveals that under HR-MAS it is possible to obtain reasonably accurate estimates of diffusion coefficients, using either full rotor synchronisation or sophisticated pulse sequences. The requirement for restricting the sample to the centre of the MAS rotor to ensure homogeneous magnetic and RF fields is also tested. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  7. Residue specific hydration of primary cell wall potato pectin identified by solid-state 13C single-pulse MAS and CP/MAS NMR spectroscopy

    DEFF Research Database (Denmark)

    Larsen, Flemming H; Byg, Inge; Damager, Iben

    2011-01-01

    Hydration of rhamnogalacturonan-I (RG-I) derived from potato cell wall was analyzed by 13C single-pulse (SP) magic-angle-spinning (MAS) and 13C cross-polarization (CP) MAS nuclear magnetic resonance (NMR) and supported by 2H SP/MAS NMR experiments. The study shows that the arabinan side chains...

  8. 1H MAS and 1H --> 31P CP/MAS NMR study of human bone mineral.

    Science.gov (United States)

    Kaflak-Hachulska, A; Samoson, A; Kolodziejski, W

    2003-11-01

    Chemical structure of human bone mineral was studied by solid-state nuclear magnetic resonance (NMR) with magic-angle spinning (MAS). Trabecular and cortical bone samples from adult subjects were compared with mineral standards: hydroxyapatite (HA), hydrated and calcined, carbonatoapatite of type B with 9 wt% of CO3(2-) (CHA-B), brushite (BRU) and mixtures of HA with BRU. Proton spectra were acquired with excellent spectral resolution provided by ultra-high speed MAS at 40 kHz. 2D 1H-31P NMR heteronuclear correlation was achieved by cross-polarization (CP) under fast MAS at 12 kHz. 31P NMR was applied with CP from protons under slow MAS at 1 kHz. Appearance of 31P rotational sidebands together with their CP kinetics were analyzed. It was suggested that the sidebands of CP spectra are particularly suitable for monitoring the state of apatite crystal surfaces. The bone samples appeared to be deficient in structural hydroxyl groups analogous to those in HA. We found no direct evidence that the HPO4(2-) brushite-like ions are present in bone mineral. The latter problem is extensively discussed in the literature. The study proves there is a similarity between CHA-B and bone mineral expressed by their similar NMR behavior.

  9. Natural Abundance 17O, 6Li NMR and Molecular Modeling Studies of the Solvation Structures of Lithium bis(fluorosulfonyl)imide/1,2-dimethoxyethane Liquid Electrolytes

    Energy Technology Data Exchange (ETDEWEB)

    Wan, Chuan; Hu, Mary Y.; Borodin, Oleg; Qian, Jiangfeng; Qin, Zhaohai; Zhang, Jiguang; Hu, Jian Z.

    2016-03-01

    Natural abundance 17O and 6Li NMR experiments, quantum chemistry and molecular dynamics studies were employed to investigate the solvation structures of Li+ at various concentrations of LiFSI in DME electrolytes in an effort to solve this puzzle. It was found that the chemical shifts of both 17O and 6Li changed with the concentration of LiFSI, indicating the changes of solvation structures with concentration. For the quantum chemistry calculations, the coordinated cluster LiFSI(DME)2 forms at first, and its relative ratio increases with increasing LiFSI concentration to 1 M. Then the solvation structure LiFSI(DME) become the dominant component. As a result, the coordination of forming contact ion pairs between Li+ and FSI- ion increases, but the association between Li+ and DME molecule decreases. Furthermore, at LiFSI concentration of 4 M the solvation structures associated with Li+(FSI-)2(DME), Li+2(FSI-)(DME)4 and (LiFSI)2(DME)3 become the dominant components. For the molecular dynamics simulation, with increasing concentration, the association between DME and Li+ decreases, and the coordinated number of FSI- increases, which is in perfect accord with the DFT results. These results provide more insight on the fundamental mechanism on the very high CE of Li deposition in these electrolytes, especially at high current density conditions.

  10. {sup 29}Si MAS NMR for the zeolite Y - gallium oxide system; {sup 29}Si mas NMR dla ukladu fojazyt-tlenek galu

    Energy Technology Data Exchange (ETDEWEB)

    Sulikowski, B.; Derewinski, M. [Inst. Katalizy i Fizykochemii Powierzchni, Polska Akademia Nauk, Cracow (Poland); Olejniczak, Z.; Segnowski, S. [Institute of Nuclear Physics, Cracow (Poland)

    1994-12-31

    Wide-pore zeolites modified by gallium oxide has been prepared for catalytic use. Its physico-chemical and catalytic properties have been studied. The structure changes of the catalyst have been investigated by means of MAS NMR spectroscopy. Spectra of {sup 29}Si has been described and discussed. 11 refs, 4 figs, 2 tabs.

  11. Temperature calibration for high-temperature MAS NMR to 913 K: 63Cu MAS NMR of CuBr and CuI, and 23Na MAS NMR of NaNbO3.

    Science.gov (United States)

    Wu, Jingshi; Kim, Namjun; Stebbins, Jonathan F

    2011-09-01

    The solid-state phase transitions of CuBr, CuI and NaNbO(3) can be readily observed using (63)Cu and (23)Na high-temperature magic-angle spinning nuclear magnetic resonance spectroscopy. Temperature has large, linear effects on the peak maximum of (63)Cu in each solid phase of CuBr and CuI, and there is large jump in shift across each phase transition. The (23)Na MAS NMR peak intensities and the line widths in NaNbO(3) also clearly show its high-temperature transition to the cubic phase. These data can be used to calibrate high-temperature MAS NMR probes up to 913 K, which is two hundred degrees higher than the commonly-used temperature calibration based on the chemical shift of (207)Pb in Pb(NO(3))(2). Copyright © 2011 Elsevier Inc. All rights reserved.

  12. Factor analysis of 27Al MAS NMR spectra for identifying nanocrystalline phases in amorphous geopolymers.

    Science.gov (United States)

    Urbanova, Martina; Kobera, Libor; Brus, Jiri

    2013-11-01

    Nanostructured materials offer enhanced physicochemical properties because of the large interfacial area. Typically, geopolymers with specifically synthesized nanosized zeolites are a promising material for the sorption of pollutants. The structural characterization of these aluminosilicates, however, continues to be a challenge. To circumvent complications resulting from the amorphous character of the aluminosilicate matrix and from the low concentrations of nanosized crystallites, we have proposed a procedure based on factor analysis of (27)Al MAS NMR spectra. The capability of the proposed method was tested on geopolymers that exhibited various tendencies to crystallize (i) completely amorphous systems, (ii) X-ray amorphous systems with nanocrystalline phases, and (iii) highly crystalline systems. Although the recorded (27)Al MAS NMR spectra did not show visible differences between the amorphous systems (i) and the geopolymers with the nanocrystalline phase (ii), the applied factor analysis unambiguously distinguished these materials. The samples were separated into the well-defined clusters, and the systems with the evolving crystalline phase were identified even before any crystalline fraction was detected by X-ray powder diffraction. Reliability of the proposed procedure was verified by comparing it with (29)Si MAS NMR spectra. Factor analysis of (27)Al MAS NMR spectra thus has the ability to reveal spectroscopic features corresponding to the nanocrystalline phases. Because the measurement time of (27)Al MAS NMR spectra is significantly shorter than that of (29)Si MAS NMR data, the proposed procedure is particularly suitable for the analysis of large sets of specifically synthesized geopolymers in which the formation of the limited fractions of nanocrystalline phases is desired. Copyright © 2013 John Wiley & Sons, Ltd.

  13. Size-exclusion chromatographic NMR under HR-MAS

    OpenAIRE

    Lucena Alcalde, Guillermo; Anderson, Natalie; Day, Iain J.

    2016-01-01

    The addition of stationary phases or sample modifiers can be used to modify the separation achievable in the diffusion domain of diffusion NMR experiments or provide information on the nature of the analyte–sample modifier interaction. Unfortunately, the addition of insoluble chromatographic stationary phases can lead to line broadening and degradation in spectral resolution, largely because of differences in magnetic susceptibility between the sample and the stationary phase. High-resolution...

  14. High temperature {sup 17}O MAS NMR study of calcia, magnesia, scandia and yttria stabilized zirconia

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Namjun; Stebbins, Jonathan F. [Department of Geological and Environmental Sciences, Stanford University, Stanford, CA 94305 (United States); Hsieh, Cheng-Han [Department of Materials Science and Engineering, Stanford University, Stanford, CA 94305 (United States); Huang, Hong [Department of Mechanical Engineering, Stanford University, Stanford, CA 94305 (United States); Prinz, Fritz B. [Department of Materials Science and Engineering, Stanford University, Stanford, CA 94305 (United States); Department of Mechanical Engineering, Stanford University, Stanford, CA 94305 (United States)

    2007-11-15

    High-resolution {sup 17}O MAS NMR can provide unique constraints on local structure and oxide ion dynamics in conductive zirconia ceramics of interest for fuel cells and other technologies. We describe here NMR and bulk conductivity measurements for scandia, yttria, calcia, and magnesia stabilized zirconias, including MAS NMR spectra collected in situ at temperatures up to 700 C. All of the cubic compounds with high dopant levels showed line narrowing and coalescence in this temperature range, and the temperature-induced changes in line widths are qualitatively correlated with the bulk conductivities. A monoclinic zirconia with 2% Sc{sub 2}O{sub 3} dopant level (expected to have relatively low ionic mobility) showed no motional averaging of its two {sup 17}O NMR peaks even at 600 C, but instead is observed to begin to transform to a disordered, possibly cubic or tetragonal phase at 600 to 700 C. {sup 17}O MAS NMR spectra of calcia stabilized zirconia were analyzed in detail and the exchange frequencies as a function of temperature, conductivity, and activation energy were estimated and compared with bulk conductivities. The activation energy estimated from NMR exchange frequencies is somewhat lower than that of bulk conductivity but the conductivities estimated from NMR appear to be lower than bulk conductivity. (author)

  15. Solid-phase enolate chemistry investigated using HR-MAS NMR spectroscopy.

    Science.gov (United States)

    Fruchart, Jean-Sébastien; Lippens, Guy; Kuhn, Cyrille; Gras-Masse, Hélène; Melnyk, Oleg

    2002-01-25

    Supported P4-t-Bu enolate chemistry of phenylacetyloxymethyl polystyrene (PS) resin was investigated using high-resolution magic angle spinning (HR-MAS) NMR spectroscopy. Direct analysis of the crude reaction suspensions through the use of a diffusion filter (DF) allowed a rapid selection of the optimal experimental conditions, but also the characterization of the enolate on the solid phase. Comparison with solution experiments and literature data allowed us to address partially the structure of the enolate. HR-MAS NMR spectra of the enolate revealed also a tight interaction of P4-t-Bu base with the polymer matrix.

  16. 27 Al MAS NMR Studies of HBEA Zeolite at Low to High Magnetic Fields

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Jian Zhi; Wan, Chuan; Vjunov, Aleksei; Wang, Meng; Zhao, Zhenchao; Hu, Mary Y.; Camaioni, Donald M.; Lercher, Johannes A.

    2017-06-01

    27Al single pulse (SP) MAS NMR spectra of HBEA zeolites with high Si/Al ratios of 71 and 75 were obtained at three magnetic field strengths of 7.05, 11.75 and 19.97 T. High field 27Al MAS NMR spectra acquired at 19.97 T show significantly improved spectral resolution, resulting in at least two well-resolved tetrahedral-Al NMR peaks. Based on the results obtained from 27Al MAS and MQMAS NMR acquired at 19.97 T, four different quadrupole peaks are used to deconvolute the 27Al SP MAS spectra acquired at vari-ous fields by using the same set of quadrupole coupling constants, asymmetric parameters and relative integrated peak intensities for the tetrahedral Al peaks. The line shapes of individual peaks change from typical quadrupole line shape at low field to essentially symmetrical line shapes at high field. We demonstrate that for fully hydrated HBEA zeolites the effect of second order quadrupole interaction can be ignored and quantitative spectral analysis can be performed by directly fitting the high field spectra using mixed Gaussian/Lorentzian line shapes. Also, the analytical steps described in our work allow direct assignment of spectral intensity to individual Al tetrahedral sites (T-sites) of zeolite HBEA. Finally, the proposed concept is suggested generally applicable to other zeo-lite framework types, thus, allowing a direct probing of Al distributions by NMR spectroscopic methods in zeolites with high confi-dence.

  17. Slow-spinning low-sideband HR-MAS NMR spectroscopy: delicate analysis of biological samples

    Science.gov (United States)

    Renault, Marie; Shintu, Laetitia; Piotto, Martial; Caldarelli, Stefano

    2013-11-01

    High-Resolution Magic-Angle Spinning (HR-MAS) NMR spectroscopy has become an extremely versatile analytical tool to study heterogeneous systems endowed with liquid-like dynamics. Spinning frequencies of several kHz are however required to obtain NMR spectra, devoid of spinning sidebands, with a resolution approaching that of purely isotropic liquid samples. An important limitation of the method is the large centrifugal forces that can damage the structure of the sample. In this communication, we show that optimizing the sample preparation, particularly avoiding air bubbles, and the geometry of the sample chamber of the HR-MAS rotor leads to high-quality low-sideband NMR spectra even at very moderate spinning frequencies, thus allowing the use of well-established solution-state NMR procedures for the characterization of small and highly dynamic molecules in the most fragile samples, such as live cells and intact tissues.

  18. Slow-spinning low-sideband HR-MAS NMR spectroscopy: delicate analysis of biological samples

    Science.gov (United States)

    Renault, Marie; Shintu, Laetitia; Piotto, Martial; Caldarelli, Stefano

    2013-01-01

    High-Resolution Magic-Angle Spinning (HR-MAS) NMR spectroscopy has become an extremely versatile analytical tool to study heterogeneous systems endowed with liquid-like dynamics. Spinning frequencies of several kHz are however required to obtain NMR spectra, devoid of spinning sidebands, with a resolution approaching that of purely isotropic liquid samples. An important limitation of the method is the large centrifugal forces that can damage the structure of the sample. In this communication, we show that optimizing the sample preparation, particularly avoiding air bubbles, and the geometry of the sample chamber of the HR-MAS rotor leads to high-quality low-sideband NMR spectra even at very moderate spinning frequencies, thus allowing the use of well-established solution-state NMR procedures for the characterization of small and highly dynamic molecules in the most fragile samples, such as live cells and intact tissues. PMID:24284435

  19. 1H HR-MAS NMR and S180 cells: metabolite assignment and evaluation of pulse sequence

    OpenAIRE

    Oliveira, Aline L.; Martinelli,Bruno César B.; Lião,Luciano M.; Pereira,Flávia C.; Silveira-Lacerda,Elisangela P.; Alcantara,Glaucia B.

    2014-01-01

    High resolution magic angle spinning ¹H nuclear magnetic resonance spectroscopy (HR-MAS NMR) is a useful technique for evaluation of intact cells and tissues. However, optimal NMR parameters are crucial in obtaining reliable results. To identify the key steps for the optimization of HR-MAS NMR parameters, we assessed different pulse sequences and NMR parameters using sarcoma 180 (S180) cells. A complete assignment of the metabolites of S180 is given to assist future studies.

  20. Optimized multiple quantum MAS lineshape simulations in solid state NMR

    Science.gov (United States)

    Brouwer, William J.; Davis, Michael C.; Mueller, Karl T.

    2009-10-01

    /Linux Operating system: UNIX/Linux Has the code been vectorised or parallelized?: Yes RAM: Example: (1597 powder angles) × (200 Samples) × (81 F2 frequency pts) × (31 F1 frequency points) = 3.5M, SMP AMD opteron Classification: 2.3 External routines: OCTAVE ( http://www.gnu.org/software/octave/), GNU Scientific Library ( http://www.gnu.org/software/gsl/), OPENMP ( http://openmp.org/wp/) Nature of problem: The optimal simulation and modeling of multiple quantum magic angle spinning NMR spectra, for general systems, especially those with mild to significant disorder. The approach outlined and implemented in C and OCTAVE also produces model parameter error estimates. Solution method: A model for each distinct chemical site is first proposed, for the individual contribution of crystallite orientations to the spectrum. This model is averaged over all powder angles [1], as well as the (stochastic) parameters; isotropic chemical shift and quadrupole coupling constant. The latter is accomplished via sampling from a bi-variate Gaussian distribution, using the Box-Muller algorithm to transform Sobol (quasi) random numbers [2]. A simulated annealing optimization is performed, and finally the non-linear jackknife [3] is applied in developing model parameter error estimates. Additional comments: The distribution contains a script, mqmasOpt.m, which runs in the OCTAVE language workspace. Running time: Example: (1597 powder angles) × (200 Samples) × (81 F2 frequency pts) × (31 F1 frequency points) = 58.35 seconds, SMP AMD opteron. References:S.K. Zaremba, Annali di Matematica Pura ed Applicata 73 (1966) 293. H. Niederreiter, Random Number Generation and Quasi-Monte Carlo Methods, SIAM, 1992. T. Fox, D. Hinkley, K. Larntz, Technometrics 22 (1980) 29.

  1. 29Si and 27AI MAS NMR Study of Alkali Feldspars

    Institute of Scientific and Technical Information of China (English)

    周玲棣; 郭九皋; 袁汉珍; 李丽云

    1994-01-01

    12 natural alkali feldspars have been studied by(29)~Si and(27)~Al MAS NMR as well as XRD,IR,EPMA and chemical analysis.Three kinds of(29)~Si NMR spectra,i.e.the spectra of microcline,perthiteand perthite with minor plagioclase,have been obtained.There are two types of(27)~Al NMR spectra.The(27)~Alspectrum of microcline is the same as that of perthite,but is different from the spectrum for perthite contain-ing plagioclase.Through this study,we found that the results of NMR and IR are inconsistent with that ofXRD,which shows that the transition of alkali feldspar from monoclinic to triclinic system might be a rathercomplicated process.

  2. Decomposition of adsorbed VX on activated carbons studied by 31P MAS NMR.

    Science.gov (United States)

    Columbus, Ishay; Waysbort, Daniel; Shmueli, Liora; Nir, Ido; Kaplan, Doron

    2006-06-15

    The fate of the persistent OP nerve agent O-ethyl S-[2-(diisopropylamino)ethyl] methylphosphonothioate (VX) on granular activated carbons that are used for gas filtration was studied by means of 31P magic angle spinning (MAS) NMR spectroscopy. VX as vapor or liquid was adsorbed on carbon granules, and MAS NMR spectra were recorded periodically. The results show that at least 90% of the adsorbed VX decomposes within 20 days or less to the nontoxic ethyl methylphosphonic acid (EMPA) and bis(S-2-diisopropylaminoethane) {(DES)2}. Decomposition occurred irrespective of the phase from which VX was loaded, the presence of metal impregnation on the carbon surface, and the water content of the carbon. Theoretical and practical aspects of the degradation are discussed.

  3. Decomposition of adsorbed VX on activated carbons studied by {sup 31}P MAS NMR

    Energy Technology Data Exchange (ETDEWEB)

    Ishay Columbus; Daniel Waysbort; Liora Shmueli; Ido Nir; Doron Kaplan [Israel Institute for Biological Research, Ness Ziona (Israel). Departments of Organic Chemistry and Physical Chemistry

    2006-06-15

    The fate of the persistent OP nerve agent O-ethyl S-(2-(diisopropylamino)ethyl) methylphosphonothioate (VX) on granular activated carbons that are used for gas filtration was studied by means of 31P magic angle spinning (MAS) NMR spectroscopy. Four types of activated carbon were used, including coal-based BPL. VX as vapor or liquid was adsorbed on carbon granules, and MAS NMR spectra were recorded periodically. The results show that at least 90% of the adsorbed VX decomposes within 20 days or less to the nontoxic ethyl methylphosphonic acid (EMPA) and bis(S-2-diisopropylaminoethane) ((DES){sub 2}). Decomposition occurred irrespective of the phase from which VX was loaded, the presence of metal impregnation on the carbon surface, and the water content of the carbon. Theoretical and practical aspects of the degradation are discussed. 17 refs., 6 figs., 3 tabs.

  4. Infrared and MAS NMR Spectroscopic Studies of Al18B4O33

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    The IR spectrum and 11B and 27Al MAS NMR spectra of Al18B4O33 are presented and discussed in relation to the possible existence of boron atoms substituting for aluminum atoms. TheIR spectrum shows that the strong vibrations of the BO3 groups are present in the 1 500~1 200em-1 region, and very weak bands of BO4 units are present in the region from 1 000 to 1 100cm-1. 11B MAS NMR spectrum indicates that the strong signal for BO3 units appears in the region from δ +5 to δ +20, and the very weak signal for BO4 units is at about δ-1, while 27AlMAS NMR spectrum shows five peaks at about δ +62, +42. 1, +14,-4.7 and-6.4, originating from AlO4, AlO4, A1O5, AlO6 and AlO6, respectively. These results reveal that there areminor BO4 units in Al18B4O33, indicating that a small amount of B atoms substitute for Al atomsin the 4-fold coordination.

  5. Increasing 13C CP-MAS NMR resolution using single crystals: application to model octaethyl porphyrins.

    Science.gov (United States)

    Dugar, Sneha; Fu, Riqiang; Dalal, Naresh S

    2012-08-02

    Octaethyl porphyrin (OEP) and its Ni and Zn derivatives are considered as model compounds in biochemical, photophysical, and fossil fuel chemistry. They have thus been investigated by high-resolution solid-state (13)C NMR using powders, but peak assignment has been difficult because of large line widths. Arguing that a significant cause of broadening might be the anisotropic bulk magnetic susceptibility, we utilized single crystals in our (13)C cross-polarization magic angle spinning (CP-MAS) measurements and observed a nearly 2-fold line narrowing. This enhanced resolution enabled us to assign chemical shifts to each carbon for all the three compounds. The new assignments are now in agreement with X-ray structural data and allowed us to probe the motional dynamics of the methyl and methylene carbons of the OEP side chains. It is apparent that the use of single crystals in (13)C CP-MAS measurements has a significantly wider impact than previously thought.

  6. Investigation of multiaxial molecular dynamics by 2H MAS NMR spectroscopy.

    Science.gov (United States)

    Kristensen, J H; Hoatson, G L; Vold, R L

    1998-11-01

    The technique of 2H MAS NMR spectroscopy is presented for the investigation of multiaxial molecular dynamics. To evaluate the effects of discrete random reorientation a Lie algebraic formalism based on the stochastic Liouville-von Neumann equation is developed. The solution to the stochastic Liouville-von Neumann equation is obtained both in the presence and absence of rf irradiation. This allows effects of molecular dynamics to be evaluated during rf pulses and extends the applicability of the formalism to arbitrary multiple pulse experiments. Theoretical methods are presented for the description of multiaxial dynamics with particular emphasis on the application of vector parameters to represent molecular rotations. Numerical time and powder integration algorithms are presented that are both efficient and easy to implement computationally. The applicability of 2H MAS NMR spectroscopy for investigating molecular dynamics is evaluated from theoretical spectra. To demonstrate the potential of the technique the dynamics of thiourea-2H4 is investigated experimentally. From a series of variable temperature MAS and quadrupole echo spectra it has been found that the dynamics can be described by composite rotation about the CS and CN bonds. Both experiments are sensitive to the fast CS rotation which is shown to be described by the Arrhenius parameters E(CS) = 46.4 +/- 2.3 kJ mol(-1) and ln(A(CS))= 32.6 +/- 0.9. The MAS experiment represents a significant improvement by simultaneously allowing the dynamics of the slow CN rotation to be fully characterized in terms of E(CN) = 56.3 +/- 3.4 kJ mol(-1) and ln(A(CN)) = 25.3 +/- 1.1.

  7. Low-power broadband solid-state MAS NMR of 14N

    Science.gov (United States)

    Pell, Andrew J.; Sanders, Kevin J.; Wegner, Sebastian; Pintacuda, Guido; Grey, Clare P.

    2017-05-01

    We propose two broadband pulse schemes for 14N solid-state magic-angle-spinning (MAS) nuclear magnetic resonance (NMR) that achieves (i) complete population inversion and (ii) efficient excitation of the double-quantum spectrum using low-power single-sideband-selective pulses. We give a comprehensive theoretical description of both schemes using a common framework that is based on the jolting-frame formalism of Caravatti et al. [J. Magn. Reson. 55, 88 (1983)]. This formalism is used to determine for the first time that we can obtain complete population inversion of 14N under low-power conditions, which we do here using single-sideband-selective adiabatic pulses. It is then used to predict that double-quantum coherences can be excited using low-power single-sideband-selective pulses. We then proceed to design a new experimental scheme for double-quantum excitation. The final double-quantum excitation pulse scheme is easily incorporated into other NMR experiments, as demonstrated here for double quantum-single quantum 14N correlation spectroscopy, and 1H-14N dipolar heteronuclear multiple-quantum correlation experiments. These pulses and irradiation schemes are evaluated numerically using simulations on single crystals and full powders, as well as experimentally on ammonium oxalate ((NH4)2C2O4) at moderate MAS and glycine at ultra-fast MAS. The performance of these new NMR methods is found to be very high, with population inversion efficiencies of 100% and double-quantum excitation efficiencies of 30%-50%, which are hitherto unprecedented for the low radiofrequency field amplitudes, up to the spinning frequency, that are used here.

  8. Separation of 2H MAS NMR Spectra by Two-Dimensional Spectroscopy

    Science.gov (United States)

    Kristensen, J. H.; Bildsøe, H.; Jakobsen, H. J.; Nielsen, N. C.

    1999-08-01

    New methods for optimum separation of 2H MAS NMR spectra are presented. The approach is based on hypercomplex spectroscopy that is useful for sign discrimination and phase separation. A new theoretical formalism is developed for the description of hypercomplex experiments. This exploits the properties of Lie algebras and hypercomplex numbers to obtain a solution to the Liouville-von Neumann equation. The solution is expressed in terms of coherence transfer functions that describe the allowed coherence transfer pathways in the system. The theoretical formalism is essential in order to understand all the features of hypercomplex experiments. The method is applied to the development of two-dimensional quadrupole-resolved 2H MAS NMR spectroscopy. The important features of this technique are discussed and two different versions are presented with widely different characteristics. An improved version of two-dimensional double-quantum 2H MAS NMR spectroscopy is developed. The conditions under which the double-quantum experiment is useful are discussed and its performance is compared with that observed for the quadrupole-resolved experiments. A general method is presented for evaluating the optimum pulse sequence parameters consistent with maximum sensitivity and resolution. This approach improves the performance of the experiments and is essential for any further development of the techniques. The effects of finite pulse width and hypercomplex data processing may lead to both intensity and phase distortions in the spectra. These effects are analyzed and general correction procedures are suggested. The techniques are applied to polycrystalline malonic-acid-2H4 for which the spinning sideband manifolds from the carboxyl and methylene deuterons are separated. The spinning sideband manifolds are simulated to determine the quadrupole parameters. The values are consistent with previous results, indicating that the techniques are both accurate and reliable.

  9. Structural characteristics of marine sedimentary humic acids by CP/MAS sup(13)C NMR spectroscopy

    Digital Repository Service at National Institute of Oceanography (India)

    Sardessai, S.; Wahidullah, S.

    stream_size 34319 stream_content_type text/plain stream_name Oceanol_Acta_21_543.pdf.txt stream_source_info Oceanol_Acta_21_543.pdf.txt Content-Encoding UTF-8 Content-Type text/plain; charset=UTF-8 OCEANOLOGICA ACTA... components of the: hydrolysate. 545 S. SARDESSAI, S. WAHlDULLAH 3.3 Nuclear magnetic resonance ~pe~t~Q~cQQy The cross-polarization technique with magic angle spin- ning (CP/MAS) was used to obtain 13C NMR spectra. Samples were thoroughly freeze...

  10. Assessing Heterogeneity of Osteolytic Lesions in Multiple Myeloma by 1H HR-MAS NMR Metabolomics

    Directory of Open Access Journals (Sweden)

    Laurette Tavel

    2016-10-01

    Full Text Available Multiple myeloma (MM is a malignancy of plasma cells characterized by multifocal osteolytic bone lesions. Macroscopic and genetic heterogeneity has been documented within MM lesions. Understanding the bases of such heterogeneity may unveil relevant features of MM pathobiology. To this aim, we deployed unbiased 1H high-resolution magic-angle spinning (HR-MAS nuclear magnetic resonance (NMR metabolomics to analyze multiple biopsy specimens of osteolytic lesions from one case of pathological fracture caused by MM. Multivariate analyses on normalized metabolite peak integrals allowed clusterization of samples in accordance with a posteriori histological findings. We investigated the relationship between morphological and NMR features by merging morphological data and metabolite profiling into a single correlation matrix. Data-merging addressed tissue heterogeneity, and greatly facilitated the mapping of lesions and nearby healthy tissues. Our proof-of-principle study reveals integrated metabolomics and histomorphology as a promising approach for the targeted study of osteolytic lesions.

  11. Bulk carbohydrate grain filling of barley ß-glucan mutants studied by 1H HR MAS NMR

    DEFF Research Database (Denmark)

    Seefeldt, Helene Fast; Larsen, Flemming Hofmann; Viereck, Nanna;

    2008-01-01

    ) during grain filling. For the first time, 1H HR MAS NMR spectra of flour from immature barley seeds are analyzed. Spectral assignments are made using two-dimensional (2D) NMR methods. Both α- and β-glucan biosynthesis were characterized by inspection of the spectra as well as by calibration......Temporal and genotypic differences in bulk carbohydrate accumulation in three barley genotypes differing in the content of mixed linkage β-(1→3),(1→4)-D-glucan (β-glucan) and starch were investigated using proton high-resolution, magic angle spinning, nuclear magnetic resonance (1H HR MAS NMR...

  12. Changes in Structural and Electronic Properties of the Zeolite Framework Induced by Extra-Framework Al and La in H-USY and La(x)NaY : A 29Si and 27Al MAS NMR and 27Al MQ MAS NMR Study

    NARCIS (Netherlands)

    Koningsberger, D.C.; Bokhoven, J.A. van; Roest, A.L.; Miller, J.T.; Nachtegaal, G.H,; Kentgens, A.

    2000-01-01

    A 27Al 3Q MAS, a quantitative 27Al MAS, and a 29Si MAS NMR study has been carried out on La(x)NaY and H-USY. Assignment of the different types of Al coordinations has been done using the results of the MQ MAS experiments. The 29Si MAS and 27Al MAS NMR results obtained at high fields (14.1 T) and

  13. Conformational analysis of capsaicin using 13C, 15N MAS NMR, GIAO DFT and GA calculations

    Science.gov (United States)

    Siudem, Paweł; Paradowska, Katarzyna; Bukowicki, Jarosław

    2017-10-01

    Capsaicin produced by plants from genus Capsicum exerts multiple pharmacological effects and has found applications in food and pharmaceutical industry. The alkaloid was studied by a combined approach: solid-state NMR, GA conformational search and GIAO DFT methods. The 13C CPMAS NMR spectra were recorded using variable contact time and dipolar dephasing experiments. The results of cross-polarization (CP) kinetics, such as TCP values and long T1ρH (100-200 ms), indicated that the capsaicin molecule is fairly mobile, especially at the end of the aliphatic chain. The15N MAS NMR spectrum showed one narrow signal at -255 ppm. Genetic algorithm (GA) search with multi modal optimization was used to find low-energy conformations of capsaicin. Theoretical GIAO DFT calculations were performed using different basis sets to characterize five selected conformations. 13C CPMAS NMR was used as a validation method and the experimental chemical shifts were compared with those calculated for selected stable conformers. Conformational analysis suggests that the side chain can be bent or extended. A comparison of the experimental and the calculated chemical shifts indicates that solid capsaicin does not have the same structure as those established by PWXRD.

  14. Indirect detection of infinite-speed MAS solid-state NMR spectra

    Science.gov (United States)

    Perras, Frédéric A.; Venkatesh, Amrit; Hanrahan, Michael P.; Goh, Tian Wei; Huang, Wenyu; Rossini, Aaron J.; Pruski, Marek

    2017-03-01

    Heavy spin-1/2 nuclides are known to possess very large chemical shift anisotropies that can challenge even the most advanced magic-angle-spinning (MAS) techniques. Wide manifolds of overlapping spinning sidebands and insufficient excitation bandwidths often obfuscate meaningful spectral information and force the use of static, low-resolution solid-state (SS)NMR methods for the characterization of materials. To address these issues, we have merged fast-magic-angle-turning (MAT) and dipolar heteronuclear multiple-quantum coherence (D-HMQC) experiments to obtain D-HMQC-MAT pulse sequences which enable the rapid acquisition of 2D SSNMR spectra that correlate isotropic 1H chemical shifts to the indirectly detected isotropic "infinite-MAS" spectra of heavy spin-1/2 nuclides. For these nuclides, the combination of fast MAS and 1H detection provides a high sensitivity, which rivals the DNP-enhanced ultra-wideline SSNMR. The new pulse sequences were used to determine the Pt coordination environments in a complex mixture of decomposition products of transplatin and in a metal-organic framework with Pt ions coordinated to the linker ligands.

  15. Lipid bilayer-bound conformation of an integral membrane beta barrel protein by multidimensional MAS NMR

    Energy Technology Data Exchange (ETDEWEB)

    Eddy, Matthew T. [The Scripps Research Institute, Department of Integrative Structural and Computational Biology (United States); Su, Yongchao; Silvers, Robert; Andreas, Loren; Clark, Lindsay [Massachusetts Institute of Technology, Department of Chemistry (United States); Wagner, Gerhard [Harvard Medical School, Department of Biological Chemistry and Molecular Pharmacology (United States); Pintacuda, Guido; Emsley, Lyndon [Université de Lyon, Centre de RMN à Très Hauts Champs, Institut des Sciences Analytiques (CNRS, ENS Lyon, UCB Lyon 1) (France); Griffin, Robert G., E-mail: rgg@mit.edu [Massachusetts Institute of Technology, Department of Chemistry (United States)

    2015-04-15

    The human voltage dependent anion channel 1 (VDAC) is a 32 kDa β-barrel integral membrane protein that controls the transport of ions across the outer mitochondrial membrane. Despite the determination of VDAC solution and diffraction structures, a structural basis for the mechanism of its function is not yet fully understood. Biophysical studies suggest VDAC requires a lipid bilayer to achieve full function, motivating the need for atomic resolution structural information of VDAC in a membrane environment. Here we report an essential step toward that goal: extensive assignments of backbone and side chain resonances for VDAC in DMPC lipid bilayers via magic angle spinning nuclear magnetic resonance (MAS NMR). VDAC reconstituted into DMPC lipid bilayers spontaneously forms two-dimensional lipid crystals, showing remarkable spectral resolution (0.5–0.3 ppm for {sup 13}C line widths and <0.5 ppm {sup 15}N line widths at 750 MHz). In addition to the benefits of working in a lipid bilayer, several distinct advantages are observed with the lipid crystalline preparation. First, the strong signals and sharp line widths facilitated extensive NMR resonance assignments for an integral membrane β-barrel protein in lipid bilayers by MAS NMR. Second, a large number of residues in loop regions were readily observed and assigned, which can be challenging in detergent-solubilized membrane proteins where loop regions are often not detected due to line broadening from conformational exchange. Third, complete backbone and side chain chemical shift assignments could be obtained for the first 25 residues, which comprise the functionally important N-terminus. The reported assignments allow us to compare predicted torsion angles for VDAC prepared in DMPC 2D lipid crystals, DMPC liposomes, and LDAO-solubilized samples to address the possible effects of the membrane mimetic environment on the conformation of the protein. Concluding, we discuss the strengths and weaknesses of the

  16. 13C CP/MAS NMR and DFT studies of thiazides

    Science.gov (United States)

    Latosińska, J. N.

    2003-02-01

    The 13C MAS solid state NMR spectra of four sulphonamide derivatives of 1,2,4-benzothiadiazine-1,1-dioxides, commonly known as thiazides, were recorded and the chemical shifts and chemical shift anisotropy (CSA) were measured. Analysis of the experimental 13C shielding parameters was supported by DFT theoretical calculations carried out within the gauge-including atomic orbital (GIAO), semiempirical Typed Neglect of Differential Overlap (TNDO/2) approach and by the spectra estimations performed by ChemNMR Pro 6.0, ACD-I/LAB, SpecInfo and gNMR. It was found that the chemical shifts obtained with ChemNMR Pro 6.0, ACD-I/LAB, SpecInfo and gNMR were insensitive to the substitution effects, whereas the semiempirical TNDO/2 and density functional theory (DFT) B3LYP/6-311+G(2d,p) methods allowed estimation of the influence of substituents on the chemical shielding and consequently, the chemical shift. The influence of the substituents at C3 position of the ring on the chemical shifts was analysed on the basis of the experimental data and results of the DFT calculations. The values of the chemical shifts and the low values of the anisotropy parameter for the C3 atom in HCTZ, TCTZ and ATZ, strongly indicated that three thiazides HCTZ, TCTZ and ATZ occurred in the form of HCTZ type with the C3 carbon atom participating in a single bond. The following ordering of the substituents according to the increasing electron accepting properties was found: -H<-CH 2SCH 2CHCH 2<-CHCl 2. A detailed analysis of the inductive and coupling effects was made on the basis of 13C chemical shifts and chemical shielding tensor asymmetry parameters on the C3 and C6 carbon atoms.

  17. Proton detection of MAS solid-state NMR spectra of half-integer quadrupolar nuclei.

    Science.gov (United States)

    Venkatesh, Amrit; Hanrahan, Michael P; Rossini, Aaron J

    Fast magic angle spinning (MAS) and proton detection has found widespread application to enhance the sensitivity of solid-state NMR experiments with spin-1/2 nuclei such as (13)C, (15)N and (29)Si, however, this approach is not yet routinely applied to half-integer quadrupolar nuclei. Here we have investigated the feasibility of using fast MAS and proton detection to enhance the sensitivity of solid-state NMR experiments with half-integer quadrupolar nuclei. The previously described dipolar hetero-nuclear multiple quantum correlation (D-HMQC) and dipolar refocused insensitive nuclei enhanced by polarization transfer (D-RINEPT) pulse sequences were used for proton detection of half-integer quadrupolar nuclei. Quantitative comparisons of signal-to-noise ratios and the sensitivity of proton detected D-HMQC and D-RINEPT and direct detection spin echo and quadrupolar Carr-Purcell Meiboom-Gill (QCPMG) solid-state NMR spectra, demonstrate that one dimensional proton detected experiments can provide sensitivity similar to or exceeding that obtainable with direct detection QCPMG experiments. 2D D-HMQC and D-RINEPT experiments provide less sensitivity than QCPMG experiments but proton detected 2D hetero-nuclear correlation solid-state NMR spectra of half-integer nuclei can still be acquired in about the same time as a 1D spin echo spectrum. Notably, the rarely used D-RINEPT pulse sequence is found to provide similar, or better sensitivity than D-HMQC in some cases. Proton detected D-RINEPT benefits from the short longitudinal relaxation times (T1) normally associated with half-integer quadrupolar nuclei, it can be combined with existing signal enhancement methods for quadrupolar nuclei, and t1-noise in the indirect dimension can easily be removed by pre-saturation of the (1)H nuclei. The rapid acquisition of proton detected 2D HETCOR solid-state NMR spectra of a range of half-integer quadrupolar nuclei such as (17)O, (27)Al, (35)Cl and (71)Ga is demonstrated. Copyright

  18. Quantitative and Structure Analysis of Cellulose in Tobacco by 13C CP / MAS NMR Spectroscopy

    Directory of Open Access Journals (Sweden)

    Zhu Xiaolan

    2016-07-01

    Full Text Available A new method utilizing 13C cross-polarization/magic angle spinning (CP/MAS nuclear magnetic resonance (NMR spectra was developed for the simultaneous quantitative determination and structure analysis of tobacco cellulose from hot water or acid detergent extraction. A reference spectrum of tobacco noncellulose components was subtracted from the spectrum of each sample to obtain a subspectrum of the cellulose components. The NMR spectra in combination with spectral fitting were analyzed in detail and some parameters, such as the content of cellulose, crystallinity, allomorph composition and lateral dimensions for cellulose elementary fibrils and microfibrils were determined. The quantitative results showed that the average recovery was 94.0% with a relative standard deviation (RSD of 4.6–4.8%. The structure results obtained by the spectral fitting for the cellulose C1-region showed that the main allomorph composition in tobacco cellulose was Iβ. The cellulose crystallinity calculated by the spectral fitting in C4 -region was about 50%. The lateral dimensions for cellulose elementary fibrils and microfibrils were in the range of 3.0–6.0 nm and 6.0–13.0 nm, respectively. Therefore, this NMR method could provide important information on both amount and structure of cellulose in tobacco.

  19. Water suppression without signal loss in HR-MAS 1H NMR of cells and tissues

    Science.gov (United States)

    Chen, Jin-Hong; Sambol, Elliot B.; Kennealey, Peter T.; O'Connor, Rachael B.; DeCarolis, Penelope L.; Cory, David G.; Singer, Samuel

    2004-11-01

    In cell and tissue samples, water is normally three orders of magnitude more abundant than other metabolites. Thus, water suppression is required in the acquisition of NMR spectra to overcome the dynamic range problem and to recover metabolites that overlap with the broad baseline of the strong water resonance. However, the heterogeneous cellular environment often complicates water suppression and the strong coupling of water to membrane lipids interferes with the NMR detection of membrane associated lipid components. The widely used water suppression techniques including presaturation and double pulsed field gradient selective echo result in more than a 70% reduction in membrane associated lipid components in proton spectra of cells and tissues compared to proton spectra acquired in the absence of water suppression. A water suppression technique based on the combination of selective excitation pulses and pulsed field gradients is proposed to use in the acquisition of high resolution MAS NMR spectra of tissue specimens and cell samples. This pulse sequence methodology enables efficient water suppression for intact cells and tissue samples and eliminates signal loss from cellular metabolites.

  20. Molecular degradation of ancient documents revealed by 1H HR-MAS NMR spectroscopy

    Science.gov (United States)

    Corsaro, Carmelo; Mallamace, Domenico; Łojewska, Joanna; Mallamace, Francesco; Pietronero, Luciano; Missori, Mauro

    2013-10-01

    For centuries mankind has stored its knowledge on paper, a remarkable biomaterial made of natural cellulose fibers. However, spontaneous cellulose degradation phenomena weaken and discolorate paper over time. The detailed knowledge of products arising from cellulose degradation is essential in understanding deterioration pathways and in improving durability of cultural heritage. In this study, for the first time, products of cellulose degradation were individually detected in solid paper samples by means of an extremely powerful proton HR-MAS NMR set-up, in combination to a wise use of both ancient and, as reference, artificially aged paper samples. Carboxylic acids, in addition to more complex dicarboxylic and hydroxy-carboxylic acids, were found in all samples studied. Since these products can catalyze further degradation, their knowledge is fundamental to improve conservation strategies of historical documents. Furthermore, the identification of compounds used in ancient production techniques, also suggests for artifacts dating, authentication and provenance.

  1. 1H MAS NMR spectra of hy- droxyl species on diatomite surface

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    High spinning speed 1H magic-angle spinning nuclear magnetic resonance (1H MAS NMR) was used to detect surface hydroxyl groups of diatomite, which include isolated hydroxyl groups and hydrogen-bonded hydroxyl groups, and water adsorbed on diatomite surface that include pore water and hydrogen-bonded water. The corresponding proton chemical shifts of above species are ca. 2.0, 6.0-7.1, 4.9 and 3.0 respectively. Accompanied by thermal treatment temperature ascending, the pore water and hydrogen-bonded water are desorbed successively. As a result, the relative intensities of the peaks assigned to protons of isolat-ed hydroxyl groups and hydrogen-bonded hydroxyl groups increase gradually and reach their maxima at 1000℃. After 1100℃ calcination, the hydroxyl groups that classified to strongly hydrogen-bonded ones and the isolated hydroxyl groups condense basically. But some weakly hydrogen-bonded hydroxyl groups may still persist in the micropores.

  2. Assessing the fate and transformation of plant residues in the terrestrial environment using HR-MAS NMR spectroscopy

    Science.gov (United States)

    Kelleher, Brian P.; Simpson, Myrna J.; Simpson, Andre J.

    2006-08-01

    Plant litter decomposition plays a fundamental role in carbon and nitrogen cycles, provides key nutrients to the soil environment and represents a potentially large positive feedback to atmospheric CO 2. However, the full details of decomposition pathways and products are unknown. Here we present the first application of HR-MAS NMR spectroscopy on 13C and 15N labeled plant materials, and apply this approach in a preliminary study to monitor the environmental degradation of the pine and wheatgrass residues over time. In HR-MAS, is it possible to acquire very high resolution NMR data of plant biomass, and apply the vast array of multidimensional experiments available in conventional solution-state NMR. High levels of isotopic enrichment combined with HR-MAS significantly enhance the detection limits, and provide a wealth of information that is unattainable by any other method. Diffusion edited HR-MAS NMR data reveal the rapid loss of carbohydrate structures, while two-dimensional (2-D) HR-MAS NMR spectra demonstrate the relatively fast loss of both hydrolysable and condensed tannin structures from all plant tissues studied. Aromatic (partially lignin) and aliphatic components (waxes, cuticles) tend to persist, along with a small fraction of carbohydrate, and become highly functionalized over time. While one-dimensional (1-D) 13C HR-MAS NMR spectra of fresh plant tissue reflect compositional differences between pine and grass, these differences become negligible after decomposition suggesting that recalcitrant carbon may be similar despite the plant source. Two-dimensional 1H- 15N HR-MAS NMR analysis of the pine residue suggests that nitrogen from specific peptides is either selectively preserved or used for the synthesis of what appears to be novel structures. The amount of relevant data generated from plant components in situ using HR-MAS NMR is highly encouraging, and demonstrates that complete assignment will yield unprecedented structural knowledge of plant cell

  3. Supra-molecular structure and chemical reactivity of cellulose I studied using CP/MAS (sup)13 C-NMR

    CSIR Research Space (South Africa)

    Chunilall, Viren

    2013-08-01

    Full Text Available medium, provided the original work is properly cited. Supra-Molecular Structure and Chemical Reactivity of Cellulose I Studied Using CP/MAS 13C-NMR Viren Chunilall, Tamara Bush and Per Tomas Larsson Additional information is available at the end... of Cellulose I Studied Using CP/MAS 13C-NMR 71 1.1.2. Dissolving pulp The unbleached pulp that results after acid bi-sulphite pulping is used as raw material for dissolving pulp production. Lignin and hemicelluloses in the unbleached pulp are considered...

  4. Relation Between Acid and Catalytic Properties of Chlorinated Gamma-Alumina. a 31p Mas Nmr and Ftir Investigation

    Directory of Open Access Journals (Sweden)

    Guillaume D.

    1999-07-01

    Full Text Available In this paper, we have studied the effect of chlorine on the surface properties of gamma-alumina, especially on their acid properties. The use of FTIR spectroscopy and 31P MAS NMR of adsorbed trimethylphosphine allows to propose a chlorination mechanism. To correlate the surface properties of these chlorinated gamma-alumina with their catalytic properties, we have used a model reaction, the cracking of n-heptane under reforming conditions. The analysis of the correlation between acid properties determined by 31P MAS NMR and the catalytic results (in terms of activities and selectivities allows to identify which sites are involved in the cracking reaction.

  5. Evidence for cross-linking in tomato cutin using HR-MAS NMR spectroscopy.

    Science.gov (United States)

    Deshmukh, Ashish P; Simpson, André J; Hatcher, Patrick G

    2003-11-01

    Cutin is a polyester biopolymer component of plant leaf and fruit cuticles, most often associated with waxes and cuticular polysaccharides, and sometimes with another aliphatic biopolymer called cutan. Insolubility of these cuticular biopolymers has made it difficult to apply traditional analytical techniques for structure determination, because most techniques providing molecular level details require solubility. By using the relatively new technique of one and two-dimensional high-resolution magic angle spinning (HR-MAS) NMR spectroscopy, with added information from solid-state 13C NMR spectroscopy, detailed through-bond connectivities and assignments are made for cutin from Lycopersicon esculentum (tomato) fruit. Based on the data obtained, tomato cutin is found to be predominantly an aliphatic polyester with some olefinic and aromatic moieties, consistent with previous studies that employed various degradative approaches. Aside from esters, there are free primary and secondary alcohol groups, as well as free fatty acids. A significant finding is the presence of alpha-branched fatty acids/esters. Mid-chain hydroxyls appear to be generally unesterified, but esters of mid-chain hydroxyls have been identified. The alpha-branched fatty acids/esters and esters of mid-chain hydroxyls could point towards cross-linking.

  6. 1H HR-MAS NMR of carotenoids in aqueous samples and raw vegetables.

    Science.gov (United States)

    Miglietta, M L; Lamanna, R

    2006-07-01

    Carotenoids are linear C40 tetraterpenoid hydrocarbons and represent a wide category of natural pigments. They are components of the pigment system of chloroplasts and are involved in the primary light absorption and the photon canalization of photosynthesis. Moreover, they also behave as quenchers of singlet oxygen, protecting cells and organisms against lipid peroxidation. Carotenoids have a strong lipophilic character and are usually analyzed in organic solvents. However, because of their biological activity, the characterization of these compounds in an aqueous environment or in the natural matrix is very important. One of the most important dietary carotenoids is beta-carotene, which has been extensively studied both in vivo and in model systems, but because of the low concentration and strong interaction with the biological matrix, beta-carotene has never been observed by NMR in solid aqueous samples.In the present work, a model system has been developed for the detection and identification of beta-carotene in solid aqueous samples by 1H HR-MAS NMR. The efficiency of the model has led to the identification of beta-carotene in a raw vegetable matrix.

  7. Heating and temperature gradients of lipid bilayer samples induced by RF irradiation in MAS solid-state NMR experiments.

    Science.gov (United States)

    Wang, Jing; Zhang, Zhengfeng; Zhao, Weijing; Wang, Liying; Yang, Jun

    2016-05-09

    The MAS solid-state NMR has been a powerful technique for studying membrane proteins within the native-like lipid bilayer environment. In general, RF irradiation in MAS NMR experiments can heat and potentially destroy expensive membrane protein samples. However, under practical MAS NMR experimental conditions, detailed characterization of RF heating effect of lipid bilayer samples is still lacking. Herein, using (1) H chemical shift of water for temperature calibration, we systematically study the dependence of RF heating on hydration levels and salt concentrations of three lipids in MAS NMR experiments. Under practical (1) H decoupling conditions used in biological MAS NMR experiments, three lipids show different dependence of RF heating on hydration levels as well as salt concentrations, which are closely associated with the properties of lipids. The maximum temperature elevation of about 10 °C is similar for the three lipids containing 200% hydration, which is much lower than that in static solid-state NMR experiments. The RF heating due to salt is observed to be less than that due to hydration, with a maximum temperature elevation of less than 4 °C in the hydrated samples containing 120 mmol l(-1) of salt. Upon RF irradiation, the temperature gradient across the sample is observed to be greatly increased up to 20 °C, as demonstrated by the remarkable broadening of (1) H signal of water. Based on detailed characterization of RF heating effect, we demonstrate that RF heating and temperature gradient can be significantly reduced by decreasing the hydration levels of lipid bilayer samples from 200% to 30%. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  8. 1H and 13C HR-MAS NMR investigations on native and enzymatically digested bovine nasal cartilage.

    Science.gov (United States)

    Schiller, J; Naji, L; Huster, D; Kaufmann, J; Arnold, K

    2001-08-01

    Rheumatic diseases are accompanied by a progressive destruction of the cartilage layer of the joints. Despite the frequency of the disease, degradation mechanisms are not yet understood and methods for early diagnosis are not available. Although some information on pathogenesis could be obtained from the analysis of degradation products of cartilage supernatants, the most direct information on degradation processes would come from the native cartilage as such. We have used 1H as well as 13C HR-MAS (high resolution magic angle spinning) NMR spectroscopy to obtain suitable line-widths of NMR resonances of native cartilage. 1D and 2D NMR spectra of native cartilage were compared with those of enzymatically-treated (collagenase and papain) samples. In the 1H NMR spectra of native cartilage, resonances of polysaccharides, lipids and a few amino acids of collagen were detectable, whereas the 13C NMR spectra primarily indicated the presence of chondroitin sulfate. Treatment with papain resulted only in small changes in the 1H NMR spectrum, whereas a clear diminution of all resonances was detectable in the 13C NMR spectra. On the other hand, treatment with collagenase caused the formation of peptides with an amino acid composition typical for collagen (glycine, proline, hydroxyproline and lysine). It is concluded that the HR-MAS NMR spectra of cartilage may be of significance for the investigation of cartilage degradation since they allow the fast evaluation of cartilage composition and only very small amounts of sample are required.

  9. Proton chemical shift tensors determined by 3D ultrafast MAS double-quantum NMR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Rongchun; Mroue, Kamal H.; Ramamoorthy, Ayyalusamy, E-mail: ramamoor@umich.edu [Biophysics and Department of Chemistry, The University of Michigan, Ann Arbor, Michigan 48109-1055 (United States)

    2015-10-14

    Proton NMR spectroscopy in the solid state has recently attracted much attention owing to the significant enhancement in spectral resolution afforded by the remarkable advances in ultrafast magic angle spinning (MAS) capabilities. In particular, proton chemical shift anisotropy (CSA) has become an important tool for obtaining specific insights into inter/intra-molecular hydrogen bonding. However, even at the highest currently feasible spinning frequencies (110–120 kHz), {sup 1}H MAS NMR spectra of rigid solids still suffer from poor resolution and severe peak overlap caused by the strong {sup 1}H–{sup 1}H homonuclear dipolar couplings and narrow {sup 1}H chemical shift (CS) ranges, which render it difficult to determine the CSA of specific proton sites in the standard CSA/single-quantum (SQ) chemical shift correlation experiment. Herein, we propose a three-dimensional (3D) {sup 1}H double-quantum (DQ) chemical shift/CSA/SQ chemical shift correlation experiment to extract the CS tensors of proton sites whose signals are not well resolved along the single-quantum chemical shift dimension. As extracted from the 3D spectrum, the F1/F3 (DQ/SQ) projection provides valuable information about {sup 1}H–{sup 1}H proximities, which might also reveal the hydrogen-bonding connectivities. In addition, the F2/F3 (CSA/SQ) correlation spectrum, which is similar to the regular 2D CSA/SQ correlation experiment, yields chemical shift anisotropic line shapes at different isotropic chemical shifts. More importantly, since the F2/F1 (CSA/DQ) spectrum correlates the CSA with the DQ signal induced by two neighboring proton sites, the CSA spectrum sliced at a specific DQ chemical shift position contains the CSA information of two neighboring spins indicated by the DQ chemical shift. If these two spins have different CS tensors, both tensors can be extracted by numerical fitting. We believe that this robust and elegant single-channel proton-based 3D experiment provides useful atomistic

  10. 1MAS NMR spectra of kao linite/formamide intercalation compound

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    The high spinning speed 1H magic angle spinning nuclear magnetic resonance (1H MAS NMR) technique was employed to distinguish the two groups of surface hydroxyls of kaolinite and investigate the intercalation mechanism of kaolinite/formamide compound. The proton chemical shifts of the inner hydroxyl and inner surface hydroxyl of kaolinte are in the range of δ-1.3-0.9 and δ 2.4-3.0 respectively. After formamide intercalation three proton peaks were detected. The proton peak of the inner surface hydroxyls of the intercalation compound shifts to high-field with δ 2.3-2.7, which is assigned to the formation of the hydrogen bond between the inner surface hydroxyl and formamide carbonyl group. Whereas, the proton peak of the inner hydroxyl shifts to δ-0.3 toward low-field, that is attributed to van der Waal's effect between the inner hydroxyl proton and the amino group proton of the formamide which may be keyed into the ditrigonal hole of the kaolinite. The third peak, additional proton peak, is in the range of δ5.4-5.6, that is ascribed to the hydrogen bond formation between the amino group proton of formimide and SiO4 tetrahedral oxygen of the kaolinite.

  11. Study on Nitrogen Forms in Phenolic Polymers Incorporating Protien by 15N CP—MAS NMR

    Institute of Scientific and Technical Information of China (English)

    CHENGLILI; WENQIXIAO; 等

    1996-01-01

    Phenolic polymers synthesized by reactions by reactions of p-benzoquinone with 15N-labelled protein or (15NH4)2SO4 were studied by using 15N CP-MAS NMR technique in combination with chemical approaches.Results showed that more than 80% of nitrogen in quinone-protein polymers was in the form of amide with some present as aromatic and /or aliphatic amine and less than 10% of nitrogen occurred as heterocyclic N.The nitrogen distribution in the non-hydrolyzable residue of the quinone-protein polymers was basically similar to that of soil humic acid reported in literature with the exception that a higher proportion of N as heterocyclic N and aromatic amine and a lower proportion of N as amide and aliphatic amine were found in the former than in the latter,More than 70% of total nitrogen in quinone-(NH4)2OS4 polymer was acid resistant ,of which about 53% occurred as pyrrole,nitrile and imion type N.The possible roles of the reactions of phenols or quinones with proteins in the formation of humic acid.especially the non-hydrolyzable nitrogen in humicacid,are discussed.

  12. High-resolution (19)F MAS NMR spectroscopy: structural disorder and unusual J couplings in a fluorinated hydroxy-silicate.

    Science.gov (United States)

    Griffin, John M; Yates, Jonathan R; Berry, Andrew J; Wimperis, Stephen; Ashbrook, Sharon E

    2010-11-10

    High-resolution (19)F magic angle spinning (MAS) NMR spectroscopy is used to study disorder and bonding in a crystalline solid. (19)F MAS NMR reveals four distinct F sites in a 50% fluorine-substituted deuterated hydrous magnesium silicate (clinohumite, 4Mg(2)SiO(4)·Mg(OD(1-x)F(x))(2) with x = 0.5), indicating extensive structural disorder. The four (19)F peaks can be assigned using density functional theory (DFT) calculations of NMR parameters for a number of structural models with a range of possible local F environments generated by F(-)/OH(-) substitution. These assignments are supported by two-dimensional (19)F double-quantum MAS NMR experiments that correlate F sites based on either spatial proximity (via dipolar couplings) or through-bond connectivity (via scalar, or J, couplings). The observation of (19)F-(19)F J couplings is unexpected as the fluorines coordinate Mg atoms and the Mg-F interaction is normally considered to be ionic in character (i.e., there is no formal F-Mg-F covalent bonding arrangement). However, DFT calculations predict significant (19)F-(19)F J couplings, and these are in good agreement with the splittings observed in a (19)F J-resolved MAS NMR experiment. The existence of these J couplings is discussed in relation to both the nature of bonding in the solid state and the occurrence of so-called "through-space" (19)F-(19)F J couplings in solution. Finally, we note that we have found similar structural disorder and spin-spin interactions in both synthetic and naturally occurring clinohumite samples.

  13. DRIFT and HR MAS NMR characterization of humic substances from a soil treated with different organic and mineral fertilizers

    Science.gov (United States)

    Ferrari, Erika; Francioso, Ornella; Nardi, Serenella; Saladini, Monica; Ferro, Nicola Dal; Morari, Francesco

    2011-07-01

    In this study, using DRIFT and HR MAS NMR, we analyzed the humic substances isolated from a soil treated, over 40 years, with different organic, mineral and organic plus mineral treatments and cultivated with maize as the main crop. As expected, the structure of humic substances was very complex but by combining both techniques (DRIFT and HR MAS NMR) additional information was obtained on aromatic and aliphatic components, the most recalcitrant parts of these macromolecules. In so doing we wanted to investigate the relationship between HS structure and long-term management practices. An elevated content of lignin, aminoacids, peptides and proteins was observed mainly for farmyard manure treatments with respect to mineral or liquid manure amendments; this supports how the different management practices have greatly influenced the humification process of cultivated soils.

  14. Thermal maturity of type II kerogen from the New Albany Shale assessed by13C CP/MAS NMR

    Science.gov (United States)

    Werner-Zwanziger, U.; Lis, G.; Mastalerz, Maria; Schimmelmann, A.

    2005-01-01

    Thermal maturity of oil and gas source rocks is typically quantified in terms of vitrinite reflectance, which is based on optical properties of terrestrial woody remains. This study evaluates 13C CP/MAS NMR parameters in kerogen (i.e., the insoluble fraction of organic matter in sediments and sedimentary rocks) as proxies for thermal maturity in marine-derived source rocks where terrestrially derived vitrinite is often absent or sparse. In a suite of samples from the New Albany Shale (Middle Devonian to the Early Mississippian, Illinois Basin) the abundance of aromatic carbon in kerogen determined by 13C CP/MAS NMR correlates linearly well with vitrinite reflectance. ?? 2004 Elsevier Inc. All rights reserved.

  15. 1H MAS NMR characterization of hydrogen over silica-supported rhodium catalyst

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Hydrogen species in both SiO2 and Rh/SiO2 catalysts pretreated indifferent atmospheres (H2, O2, helium or air) at different temperatures (773 or 973 K) were investigated by means of 1H MAS NMR. In SiO2 and O2-pretreated catalysts, a series of downfield signals at ~7.0, 3.8-4.0, 2.0 and 1.5-1.0 were detected. The first two signals can be attributed to strongly adsorbed and physisorbed water and the others to terminal silanol (SiOH) and SiOH under the screening of oxygen vacancies in SiO2 lattice, respectively. Besides the above signals, both upfield signal at ~-110 and downfield signals at 3.0 and 0.0 were also detected in H2-pretreated catalyst, respectively. The upfield signal at ~-110 originated from the dissociative adsorption of H2 over rhodium and was found to consist of both the contributions of reversible and irreversible hydrogen. There also probably existed another dissociatively adsorbed hydrogen over rhodium, which was known to be b hydrogen and in a unique form of "delocalized hydrogen". It was presumed that the b hydrogen had an upfield shift of ca. -20- -50, though its 1H NMR signals, which, having been masked by the spinning sidebands of Si-OH, failed to be directly detected out. The downfield signal at 3.0 was assigned to spillover hydrogen weakly bound by the bridge oxygen of SiO2. Another downfield signal at 0.0 was assigned to hydrogen held in the oxygen vacancies of SiO2 (Si-H species), suffering from the screening of trapped electrons. Both the spillover hydrogen and the Si-H resulted from the migration of the reversible hydrogen and the b hydrogen from rhodium to SiO2 in the close vicinity. It was proved that the above migration of hydrogen was preferred to occur at higher temperature than at lower temperature.

  16. Molecular dynamics of spider dragline silk fiber investigated by 2H MAS NMR.

    Science.gov (United States)

    Shi, Xiangyan; Holland, Gregory P; Yarger, Jeffery L

    2015-03-09

    The molecular dynamics of the proteins that comprise spider dragline silk were investigated with solid-state (2)H magic angle spinning (MAS) NMR line shape and spin-lattice relaxation time (T1) analysis. The experiments were performed on (2)H/(13)C/(15)N-enriched N. clavipes dragline silk fibers. The silk protein side-chain and backbone dynamics were probed for Ala-rich regions (β-sheet and 31-helical domains) in both native (dry) and supercontracted (wet) spider silk. In native (dry) silk fibers, the side chains in all Ala containing regions undergo similar fast methyl rotations (>10(9) s(-1)), while the backbone remains essentially static (silk is wet and supercontracted, the presence of water initiates fast side-chain and backbone motions for a fraction of the β-sheet region and 31-helicies. β-Sheet subregion 1 ascribed to the poly(Ala) core exhibits slower dynamics, while β-sheet subregion 2 present in the interfacial, primarily poly(Gly-Ala) region that links the β-sheets to disordered 31-helical motifs, exhibits faster motions when the silk is supercontracted. Particularly notable is the observation of microsecond backbone motions for β-sheet subregion 2 and 31-helicies. It is proposed that these microsecond backbone motions lead to hydrogen-bond disruption in β-sheet subregion 2 and helps to explain the decrease in silk stiffness when the silk is wet and supercontracted. In addition, water mobilizes and softens 31-helical motifs, contributing to the increased extensibility observed when the silk is in a supercontracted state. The present study provides critical insight into the supercontraction mechanism and corresponding changes in mechanical properties observed for spider dragline silks.

  17. Characterizing crystal disorder of trospium chloride: a comprehensive,(13) C CP/MAS NMR, DSC, FTIR, and XRPD study.

    Science.gov (United States)

    Urbanova, Martina; Sturcova, Adriana; Brus, Jiri; Benes, Hynek; Skorepova, Eliska; Kratochvil, Bohumil; Cejka, Jan; Sedenkova, Ivana; Kobera, Libor; Policianova, Olivia; Sturc, Antonin

    2013-04-01

    Analysis of C cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance (NMR), differential scanning calorimetry (DSC), Fourier transform infrared (FTIR), and X-ray powder diffraction data of trospium chloride (TCl) products crystallized from different mixtures of water-ethanol [φ(EtOH) = 0.5-1.0] at various temperatures (0°C, 20°C) and initial concentrations (saturated solution, 30%-50% excess of solvent) revealed extensive structural variability of TCl. Although (13) C CP/MAS NMR spectra indicated broad variety of structural phases arising from molecular disorder, temperature-modulated DSC identified presence of two distinct components in the products. FTIR spectra revealed alterations in the hydrogen bonding network (ionic hydrogen bond formation), whereas the X-ray diffraction reflected unchanged unit cell parameters. These results were explained by a two-component character of TCl products in which a dominant polymorphic form is accompanied by partly separated nanocrystalline domains of a secondary phase that does not provide clear Bragg reflections. These phases slightly differ in the degree of molecular disorder, in the quality of crystal lattice and hydrogen bonding network. It is also demonstrated that, for the quality control of such complex products, (13) C CP/MAS NMR spectroscopy combined with factor analysis (FA) can satisfactorily be used for categorizing the individual samples: FA of (13) C CP/MAS NMR spectra found clear relationships between the extent of molecular disorder and crystallization conditions. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 102:1235-1248, 2013.

  18. Characterization of solid polymer dispersions of active pharmaceutical ingredients by 19F MAS NMR and factor analysis

    Science.gov (United States)

    Urbanova, Martina; Brus, Jiri; Sedenkova, Ivana; Policianova, Olivia; Kobera, Libor

    In this contribution the ability of 19F MAS NMR spectroscopy to probe structural variability of poorly water-soluble drugs formulated as solid dispersions in polymer matrices is discussed. The application potentiality of the proposed approach is demonstrated on a moderately sized active pharmaceutical ingredient (API, Atorvastatin) exhibiting extensive polymorphism. In this respect, a range of model systems with the API incorporated in the matrix of polvinylpyrrolidone (PVP) was prepared. The extent of mixing of both components was determined by T1(1H) and T1ρ(1H) relaxation experiments, and it was found that the API forms nanosized domains. Subsequently it was found out that the polymer matrix induces two kinds of changes in 19F MAS NMR spectra. At first, this is a high-frequency shift reaching 2-3 ppm which is independent on molecular structure of the API and which results from the long-range polarization of the electron cloud around 19F nucleus induced by electrostatic fields of the polymer matrix. At second, this is broadening of the signals and formation of shoulders reflecting changes in molecular arrangement of the API. To avoid misleading in the interpretation of the recorded 19F MAS NMR spectra, because both the contributions act simultaneously, we applied chemometric approach based on multivariate analysis. It is demonstrated that factor analysis of the recorded spectra can separate both these spectral contributions, and the subtle structural differences in the molecular arrangement of the API in the nanosized domains can be traced. In this way 19F MAS NMR spectra of both pure APIs and APIs in solid dispersions can be directly compared. The proposed strategy thus provides a powerful tool for the analysis of new formulations of fluorinated pharmaceutical substances in polymer matrices.

  19. MAS-NMR study of lithium zinc silicate glasses and glass-ceramics with various ZnO content

    Science.gov (United States)

    Goswami, Madhumita; Kothiyal, Govind P.; Montagne, Lionel; Delevoye, Laurent

    2008-02-01

    Lithium zinc silicate glasses of composition (mol%): 17.5Li 2O-(72- x)SiO 2- xZnO-5.1Na 2O-1.3P 2O 5-4.1B 2O 3, 5.5⩽ x⩽17.7, were prepared by conventional melt-quenched technique and converted to glass-ceramic by controlled crystallization process. 29Si and 31P MAS-NMR was used to characterize the structure of both glass and glass-ceramic samples. Despite the complex glass composition, Q2, Q3 and Q4 sites are identified from 29Si MAS-NMR, which relative intensities are found to vary with the ZnO content, indicating a network depolymerization by ZnO. Moreover, well separated Q3 and Q4 resonances for low ZnO content indicates the occurrence of phase separation. From 31P MAS-NMR, it is seen that phosphorus is mainly present in the form of ortho-( Q0) and pyro-phosphate ( Q1) structural units and variation of ZnO content did not have much effect on these resonances, which provides an additional evidence for phase separation in the glass. On conversion to glass-ceramics, lithium disilicate (Li 2Si 2O 5), lithium zinc ortho-silicate (Li 3Zn 0.5SiO 4), tridymite (SiO 2) and cristobalite (SiO 2) were identified as major silicate crystalline phases. Using 29Si MAS-NMR, quantification of these silicate crystalline phases is carried out and correlated with the ZnO content in the glass-ceramics samples. In addition, 31P spectra unambiguously revealed the presence of crystalline Li 3PO 4 and (Na,Li) 3PO 4 in the glass-ceramics.

  20. Transport Properties of Ibuprofen Encapsulated in Cyclodextrin Nanosponge Hydrogels: A Proton HR-MAS NMR Spectroscopy Study.

    Science.gov (United States)

    Ferro, Monica; Castiglione, Franca; Punta, Carlo; Melone, Lucio; Panzeri, Walter; Rossi, Barbara; Trotta, Francesco; Mele, Andrea

    2016-08-15

    The chemical cross-linking of β-cyclodextrin (β-CD) with ethylenediaminetetraacetic dianhydride (EDTA) led to branched polymers referred to as cyclodextrin nanosponges (CDNSEDTA). Two different preparations are described with 1:4 and 1:8 CD-EDTA molar ratios. The corresponding cross-linked polymers were contacted with 0.27 M aqueous solution of ibuprofen sodium salt (IP) leading to homogeneous, colorless, drug loaded hydrogels. The systems were characterized by high resolution magic angle spinning (HR-MAS) NMR spectroscopy. Pulsed field gradient spin echo (PGSE) NMR spectroscopy was used to determine the mean square displacement (MSD) of IP inside the polymeric gel at different observation times td. The data were further processed in order to study the time dependence of MSD: MSD = f(td). The proposed methodology is useful to characterize the different diffusion regimes that, in principle, the solute may experience inside the hydrogel, namely normal or anomalous diffusion. The full protocols including the polymer preparation and purification, the obtainment of drug-loaded hydrogels, the NMR sample preparation, the measurement of MSD by HR-MAS NMR spectroscopy and the final data processing to achieve the time dependence of MSD are here reported and discussed. The presented experiments represent a paradigmatic case and the data are discussed in terms of innovative approach to the characterization of the transport properties of an encapsulated guest within a polymeric host of potential application for drug delivery.

  1. Solid-state (13)C CP MAS NMR spectroscopy of mushrooms gives directly the ratio between proteins and polysaccharides.

    Science.gov (United States)

    Pizzoferrato, L; Manzi, P; Bertocchi, F; Fanelli, C; Rotilio, G; Paci, M

    2000-11-01

    The solid-state (13)C CP MAS NMR technique has the potential of monitoring the chemical composition in the solid state of an intact food sample. This property has been utilized to study mushrooms of different species (Pleurotus ostreatus, Pleurotus eryngii, Pleurotus pulmunarius, and Lentinula edodes), already characterized by chemical analyses for protein and dietary fiber components. Solid-state (13)C CP MAS NMR spectroscopy reveals a large difference in the ratio between the glucidic and the proteic resonances probably depending on the mushroom species. An accurate inspection by model compounds and suitable mixtures of proteins and saccharides gives a methodology to interpret these experimental data. A good correlation (R(2) = 0.93; R(2) = 0.81) has been obtained by comparing the NMR data with the results of the chemical analyses. The results suggest the possibility to perform a taxonomic study and/or a nutritional study on the basis of the ratio between protein and polysaccharide levels determined by NMR or chemical methodologies.

  2. Application of 119Sn CPMG MAS NMR for Fast Characterization of Sn Sites in Zeolites with Natural 119Sn Isotope Abundance

    DEFF Research Database (Denmark)

    G. Kolyagin, Yury; V. Yakimo, Alexander; Tolborg, Søren

    2016-01-01

    119Sn CPMG MAS NMR is demonstrated to be a fast and efficient method for characterization of Sn-sites in Sn-containing zeolites. Tuning of the CPMG echo-train sequence decreases the experimental time by a factor of 5–40 in the case of as-synthesized and hydrated Sn-BEA samples and by 3 orders......-BEA zeolites with natural 119Sn isotope abundance using conventional MAS NMR equipment....

  3. Determination of the structural changes by Raman and {sup 13}C CP/MAS NMR spectroscopy on native corn starch with plasticizers

    Energy Technology Data Exchange (ETDEWEB)

    Cozar, O. [Academy of Romanian Scientists, Splaiul Independentei 54, 050094, Bucharest, Romania and National Institute of Research-Development for Machines and Installations Designed to Agriculture and Food Industry - INMA Bucureşti - Cluj-Napoca Branch (Romania); Filip, C.; Tripon, C. [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath, 400293 Cluj-Napoca (Romania); Cioica, N.; Coţa, C.; Nagy, E. M. [National Institute of Research-Development for Machines and Installations Designed to Agriculture and Food Industry - INMA Bucureşti - Cluj-Napoca Branch, RO-400458 Cluj-Napoca (Romania)

    2013-11-13

    The plasticizing - antiplasticizing effect of water and glycerol contents on native corn starch samples is investigated by FT-Raman and {sup 13}C CP/MAS NMR spectroscopy. The presence of both amorphous and crystalline structural phases was evidenced in pure native corn starch and also in the samples containing plasticizers. Among the crystalline starch structures, the A- and V- types were suggested by CP/MAS NMR spectra.

  4. 1H HR-MAS NMR Spectroscopy and the Metabolite Determination of Typical Foods in Mediterranean Diet

    Directory of Open Access Journals (Sweden)

    Carmelo Corsaro

    2015-01-01

    Full Text Available NMR spectroscopy has become an experimental technique widely used in food science. The experimental procedures that allow precise and quantitative analysis on different foods are relatively simple. For a better sensitivity and resolution, NMR spectroscopy is usually applied to liquid sample by means of extraction procedures that can be addressed to the observation of particular compounds. For the study of semisolid systems such as intact tissues, High-Resolution Magic Angle Spinning (HR-MAS has received great attention within the biomedical area and beyond. Metabolic profiling and metabolism changes can be investigated both in animal organs and in foods. In this work we present a proton HR-MAS NMR study on the typical vegetable foods of Mediterranean diet such as the Protected Geographical Indication (PGI cherry tomato of Pachino, the PGI Interdonato lemon of Messina, several Protected Designation of Origin (PDO extra virgin olive oils from Sicily, and the Traditional Italian Food Product (PAT red garlic of Nubia. We were able to identify and quantify the main metabolites within the studied systems that can be used for their characterization and authentication.

  5. Structural analysis of alkali cations in mixed alkali silicate glasses by 23Na and 133Cs MAS NMR

    Directory of Open Access Journals (Sweden)

    T. Minami

    2014-12-01

    Full Text Available We report the structural analysis of Na+ and Cs+ in sodium cesium silicate glasses by using 23Na and 133Cs magic-angle spinning nuclear magnetic resonance (MAS NMR spectroscopy. In the NMR spectra of cesium silicate crystals, the peak position shifted to higher magnetic field for structures with larger Cs+ coordination numbers and to lower magnetic field for smaller Cs+ coordination numbers. The MAS NMR spectra of xNa2O-yCs2O-2SiO2 (x = 0, 0.2, 0.33, 0.5, 0.66, 0.8, 1.0; x + y = 1 glass reveal that the average coordination number of both the alkali cations decreases with increasing Cs+/(Na+ + Cs+ ratio. In addition, the coordination number of Na+ in xNa2O-yCs2O-2SiO2 glass is smaller than that of Cs+. This difference between the average coordination numbers of the alkali cations is considered to be one structural reason of the mixed alkali effect.

  6. Hydration properties and phosphorous speciation in native, gelatinized and enzymatically modified potato starch analyzed by solid-state MAS NMR

    DEFF Research Database (Denmark)

    Larsen, Flemming H.; Kasprzak, Miroslaw Marek; Lærke, Helle Nygaard

    2013-01-01

    Hydration of granular, gelatinized and molecularly modified states of potato starch in terms of molecular mobility were analyzed by 13C and 31P solid-state MAS NMR. Gelatinization (GEL) tremendously reduced the immobile fraction compared to native (NA) starch granules. This effect was enhanced...... by enzyme-assisted catalytic branching with branching enzyme (BE) or combined BE and β-amylase (BB) catalyzed exo-hydrolysis. Carbons of the glycosidic α-1,6 linkages required high hydration rates before adopting uniform chemical shifts indicating solid-state disorder and poor water accessibility...

  7. Hydration properties and phosphorous speciation in native, gelatinized and enzymatically modified potato starch analyzed by solid-state MAS NMR

    DEFF Research Database (Denmark)

    Larsen, Flemming H.; Kasprzak, Miroslaw Marek; Lærke, Helle Nygaard

    2013-01-01

    Hydration of granular, gelatinized and molecularly modified states of potato starch in terms of molecular mobility were analyzed by 13C and 31P solid-state MAS NMR. Gelatinization (GEL) tremendously reduced the immobile fraction compared to native (NA) starch granules. This effect was enhanced....... Comparative analysis of wheat and waxy maize starches demonstrated that starches were similar upon gelatinization independent of botanical origin and that the torsion angles of the glycosidic linkages were averages of the crystalline A and B type structures. In starch suspension phosphorous in immobile...

  8. Improved quantification of alite and belite in anhydrous Portland cements by 29Si MAS NMR: Effects of paramagnetic ions

    DEFF Research Database (Denmark)

    Poulsen, Søren Lundsted; Kocaba, Vanessa; Le Saoût, Gwenn;

    2009-01-01

    The applicability, reliability, and repeatability of 29Si MAS NMR for determination of the quantities of alite (Ca3SiO5) and belite (Ca2SiO4) in anhydrous Portland cement was investigated in detail for 11 commercial Portland cements and the results compared with phase quantifications based...... on powder X-ray diffraction combined with Rietveld analysis and with Taylor-Bogue calculations. The effects from paramagnetic ions (Fe3+) on the spinning sideband intensities, originating from dipolar couplings between 29Si and the spins of the paramagnetic electrons, were considered and analyzed in spectra...

  9. High-resolution and high-temperature {sup 19} F MAS NMR study of fluorozirconate glasses and liquids

    Energy Technology Data Exchange (ETDEWEB)

    Youngman, R.E.; Sem, S. [Corning Inc., NY (United States)

    2000-07-01

    This paper reports the first results of a high-resolution and high-temperature {sup 19}F MAS NMR spectroscopic study of the atomic structure and its temperature dependence in two binary Zr F{sub 4} (Z B) glasses with 62 and 70 mol % Zr F{sub 4} and a multicomponent ZBLAN (51.7% Zr-F{sub 4}-20.7% Ba F{sub 2}-4.5% La F{sub 3}-3.4% Al F{sub 3}-19.7% Na F) glass.

  10. Microscopic structural analysis of fractured silk fibers from Bombyx mori and Samia cynthia ricini using 13C CP/MAS NMR with a 1 mm microcoil MAS NMR probehead

    KAUST Repository

    Yamauchi, Kazuo

    2010-07-01

    Conformational changes have been studied in silk fibers from the domestic silkworm Bombyx mori and a wild silkworm Samia cynthia ricini as a result of fractured by stretching. About 300 samples consisting of only the fractured regions of [1-13C]Ala or [1-13C]Gly labeled silk fibers were collected and observed by 13C CP/MAS NMR spectra. The total amount of these fractured fibers is only about 1 mg and therefore we used a home-built 1 mm microcoil MAS NMR probehead. A very small increase in the fraction of random coil was noted for the alanine regions of both silk fibroins and for the glycine region of B. mori silk fibroin. However, there is no difference in the spectra before and after fractured for the glycine region of S. c. ricini silk fibroin. Thus, the influence of fracture occurs exclusively at the Ala region for S. c. ricini. The relationship between sequence, fracture and structure is discussed. © 2010 Elsevier Inc. All rights reserved.

  11. Site-resolved 2H relaxation experiments in solid materials by global line-shape analysis of MAS NMR spectra

    Science.gov (United States)

    Lindh, E. L.; Stilbs, P.; Furó, I.

    2016-07-01

    We investigate a way one can achieve good spectral resolution in 2H MAS NMR experiments. The goal is to be able to distinguish between and study sites in various deuterated materials with small chemical shift dispersion. We show that the 2H MAS NMR spectra recorded during a spin-relaxation experiment are amenable to spectral decomposition because of the different evolution of spectral components during the relaxation delay. We verify that the results are robust by global least-square fitting of the spectral series both under the assumption of specific line shapes and without such assumptions (COmponent-REsolved spectroscopy, CORE). In addition, we investigate the reliability of the developed protocol by analyzing spectra simulated with different combinations of spectral parameters. The performance is demonstrated in a model material of deuterated poly(methacrylic acid) that contains two 2H spin populations with similar chemical shifts but different quadrupole splittings. In 2H-exchanged cellulose containing two 2H spin populations with very similar chemical shifts and quadrupole splittings, the method provides new site-selective information about the molecular dynamics.

  12. CaCl2-Accelerated Hydration of Tricalcium Silicate: A STXM Study Combined with 29Si MAS NMR

    Directory of Open Access Journals (Sweden)

    Qinfei Li

    2015-01-01

    Full Text Available The effect of calcium chloride (CaCl2 on tricalcium silicate (C3S hydration was investigated by scanning transmission X-ray microscopy (STXM with Near Edge X-ray Absorption Fine Structure (NEXAFS spectra and 29Si MAS NMR. STXM is demonstrated to be a powerful tool for studying the chemical composition of a cement-based hydration system. The Ca L3,2-edge NEXAFS spectra obtained by examining C3S hydration in the presence of CaCl2 showed that this accelerator does not change the coordination of calcium in the calcium silicate hydrate (C-S-H, which is the primary hydration product. O K-edge NEXAFS is also very useful in distinguishing the chemical components in hydrated C3S. Based on the Ca L3,2-edge spectra and chemical component mapping, we concluded that CaCl2 prefers to coexist with unhydrated C3S instead of C-S-H. In Si K-edge NEXAFS analysis, CaCl2 increases the degree of silicate polymerization of C-S-H in agreement with the 29Si CP/MAS NMR results, which show that the presence of CaCl2 in hydrated C3S considerably accelerates the formation of middle groups (Q2 and branch sites (Q3 in the silicate chains of C-S-H gel at 1-day hydration.

  13. Polydisperse methyl β-cyclodextrin–epichlorohydrin polymers: variable contact time 13C CP-MAS solid-state NMR characterization

    Science.gov (United States)

    Mallard, Isabelle; Baudelet, Davy; Castiglione, Franca; Ferro, Monica; Panzeri, Walter; Ragg, Enzio

    2015-01-01

    Summary The polymerization of partially methylated β-cyclodextrin (CRYSMEB) with epichlorohydrin was carried out in the presence of a known amount of toluene as imprinting agent. Three different preparations (D1, D2 and D3) of imprinted polymers were obtained and characterized by solid-state 13C NMR spectroscopy under cross-polarization magic angle spinning (CP-MAS) conditions. The polymers were prepared by using the same synthetic conditions but with different molar ratios of imprinting agent/monomer, leading to morphologically equivalent materials but with different absorption properties. The main purpose of the work was to find a suitable spectroscopic descriptor accounting for the different imprinting process in three homogeneous polymeric networks. The polymers were characterized by studying the kinetics of the cross-polarization process. This approach is based on variable contact time CP-MAS spectra, referred to as VCP-MAS. The analysis of the VCP-MAS spectra provided two relaxation parameters: T CH (the CP time constant) and T 1ρ (the proton spin-lattice relaxation time in the rotating frame). The results and the analysis presented in the paper pointed out that T CH is sensitive to the imprinting process, showing variations related to the toluene/cyclodextrin molar ratio used for the preparation of the materials. Conversely, the observed values of T 1ρ did not show dramatic variations with the imprinting protocol, but rather confirmed that the three polymers are morphologically similar. Thus the combined use of T CH and T 1ρ can be helpful for the characterization and fine tuning of imprinted polymeric matrices. PMID:26877800

  14. Polydisperse methyl β-cyclodextrin–epichlorohydrin polymers: variable contact time 13C CP-MAS solid-state NMR characterization

    Directory of Open Access Journals (Sweden)

    Isabelle Mallard

    2015-12-01

    Full Text Available The polymerization of partially methylated β-cyclodextrin (CRYSMEB with epichlorohydrin was carried out in the presence of a known amount of toluene as imprinting agent. Three different preparations (D1, D2 and D3 of imprinted polymers were obtained and characterized by solid-state 13C NMR spectroscopy under cross-polarization magic angle spinning (CP-MAS conditions. The polymers were prepared by using the same synthetic conditions but with different molar ratios of imprinting agent/monomer, leading to morphologically equivalent materials but with different absorption properties. The main purpose of the work was to find a suitable spectroscopic descriptor accounting for the different imprinting process in three homogeneous polymeric networks. The polymers were characterized by studying the kinetics of the cross-polarization process. This approach is based on variable contact time CP-MAS spectra, referred to as VCP-MAS. The analysis of the VCP-MAS spectra provided two relaxation parameters: TCH (the CP time constant and T1ρ (the proton spin-lattice relaxation time in the rotating frame. The results and the analysis presented in the paper pointed out that TCH is sensitive to the imprinting process, showing variations related to the toluene/cyclodextrin molar ratio used for the preparation of the materials. Conversely, the observed values of T1ρ did not show dramatic variations with the imprinting protocol, but rather confirmed that the three polymers are morphologically similar. Thus the combined use of TCH and T1ρ can be helpful for the characterization and fine tuning of imprinted polymeric matrices.

  15. Processing of CP MAS kinetics: Towards NMR crystallography for complex solids

    Science.gov (United States)

    Dagys, Laurynas; Klimavicius, Vytautas; Balevicius, Vytautas

    2016-09-01

    Variable temperature and high data point density measurements of 1H-31P cross-polarization kinetics in the powdered ammonium dihydrogen phosphate (ADP) have been carried out in the range of -40 °C to +90 °C upon 7 and 10 kHz MAS. The advanced route of processing CP MAS kinetic data has been developed. It is based on reducing the incoherent far range order spin couplings and extracting the CP oscillatory term with the sequent mathematical treatment. The proper replica has been found, which allowed to reduce the Fourier-Bessel (Hankel) transform calculating the angularly averaged and purely distance-depending spin distribution profile to the routine Fourier transform. The shortest 31P-1H distances determined by CP MAS kinetics get between the values obtained by neutron and X-ray diffraction, whereas those for more remote protons are slightly larger. The changes in P⋯H distances are hardly noticeable, though a certain trend to increase upon the heating can be deduced. The clearly pronounced effect was the increase of the spin-diffusion rate constant upon heating. It allows to state that the communication between interacting spins is the process extremely easy to activate.

  16. Phase cycling schemes for finite-pulse-RFDR MAS solid state NMR experiments.

    Science.gov (United States)

    Zhang, Rongchun; Nishiyama, Yusuke; Sun, Pingchuan; Ramamoorthy, Ayyalusamy

    2015-03-01

    The finite-pulse radio frequency driven dipolar recoupling (fp-RFDR) pulse sequence is used in 2D homonuclear chemical shift correlation experiments under magic angle spinning (MAS). A recent study demonstrated the advantages of using a short phase cycle, XY4, and its super-cycle, XY4(1)4, for the fp-RFDR pulse sequence employed in 2D (1)H/(1)H single-quantum/single-quantum correlation experiments under ultrafast MAS conditions. In this study, we report a comprehensive analysis on the dipolar recoupling efficiencies of XY4, XY4(1)2, XY4(1)3, XY4(1)4, and XY8(1)4 phase cycles under different spinning speeds ranging from 10 to 100 kHz. The theoretical calculations reveal the presence of second-order terms (T(10)T(2,±2), T(1,±1)T(2,±1), etc.) in the recoupled homonuclear dipolar coupling Hamiltonian only when the basic XY4 phase cycle is utilized, making it advantageous for proton-proton magnetization transfer under ultrafast MAS conditions. It is also found that the recoupling efficiency of fp-RFDR is quite dependent on the duty factor (τ180/τR) as well as on the strength of homonuclear dipolar couplings. The rate of longitudinal magnetization transfer increases linearly with the duty factor of fp-RFDR for all the XY-based phase cycles investigated in this study. Examination of the performances of different phase cycles against chemical shift offset and RF field inhomogeneity effects revealed that XY4(1)4 is the most tolerant phase cycle, while the shortest phase cycle XY4 suppressed the RF field inhomogeneity effects most efficiently under slow spinning speeds. Our results suggest that the difference in the fp-RFDR recoupling efficiencies decreases with the increasing MAS speed, while ultrafast (>60 kHz) spinning speed is advantageous as it recouples a large amount of homonuclear dipolar couplings and therefore enable fast magnetization exchange. The effects of higher-order terms and cross terms between various interactions in the effective Hamiltonian of fp

  17. Acceleration of natural-abundance solid-state MAS NMR measurements on bone by paramagnetic relaxation from gadolinium-DTPA

    Science.gov (United States)

    Mroue, Kamal H.; Zhang, Rongchun; Zhu, Peizhi; McNerny, Erin; Kohn, David H.; Morris, Michael D.; Ramamoorthy, Ayyalusamy

    2014-07-01

    Reducing the data collection time without affecting the signal intensity and spectral resolution is one of the major challenges for the widespread application of multidimensional nuclear magnetic resonance (NMR) spectroscopy, especially in experiments conducted on complex heterogeneous biological systems such as bone. In most of these experiments, the NMR data collection time is ultimately governed by the proton spin-lattice relaxation times (T1). For over two decades, gadolinium(III)-DTPA (Gd-DTPA, DTPA = Diethylene triamine pentaacetic acid) has been one of the most widely used contrast-enhancement agents in magnetic resonance imaging (MRI). In this study, we demonstrate that Gd-DTPA can also be effectively used to enhance the longitudinal relaxation rates of protons in solid-state NMR experiments conducted on bone without significant line-broadening and chemical-shift-perturbation side effects. Using bovine cortical bone samples incubated in different concentrations of Gd-DTPA complex, the 1H T1 values were calculated from data collected by 1H spin-inversion recovery method detected in natural-abundance 13C cross-polarization magic angle spinning (CPMAS) NMR experiments. Our results reveal that the 1H T1 values can be successfully reduced by a factor of 3.5 using as low as 10 mM Gd-DTPA without reducing the spectral resolution and thus enabling faster data acquisition of the 13C CPMAS spectra. These results obtained from 13C-detected CPMAS experiments were further confirmed using 1H-detected ultrafast MAS experiments on Gd-DTPA doped bone samples. This approach considerably improves the signal-to-noise ratio per unit time of NMR experiments applied to bone samples by reducing the experimental time required to acquire the same number of scans.

  18. Incorporation of phosphorus guest ions in the calcium silicate phases of Portland cement from 31P MAS NMR spectroscopy.

    Science.gov (United States)

    Poulsen, Søren L; Jakobsen, Hans J; Skibsted, Jørgen

    2010-06-21

    Portland cements may contain small quantities of phosphorus (typically below 0.5 wt % P(2)O(5)), originating from either the raw materials or alternative sources of fuel used to heat the cement kilns. This work reports the first (31)P MAS NMR study of anhydrous and hydrated Portland cements that focuses on the phase and site preferences of the (PO(4))(3-) guest ions in the main clinker phases and hydration products. The observed (31)P chemical shifts (10 to -2 ppm), the (31)P chemical shift anisotropy, and the resemblance of the lineshapes in the (31)P and (29)Si MAS NMR spectra strongly suggest that (PO(4))(3-) units are incorporated in the calcium silicate phases, alite (Ca(3)SiO(5)) and belite (Ca(2)SiO(4)), by substitution for (SiO(4))(4-) tetrahedra. This assignment is further supported by a determination of the spin-lattice relaxation times for (31)P in alite and belite, which exhibit the same ratio as observed for the corresponding (29)Si relaxation times. From simulations of the intensities, observed in inversion-recovery spectra for a white Portland cement, it is deduced that 1.3% and 2.1% of the Si sites in alite and belite, respectively, are replaced by phosphorus. Charge balance may potentially be achieved to some extent by a coupled substitution mechanism where Ca(2+) is replaced by Fe(3+) ions, which may account for the interaction of the (31)P spins with paramagnetic Fe(3+) ions as observed for the ordinary Portland cements. A minor fraction of phosphorus may also be present in the separate phase Ca(3)(PO(4))(2), as indicated by the observation of a narrow resonance at delta((31)P) = 3.0 ppm for two of the studied cements. (31)P{(1)H} CP/MAS NMR spectra following the hydration of a white Portland cement show that the resonances from the hydrous phosphate species fall in the same spectral range as observed for (PO(4))(3-) incorporated in alite. This similarity and the absence of a large (31)P chemical shift ansitropy indicate that the hydrous (PO(4

  19. Investigation on Acute Biochemical Effects of Ce(NO3)3 on Liver and Kidney Tissues by MAS 1H NMR Spectroscopic-Based Metabonomic Approach

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    High resolution magic angle spinning (MAS)-1 H nuclear magnetic resonance (NMR) spectroscopic-based metabonomic approach was applied to the investigation on the acute biochemical effects of Ce(NO3)3. Male Wistar rats were liver and kidney tissues were analyzed using principal component analysis to extract toxicity information. The biochemical effects of Ce(NO3)3 were characterized by the increase of triglycerides and lactate and the decrease of glycogen in rat liver tissue, together with an elevation of the triglyceride level and a depletion of glycerophosphocholine and betaine in kidney tissues. The target lesions of Ce(NO3)3 on liver and kidney were found by MAS NMR-based metabonomic method. This study demonstrates that the combination of MAS 1H NMR and pattern recognition analysis can be an effective method for studies of biochemical effects of rare earths.

  20. Solid-state 51V MAS NMR spectroscopy determines component concentration and crystal phase in co-crystallised mixtures of vanadium complexes

    DEFF Research Database (Denmark)

    Nielsen, Ulla Gro; Hazell, Alan Charles; Skibsted, Jørgen Bengaard

    2010-01-01

    resonances are sensitive to intermolecular interactions specific to each crystal phase. The solid-state V-51 MAS NMR spectroscopic data show that the different phases do not co-precipitate but the concentration of the solute (which can be either 1 or 2) can vary. Thus co-crystallised mixtures of 1 and 2 can...... be classed as a molecular mixture capable of forming continuous solid solutions....... for the vanadium atoms of the two complexes mean that V-51 solution state and MAS NMR spectroscopy can be used to determine the concentration of 1 and 2 in bulk samples. Significantly, however, V-51 MAS NMR spectroscopy also reports on the identity of the crystal phase. This is possible because the isotropic V-51...

  1. Red coralline algae assessed as marine pH proxies using 11B MAS NMR

    OpenAIRE

    M. Cusack; Kamenos, N. A.; Rollion-Bard, C.; Tricot, G

    2015-01-01

    Reconstructing pH from biogenic carbonates using boron isotopic compositions relies on the assumption that only borate, and no boric acid, is present. Red coralline algae are frequently used in palaeoenvironmental reconstruction due to their widespread distribution and regular banding frequency. Prior to undertaking pH reconstructions using red coralline algae we tested the boron composition of the red coralline alga Lithothamnion glaciale using high field NMR. In bulk analysed samples, thirt...

  2. Metabolic Profiling of Cells in Response to Drug Treatment using (1)H High-resolution Magic Angle Spinning (HR-MAS) NMR Spectroscopy.

    Science.gov (United States)

    Vermathen, Martina; Diserens, Gaëlle; Vermathen, Peter; Furrer, Julien

    2017-03-29

    High-resolution magic angle spinning (HR-MAS) is an NMR technique that provides access to well resolved liquid-like 1H NMR spectra of semi-solid samples. Therefore, 1H HR-MAS NMR spectroscopy has become an important tool for the direct analysis of biological samples such as tissues and cells in a mostly non-destructive way. Here, we focus on the application of HR-MAS NMR combined with multivariate statistical methods used for metabolic profiling of cells and in particular for the study of cellular metabolic responses to drug exposure. The principles of HR-MAS and the metabolomic approach are briefly described. As an example, a study on the metabolic response of different cell types towards treatment with a highly cytotoxic hexacationic ruthenium metallaprism as potential anti-cancer drug is presented. Specific metabolites and metabolic pathways are suggested to be associated with the cellular response. The study demonstrates the potential of HR-MAS metabolomics applied to cells for addressing the intracellular processes involved in the treatment with organometallic drugs.

  3. 13C MAS NMR studies of the effects of hydration on the cell walls of potatoes and Chinese water chestnuts.

    Science.gov (United States)

    Tang, H; Belton, P S; Ng, A; Ryden, P

    1999-02-01

    13C NMR with magic angle spinning (MAS) has been employed to investigate the cell walls of potatoes and Chinese water chestnuts over a range of hydration levels. Both single-pulse excitation (SPEMAS) and cross-polarization (CPMAS) experiments were carried out. Hydration led to a substantial increase in signal intensities of galactan and galacturonan in the SPEMAS spectra and a decrease in line width, implying mobilization in the backbone and side chains of pectin. In CPMAS spectra of both samples, noncellulose components showed signal loss as hydration increased. However, the signals of some galacturonan in the 3(1) helix configuration remained in the spectra even when the water content was as high as 110%. Cellulose was unaffected. It is concluded that the pectic polysaccharides experience a distribution of molecular conformations and mobility, whereas cellulose remained as typical rigid solid.

  4. Hydration kinetics for the alite, belite, and calcium aluminate phase in Portland cements from 27Al and 29Si MAS NMR spectroscopy

    DEFF Research Database (Denmark)

    Skibsted, Jørgen; Jensen, Ole Mejlhede; Jakobsen, Hans Jørgen

    1997-01-01

    29Si magic-angle spinning (MAS) NMR spectroscopy is shown to be a valuable tool for obtaining the quantities of alite and belite in hydrated Portland cements. The hydration (1-180 days) of a white Portland cement with 10 wt.% silica fume added is investigated and the degrees of hydration for alite...... belite, and silica fume are determined. It is demonstrated that 27Al MAS NMR spectra of hydrated Portland cements can give quantitative information about the formation of ettringite and the conversion of this phase to monosulphate during hydration....

  5. MAS-NMR investigations of the crystallization behaviour of lithium aluminum silicate (LAS) glasses containing P 2O 5 and TiO 2 nucleants

    Science.gov (United States)

    Ananthanarayanan, A.; Kothiyal, G. P.; Montagne, L.; Revel, B.

    2010-06-01

    Lithium aluminum silicate (LAS) glass of composition (mol%) 20.4Li 2O-4.0Al 2O 3-68.6SiO 2-3.0K 2O-2.6B 2O 3-0.5P 2O 5-0.9TiO 2 was prepared by melt quenching. The glass was then nucleated and crystallized based on differential thermal analysis (DTA) data and was characterized by 29Si, 31P, 11B and 27Al MAS-NMR. XRD and 29Si NMR showed that lithium metasilicate (Li 2SiO 3) is the first phase to c form followed by cristobalite (SiO 2) and lithium disilicate (Li 2Si 2O 5). 29Si MAS-NMR revealed a change in the network structure already for the glasses nucleated at 550 °C. Since crystalline Li 3PO 4, as observed by 31P MAS-NMR, forms concurrently with the silicate phases, we conclude that crystalline Li 3PO 4 does not act as a nucleating agent for lithium silicate phases. Moreover, 31P NMR indicates the formation of M-PO 4 ( M=B, Al or Ti) complexes. The presence of BO 3 and BO 4 structural units in all the glass/glass-ceramic samples is revealed through 11B MAS-NMR. B remains in the residual glass and the crystallization of silicate phases causes a reduction in the number of alkali ions available for charge compensation. As a result, the number of trigonally coordinated B (BO 3) increases at the expense of tetrahedrally coordinated B (BO 4). The 27Al MAS-NMR spectra indicate the presence of tetrahedrally coordinated Al species, which are only slightly perturbed by the crystallization.

  6. Surface Characterization of Some Novel Bonded Phase Packing Materials for HPLC Columns Using MAS-NMR Spectroscopy

    Directory of Open Access Journals (Sweden)

    Jude Abia

    2015-03-01

    Full Text Available Information on the surface properties of three novel chemically bonded phase packing materials for High performance liquid chromatography (HPLC were obtained using spectra obtained by solid state cross-polarization (CP magic-angle spinning (MAS nuclear magnetic resonance (NMR spectroscopic experiments for the 29Si, and 13C nuclei. These packing materials were: Cogent bidentate C18 bonded to type-C silica, hybrid packing materials XTerra MS C18, and XBridge Prep. C18. The spectra obtained using cross-polarization magic angle spinning (CP-MAS on the Cogent bidentate C18 bonded to type-C silica show the surface to be densely populated with hydride groups (Si-H, with a relative surface coverage exceeding 80%. The hybrid packing materials XTerra and XBridge gave spectra that reveal the silicon atoms to be bonded to organic moieties embedded in the molecular structure of these materials with over 90% of the alkyl silicon atoms found within the completely condensed silicon environments. The hydrolytic stability of these materials were investigated in acidic aqueous solutions at pHs of 7.0 and 3.0, and it was found that while the samples of XTerra and XBridge were not affected by hydrolysis at this pH range, the sample of Cogent lost a significant proportion of its Si-H groups after five days of treatment in acidic aqueous solution.

  7. Sensitivity gains, linearity, and spectral reproducibility in nonuniformly sampled multidimensional MAS NMR spectra of high dynamic range

    Science.gov (United States)

    Suiter, Christopher L.; Paramasivam, Sivakumar; Hou, Guangjin; Sun, Shangjin; Rice, David; Hoch, Jeffrey C.; Rovnyak, David

    2014-01-01

    Recently, we have demonstrated that considerable inherent sensitivity gains are attained in MAS NMR spectra acquired by nonuniform sampling (NUS) and introduced maximum entropy interpolation (MINT) processing that assures the linearity of transformation between the time and frequency domains. In this report, we examine the utility of the NUS/MINT approach in multidimensional datasets possessing high dynamic range, such as homonuclear 13C–13C correlation spectra. We demonstrate on model compounds and on 1–73-(U-13C, 15N)/74–108-(U-15N) E. coli thioredoxin reassembly, that with appropriately constructed 50 % NUS schedules inherent sensitivity gains of 1.7–2.1-fold are readily reached in such datasets. We show that both linearity and line width are retained under these experimental conditions throughout the entire dynamic range of the signals. Furthermore, we demonstrate that the reproducibility of the peak intensities is excellent in the NUS/MINT approach when experiments are repeated multiple times and identical experimental and processing conditions are employed. Finally, we discuss the principles for design and implementation of random exponentially biased NUS sampling schedules for homonuclear 13C–13C MAS correlation experiments that yield high-quality artifact-free datasets. PMID:24752819

  8. Sensitivity Gains, Linearity, and Spectral Reproducibility in Nonuniformly Sampled Multidimensional MAS NMR Spectra of High Dynamic Range.

    Energy Technology Data Exchange (ETDEWEB)

    Suiter, Christopher L.; Paramasivam, Sivakumar; Hou, Guangjin; Sun, Shangjin; Rice, David M.; Hoch, Jeffrey C.; Rovnyak, David S.; Polenova, Tatyana E.

    2014-04-22

    Recently, we have demonstrated that considerable inherent sensitivity gains are attained in MAS NMR spectra acquired by nonuniform sampling (NUS) and introduced maximum entropy interpolation (MINT) processing that assures the linearity of transformation between the time and frequency domains. In this report, we examine the utility of the NUS/MINT approach in multidimensional datasets possessing high dynamic range, such as homonuclear 13C–13C correlation spectra. We demonstrate on model compounds and on 1–73-(U-13C,15N)/74–108-(U-15N) E. coli thioredoxin reassembly, that with appropriately constructed 50 % NUS schedules inherent sensitivity gains of 1.7–2.1-fold are readily reached in such datasets. We show that both linearity and line width are retained under these experimental conditions throughout the entire dynamic range of the signals. Furthermore, we demonstrate that the reproducibility of the peak intensities is excellent in the NUS/MINT approach when experiments are repeated multiple times and identical experimental and processing conditions are employed. Finally, we discuss the principles for design and implementation of random exponentially biased NUS sampling schedules for homonuclear 13C–13C MAS correlation experiments that yield high quality artifact-free datasets.

  9. Red coralline algae assessed as marine pH proxies using 11B MAS NMR

    Science.gov (United States)

    Cusack, M.; Kamenos, N. A.; Rollion-Bard, C.; Tricot, G.

    2015-02-01

    Reconstructing pH from biogenic carbonates using boron isotopic compositions relies on the assumption that only borate, and no boric acid, is present. Red coralline algae are frequently used in palaeoenvironmental reconstruction due to their widespread distribution and regular banding frequency. Prior to undertaking pH reconstructions using red coralline algae we tested the boron composition of the red coralline alga Lithothamnion glaciale using high field NMR. In bulk analysed samples, thirty percent of boron was present as boric acid. We suggest that prior to reconstructing pH using coralline algae 1) species-specific boron compositions and 2) within-skeleton special distributions of boron are determined for multiple species. This will enable site selective boron analyses to be conducted validating coralline algae as palaeo-pH proxies based on boron isotopic compositions.

  10. Red coralline algae assessed as marine pH proxies using 11B MAS NMR.

    Science.gov (United States)

    Cusack, M; Kamenos, N A; Rollion-Bard, C; Tricot, G

    2015-02-02

    Reconstructing pH from biogenic carbonates using boron isotopic compositions relies on the assumption that only borate, and no boric acid, is present. Red coralline algae are frequently used in palaeoenvironmental reconstruction due to their widespread distribution and regular banding frequency. Prior to undertaking pH reconstructions using red coralline algae we tested the boron composition of the red coralline alga Lithothamnion glaciale using high field NMR. In bulk analysed samples, thirty percent of boron was present as boric acid. We suggest that prior to reconstructing pH using coralline algae 1) species-specific boron compositions and 2) within-skeleton special distributions of boron are determined for multiple species. This will enable site selective boron analyses to be conducted validating coralline algae as palaeo-pH proxies based on boron isotopic compositions.

  11. Resolution of the Two Aluminum Sites in Ettringite by Al-27 MAS and MQMAS NMR at Very High Magnetic Field (22.3 T)

    DEFF Research Database (Denmark)

    Skibsted, Jorgen; Pedersen, Malene T.; Holzinger, Julian

    2017-01-01

    Ettringite (Ca-6[Al(OH)(6)](2)(SO4)(3)center dot 26H(2)O) is the first hydration product formed during Portland cement hydration. Al-27 MAS NMR has been used in a wide number of studies to detect and quantify ettringite in hydrated cement blends by the observation of a single, narrow resonance...

  12. Non-destructive and direct determination of the degree of substitution of carboxymethyl cellulose by HR-MAS (13)C NMR spectroscopy.

    Science.gov (United States)

    Ferro, M; Castiglione, F; Panzeri, W; Dispenza, R; Santini, L; Karlsson, H J; de Wit, P P; Mele, A

    2017-08-01

    We report on the direct assessment of the degree of substitution (DS) of carboxymethyl cellulose (CMC) by High Resolution Magic Angle Spinning (HR-MAS) (13)C NMR spectroscopy. The method is applied to industrial CMCs with low and high viscosity and nominal DS, purified and technical samples, and from cellulose linters or wood. The preparation of a set of purified CMC working standards with accurate DS values for the method validation is also described. The DS values determined via HR-MAS (13)C NMR on the industrial samples are critically compared to the corresponding values achieved through the USP 37 〈281〉 method (ASH method) and the HPLC method, and the advantages and limitations of the HR-MAS NMR method highlighted. Finally, the HR-MAS NMR approach allowed the accurate DS assessment in CMC with low DS, characterized by a non-negligible fraction of non-functionalized cellulose. The proposed "effective DS" accounts for the DS of the solvent-exposed CMC. Copyright © 2017. Published by Elsevier Ltd.

  13. Observation of immobile regions in natural rubber at ambient temperature by solid-state C-13 CP/MAS NMR spectroscopy

    DEFF Research Database (Denmark)

    Larsen, F.H.; Rasmussen, T.; Pedersen, Walther Batsberg

    1999-01-01

    Employing C-13 CP/MAS NMR spectroscopy, the existence of immobile regions in natural rubber (cis-1,4-polyisoprene) corresponding to a few percent of the monomer units has been detected at ambient temperature. For synthetic rubbers no immobile regions have been detected at all. Applying different...

  14. Heterogeneous Coordination Environments in Lithium-Neutralized Ionomers Identified Using 1H and 7Li MAS NMR

    Directory of Open Access Journals (Sweden)

    Kenneth B. Wagener

    2012-08-01

    Full Text Available The carboxylic acid proton and the lithium coordination environments for precise and random Li-neutralized polyethylene acrylic acid P(E-AA ionomers were explored using high speed solid-state 1H and 7Li MAS NMR. While the 7Li NMR revealed only a single Li coordination environment, the chemical shift temperature variation was dependent on the precise or random nature of the P(E-AA ionomer. The 1H MAS NMR revealed two different carboxylic acid proton environments in these materials. By utilizing 1H-7Li rotational echo double resonance (REDOR MAS NMR experiments, it was demonstrated that the proton environments correspond to different average 1H-7Li distances, with the majority of the protonated carboxylic acids having a close through space contact with the Li. Molecular dynamics simulations suggest that the shortest 1H-7Li distance corresponds to un-neutralized carboxylic acids directly involved in the coordination environment of Li clusters. These solid-state NMR results show that heterogeneous structural motifs need to be included when developing descriptions of these ionomer materials.

  15. Local environments and lithium adsorption on the iron oxyhydroxides lepidocrocite (gamma-FeOOH) and goethite (alpha-FeOOH): A 2H-2 and 7Li solid-state MAS NMR study

    DEFF Research Database (Denmark)

    Nielsen, Ulla Gro; Grey, Clare P.; Paik, Jonkim

    2008-01-01

    2H and 7LiMAS NMR spectroscopy techniques were applied to study the local surface and bulk environments of iron oxyhydroxide lepiclocrocite (gamma-FeOOH). 2H variable-temperature (VT) MAS NMR experiments were performed, showing the presence of short-range, strong antiferromagnetic correlations, e...

  16. Probing sol-gel matrices microenvironments by PGSE HR-MAS NMR.

    Science.gov (United States)

    Ferreira, Ana S D; Barreiros, Susana; Cabrita, Eurico J

    2017-05-01

    We applied Pulsed Gradient Spin Echo diffusion with high-resolution magic angle spinning NMR to study sol-gel matrices used to encapsulate enzymes for biocatalysis (TMOS/MTMS and TMOS/BTMS) to gain insight into the local chemical microenvironment. Transport properties of solvents with different polarities (1-pentanol, acetonitrile and n-hexane) were studied through their apparent self-diffusion coefficients. The spin echo attenuation of the solvents shows two distinct diffusion domains, one with fast diffusion (Dfast ) associated with interparticle diffusion and another with slow diffusion (Dslow ) corresponding to the displacement inside the pores within the sol-gel particles. The analysis of the root mean square displacements at different diffusion times showed that the Dfast domain has a free diffusion regime in both matrices (the root mean square displacement is linearly dependent of the diffusion time), while the Dslow domain shows a different regime that depends on the matrix. We investigated the exchange regime between the two diffusion sites. In both matrices, n-hexane was in intermediate exchange between diffusion domains, while the polar solvents were in slow exchange in TMOS/BTMS and in intermediate exchange in TMOS/MTMS. Data were fitted for TMOS/BTMS with the Kärger model, and the physical parameters were obtained. The results add to the evidence that the pores are a hydrophobic environment but that the presence of some free hydrophilic groups inside the pore, as observed in the TMOS/BTMS, has a key role in slowing down the exchange of polar solvents and that this is relevant to explain previously reported enzyme activity in these materials. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  17. Response of Degarelix treatment in human prostate cancer monitored by HR-MAS (1)H NMR spectroscopy.

    Science.gov (United States)

    Madhu, Basetti; Shaw, Greg L; Warren, Anne Y; Neal, David E; Griffiths, John R

    The androgen receptor (AR) is the master regulator of prostate cancer cell metabolism. Degarelix is a novel gonadotrophin-releasing hormone blocker, used to decrease serum androgen levels in order to treat advanced human prostate cancer. Little is known of the rapid metabolic response of the human prostate cancer tissue samples to the decreased androgen levels. To investigate the metabolic responses in benign and cancerous tissue samples from patients after treatment with Degarelix by using HRMAS (1)H NMR spectroscopy. Using non-destructive HR-MAS (1)H NMR spectroscopy we analysed the metabolic changes induced by decreased AR signalling in human prostate cancer tissue samples. Absolute concentrations of the metabolites alanine, lactate, glutamine, glutamate, citrate, choline compounds [t-choline = choline + phosphocholine (PC) + glycerophosphocholine (GPC)], creatine compounds [t-creatine = creatine (Cr) + phosphocreatine (PCr)], taurine, myo-inositol and polyamines were measured in benign prostate tissue samples (n = 10), in prostate cancer specimens from untreated patients (n = 7) and prostate cancer specimens from patients treated with Degarelix (n = 6). Lactate, alanine and t-choline concentrations were significantly elevated in high-grade prostate cancer samples when compared to benign samples in untreated patients. Decreased androgen levels resulted in significant decreases of lactate and t-choline concentrations in human prostate cancer biopsies. The reduced concentrations of lactate and t-choline metabolites due to Degarelix could in principle be monitored by in vivo (1)H MRS, which suggests that it would be possible to monitor the effects of physical or chemical castration in patients by that non-invasive method.

  18. Determination of structural topology of a membrane protein in lipid bilayers using polarization optimized experiments (POE) for static and MAS solid state NMR spectroscopy.

    Science.gov (United States)

    Mote, Kaustubh R; Gopinath, T; Veglia, Gianluigi

    2013-10-01

    The low sensitivity inherent to both the static and magic angle spinning techniques of solid-state NMR (ssNMR) spectroscopy has thus far limited the routine application of multidimensional experiments to determine the structure of membrane proteins in lipid bilayers. Here, we demonstrate the advantage of using a recently developed class of experiments, polarization optimized experiments, for both static and MAS spectroscopy to achieve higher sensitivity and substantial time-savings for 2D and 3D experiments. We used sarcolipin, a single pass membrane protein, reconstituted in oriented bicelles (for oriented ssNMR) and multilamellar vesicles (for MAS ssNMR) as a benchmark. The restraints derived by these experiments are then combined into a hybrid energy function to allow simultaneous determination of structure and topology. The resulting structural ensemble converged to a helical conformation with a backbone RMSD ~0.44 Å, a tilt angle of 24° ± 1°, and an azimuthal angle of 55° ± 6°. This work represents a crucial first step toward obtaining high-resolution structures of large membrane proteins using combined multidimensional oriented solid-state NMR and magic angle spinning solid-state NMR.

  19. Determination of structural topology of a membrane protein in lipid bilayers using polarization optimized experiments (POE) for static and MAS solid state NMR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Mote, Kaustubh R. [University of Minnesota, Department of Chemistry (United States); Gopinath, T. [University of Minnesota, Department of Biochemistry, Molecular Biology and Biophysics (United States); Veglia, Gianluigi, E-mail: vegli001@umn.edu [University of Minnesota, Department of Chemistry (United States)

    2013-10-15

    The low sensitivity inherent to both the static and magic angle spinning techniques of solid-state NMR (ssNMR) spectroscopy has thus far limited the routine application of multidimensional experiments to determine the structure of membrane proteins in lipid bilayers. Here, we demonstrate the advantage of using a recently developed class of experiments, polarization optimized experiments, for both static and MAS spectroscopy to achieve higher sensitivity and substantial time-savings for 2D and 3D experiments. We used sarcolipin, a single pass membrane protein, reconstituted in oriented bicelles (for oriented ssNMR) and multilamellar vesicles (for MAS ssNMR) as a benchmark. The restraints derived by these experiments are then combined into a hybrid energy function to allow simultaneous determination of structure and topology. The resulting structural ensemble converged to a helical conformation with a backbone RMSD {approx}0.44 A, a tilt angle of 24 Degree-Sign {+-} 1 Degree-Sign , and an azimuthal angle of 55 Degree-Sign {+-} 6 Degree-Sign . This work represents a crucial first step toward obtaining high-resolution structures of large membrane proteins using combined multidimensional oriented solid-state NMR and magic angle spinning solid-state NMR.

  20. 1H and 23Na MAS NMR spectroscopy of cationic species in CO2 selective alkaline earth metal porous silicoaluminophosphates prepared via liquid and solid state ion exchange

    Science.gov (United States)

    Arévalo-Hidalgo, Ana G.; Dugar, Sneha; Fu, Riqiang; Hernández-Maldonado, Arturo J.

    2012-07-01

    The location of extraframework cations in Sr2+ and Ba2+ ion-exchanged SAPO-34 was estimated by means of 1H and 23Na MAS NMR spectroscopy and spectral deconvolution. Incorporation of the alkaline earth metal cations onto the SAPO framework was achieved via liquid state ion exchange, coupled partial detemplation/solid-state ion exchange, and combination of both techniques. MAS NMR revealed that the level of ion exchange was limited by the presence of protons and sodium cations near hexagonal prisms (site SI), which are relatively difficult to exchange with the alkaline earth metal due to steric and charge repulsion criteria. In addition, the presence of ammonium cations in the supercages facilitated the exchange of otherwise tenacious hydrogen as corroborated by unit cell compositional data as well as enhanced CO2 adsorption at low partial pressures. The extraframework ammonium species were produced from partial detemplation of the structure-directing agent employed for the SAPO-34 synthesis, tetraethylammonium.

  1. Hysteresis effect of ammonium and water protons by 1H MAS NMR in (NH4)2CuBr4·2H2O

    Science.gov (United States)

    Lim, Ae Ran; Cho, Jiung

    2017-10-01

    The chemical shifts, linewidths, and spin-lattice relaxation times for ammonium and water protons in (NH4)2CuBr4·2H2O were investigated by 1H magic angle spinning nuclear magnetic resonance (MAS NMR) with a focus on the roles of NH4+ and H2O at high temperatures. The changes in the temperature dependence of the data near Td (=360 K) were related to variations of the H environments; the mechanism above Td was related to hydrogen-bond transfer involving breakage of the weak part of the hydrogen bond. The hysteresis effects for the ammonium and water protons in (NH4)2CuBr4·2H2O by MAS NMR were described with respect to heating and cooling.

  2. The metabolic profile of lemon juice by proton HR-MAS NMR: the case of the PGI Interdonato Lemon of Messina.

    Science.gov (United States)

    Cicero, Nicola; Corsaro, Carmelo; Salvo, Andrea; Vasi, Sebastiano; Giofré, Salvatore V; Ferrantelli, Vincenzo; Di Stefano, Vita; Mallamace, Domenico; Dugo, Giacomo

    2015-01-01

    We have studied by means of High Resolution Magic Angle Spinning Nuclear Magnetic Resonance (HR-MAS NMR) the metabolic profile of the famous Sicilian lemon known as 'Interdonato Lemon of Messina PGI'. The PGI Interdonato Lemon of Messina possesses high organoleptic and healthy properties and is recognised as one of the most nutrient fruits. In particular, some of its constituents are actively studied for their chemo-preventive and therapeutic properties. In this paper, we have determined by means of HR-MAS NMR spectroscopy the molar concentration of the main metabolites constituent the juice of PGI Interdonato Lemon of Messina in comparison with that of the not-PGI Interdonato Lemon of Turkey. Our aim is to develop an analytical technique, in order to determine a metabolic fingerprint able to reveal commercial frauds in national and international markets.

  3. Fine-tuned characterization at the solid/solution interface of organotin compounds grafted onto cross-linked polystyrene by using high-resolution MAS NMR spectroscopy.

    Science.gov (United States)

    Martins, José C; Mercier, Frédéric A G; Vandervelden, Alexander; Biesemans, Monique; Wieruszeski, Jean-Michel; Humpfer, Eberhard; Willem, Rudolph; Lippens, Guy

    2002-08-02

    The structural characterization of organotin compounds that are grafted onto insoluble cross-linked polymers has necessarily been limited to elemental analysis, infrared spectroscopy, and in a few instances, solid-state NMR spectroscopy. This important bottleneck in the development of such grafted systems has been addressed by using high-resolution magic angle spinning (hr-MAS) NMR spectroscopy. The great potential of this technique is demonstrated through the structural characterization of diphenylbutyl-(3,4) and dichlorobutylstannanes (5,6), grafted onto divinylbenzene cross-linked polystyrene by means of a suitable linker (1, 2). First, conditions suitable for the application of hr-MAS NMR spectroscopy were identified by characterizing the (1)H resonance line widths of the grafted organotin moiety following swelling of the functionalized beads in eight representative solvents. The presence of clearly identifiable tin coupling patterns in both the 1D (13)C and 2D (1)H-(13)C HSQC spectra, and the incorporation of (119)Sn chemical shift and connectivity information from hr-MAS 1D (119)Sn and 2D (1)H-(119)Sn HMQC spectra, provide an unprecedented level of characterization of grafted organotins directly at the solid/liquid interface. In addition, the use of hr-MAS (119)Sn NMR for reaction monitoring, impurity detection, and quantification and assessment of the extent of coordination reveals its promise as a novel tool for the investigation of polymer-grafted organotin compounds. The approach described here should be sufficiently general for extension to a variety of other nuclei of interest in polymer-supported organometallic chemistry.

  4. Probing intermolecular interactions in a diethylcarbamazine citrate salt by fast MAS (1)H solid-state NMR spectroscopy and GIPAW calculations.

    Science.gov (United States)

    Venâncio, Tiago; Oliveira, Lyege Magalhaes; Ellena, Javier; Boechat, Nubia; Brown, Steven P

    2017-03-02

    Fast magic-angle spinning (MAS) NMR is used to probe intermolecular interactions in a diethylcarbamazine salt, that is widely used as a treatment against adult worms of Wuchereria bancrofti which cause a common disease in tropical countries named filariasis. Specifically, a dihydrogen citrate salt that has improved thermal stability and solubility as compared to the free form is studied. One-dimensional (1)H, (13)C and (15)N and two-dimensional (1)H-(13)C and (14)N-(1)H heteronuclear correlation NMR experiments under moderate and fast MAS together with GIPAW (CASTEP) calculations enable the assignment of the (1)H, (13)C and (14)N/(15)N resonances. A two-dimensional (1)H-(1)H double-quantum (DQ) -single-quantum (SQ) MAS spectrum recorded with BaBa recoupling at 60kHz MAS identifies specific proton-proton proximities associated with citrate-citrate and citrate-diethylcarbamazine intermolecular interactions. Copyright © 2017 Elsevier Inc. All rights reserved.

  5. Metabolic and histopathological alterations of Jatropha mosaic begomovirus-infected Jatropha curcas L. by HR-MAS NMR spectroscopy and magnetic resonance imaging.

    Science.gov (United States)

    Sidhu, O P; Annarao, Sanjay; Pathre, Uday; Snehi, S K; Raj, S K; Roy, Raja; Tuli, Rakesh; Khetrapal, C L

    2010-06-01

    Alterations in the anatomical structures, sap translocation and metabolic profiles in Jatropha curcas L. (Euphorbiaceae), infected with Jatropha mosaic virus (JMV) have been investigated using MRI and HR-MAS NMR spectroscopy. The contrast of MRI images distinguishes abnormalities in anatomical structures of infected and healthy stem. The HR-MAS NMR spectroscopic analysis indicated that viral infection significantly affected the plant metabolism. Higher accumulation of TCA cycle intermediates, such as citrate and malate, in JMV-infected plants suggested a higher rate of respiration. The respiration rate was more than twofold as compared to healthy ones. The viral stress also significantly increases the concentrations of alanine, arginine, glutamine, valine, GABA and choline as compared to healthy ones. Microscopic examination revealed severe hyperplasia caused by JMV with a considerable reduction in the size of stem cells. Lower concentration of glucose and sucrose in viral-infected stem tissues indicates decreased translocation of photosynthates from leaves to stem due to hyperplasia caused by JMV. The MR images distinguished stele, cortical and pith regions of JMV-infected and healthy stems. Contrast of T(1)- and T(2)-weighted images showed significant differences in the spatial distribution of water, lipids and macromolecules in virus-infected and healthy stem tissues. The results demonstrated the value of MRI and HR-MAS NMR spectroscopy in studying viral infection and metabolic shift in plants. The present methodology may help in better understanding the metabolic alterations during biotic stress in other plant species of agricultural and commercial importance.

  6. A spectrometer designed for 6.7 and 14.1 T DNP-enhanced solid-state MAS NMR using quasi-optical microwave transmission.

    Science.gov (United States)

    Pike, Kevin J; Kemp, Thomas F; Takahashi, Hiroki; Day, Robert; Howes, Andrew P; Kryukov, Eugeny V; MacDonald, James F; Collis, Alana E C; Bolton, David R; Wylde, Richard J; Orwick, Marcella; Kosuga, Kosuke; Clark, Andrew J; Idehara, Toshitaka; Watts, Anthony; Smith, Graham M; Newton, Mark E; Dupree, Ray; Smith, Mark E

    2012-02-01

    A Dynamic Nuclear Polarisation (DNP) enhanced solid-state Magic Angle Spinning (MAS) NMR spectrometer operating at 6.7 T is described and demonstrated. The 187 GHz TE(13) fundamental mode of the FU CW VII gyrotron is used as the microwave source for this magnetic field strength and 284 MHz (1)H DNP-NMR. The spectrometer is designed for use with microwave frequencies up to 395 GHz (the TE(16) second-harmonic mode of the gyrotron) for DNP at 14.1T (600 MHz (1)H NMR). The pulsed microwave output from the gyrotron is converted to a quasi-optical Gaussian beam using a Vlasov antenna and transmitted to the NMR probe via an optical bench, with beam splitters for monitoring and adjusting the microwave power, a ferrite rotator to isolate the gyrotron from the reflected power and a Martin-Puplett interferometer for adjusting the polarisation. The Gaussian beam is reflected by curved mirrors inside the DNP-MAS-NMR probe to be incident at the sample along the MAS rotation axis. The beam is focussed to a ~1 mm waist at the top of the rotor and then gradually diverges to give much more efficient coupling throughout the sample than designs using direct waveguide irradiation. The probe can be used in triple channel HXY mode for 600 MHz (1)H and double channel HX mode for 284 MHz (1)H, with MAS sample temperatures ≥85 K. Initial data at 6.7 T and ~1 W pulsed microwave power are presented with (13)C enhancements of 60 for a frozen urea solution ((1)H-(13)C CP), 16 for bacteriorhodopsin in purple membrane ((1)H-(13)C CP) and 22 for (15)N in a frozen glycine solution ((1)H-(15)N CP) being obtained. In comparison with designs which irradiate perpendicular to the rotation axis the approach used here provides a highly efficient use of the incident microwave beam and an NMR-optimised coil design.

  7. Characterization of a chiral stationary phase by HR/MAS NMR spectroscopy and investigation of enantioselective interaction with chiral ligates by transferred NOE.

    Science.gov (United States)

    Hellriegel, Christine; Skogsberg, Urban; Albert, Klaus; Lämmerhofer, Michael; Maier, Norbert M; Lindner, Wolfgang

    2004-03-31

    The surface chemistry of a chiral stationary phase (CSP) with a (tert-butyl carbamoyl) quinine selector immobilized on thiol-modified silica has been characterized by (1)H HR/MAS NMR and (29)Si CP/MAS NMR spectroscopy. The mostly well-resolved (1)H signals could be assigned to stem from the surface-bound selector and the latter suggested a bi- and trifunctional silane linkage. Suspended-state NMR spectroscopy thus proved a well-characterized surface chemistry as proposed. To study chiral recognition phenomena in the presence of the CSP, (1)H HR/MAS 2D transfer NOESY investigations in methanol-d(4) have been undertaken with various solutes including N-3,5-dinitrobenzoyl derivatives of leucine (DNB-Leu) and N-acetyl phenylalanine (Ac-Phe). Both (R)- and (S)-enantiomers of DNB-Leu and Ac-Phe interacted with the tBuCQN-CSP as indicated by negative cross-peaks in the trNOESY spectra, while the 2D NOESY of the dissolved solutes in absence of the chiral stationary phase showed positive cross-peaks. The intensities of the trNOE cross-peaks were much stronger for the (S)-enantiomers. This stereoselectivity paralleled the experimental chromatographic behavior, where the (S)-enantiomers revealed stronger binding and retention on the tBuCQN-CSP as well. Hence, we were able to correlate the retention behavior to the trNOE NMR spectroscopic data in a qualitative manner.

  8. High field 27Al MAS NMR and TPD studies of active sites in ethanol dehydration using thermally treated transitional aluminas as catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Jian Zhi; Xu, Suochang; Kwak, Ja Hun; Hu, Mary Y.; Wan, Chuan; Zhao, Zhenchao; Szanyi, Janos; Bao, Xinhe; Han, Xiuwen; Wang, Yong; Peden, Charles H. F.

    2016-04-01

    Gamma-, sigma- and theta-Al2O3 are well known metastable “transitional” alumina structural polymorphs. Upon heating, Al2O3 transitions to the so-called and Al2O3 polymorphs and finally forms the thermally stable Al2O3. The poorly developed crystallinity and co-existence of the , , and Al2O3 prior to forming all Al2O3, making it difficult to characterize the structures as well as to quantify the various phases of the transition alumina. As a result, there are significant controversies in the literatures. In this work, a detailed NMR analysis was carried out at high magnetic field on three special aluminum oxide samples where the, , , Al2O3 phases are made dominant, respectively, by controlling the synthesis conditions. The goal is to simplify, including making unambiguous, spectral assignments in 27Al MAS NMR spectra of transition alumina that have not yet been commonly agreed previously. Specifically, quantitative 1D 27Al MAS NMR was used to quantify the ratios of the different alumina structural units, 2D MQMAS 27Al MAS was used for obtaining the highest spectral resolution to guide the analysis of the 1D spectrum, and a saturation pulse sequence was integrated into the 1D NMR to select the amorphous structures, including obtain spectra where the penta-coordinate sites are observed with enhanced relative intensity. Collectively, this study uniquely assigns Al-peaks (both octahedral and tetrahedral) to the Al2O3 and the Al2O3 phases and offers a new way of understanding, including quantifying, the different structural units and sites in transition alumina samples.

  9. Expanding the horizons for structural analysis of fully protonated protein assemblies by NMR spectroscopy at MAS frequencies above 100 kHz.

    Science.gov (United States)

    Struppe, Jochem; Quinn, Caitlin M; Lu, Manman; Wang, Mingzhang; Hou, Guangjin; Lu, Xingyu; Kraus, Jodi; Andreas, Loren B; Stanek, Jan; Lalli, Daniela; Lesage, Anne; Pintacuda, Guido; Maas, Werner; Gronenborn, Angela M; Polenova, Tatyana

    2017-07-03

    The recent breakthroughs in NMR probe technologies resulted in the development of MAS NMR probes with rotation frequencies exceeding 100 kHz. Herein, we explore dramatic increases in sensitivity and resolution observed at MAS frequencies of 110-111 kHz in a novel 0.7 mm HCND probe that enable structural analysis of fully protonated biological systems. Proton- detected 2D and 3D correlation spectroscopy under such conditions requires only 0.1-0.5 mg of sample and a fraction of time compared to conventional (13)C-detected experiments. We discuss the performance of several proton- and heteronuclear- ((13)C-,(15)N-) based correlation experiments in terms of sensitivity and resolution, using a model microcrystalline fMLF tripeptide. We demonstrate the applications of ultrafast MAS to a large, fully protonated protein assembly of the 231-residue HIV-1 CA capsid protein. Resonance assignments of protons and heteronuclei, as well as (1)H-(15)N dipolar and (1)H(N) CSA tensors are readily obtained from the high sensitivity and resolution proton-detected 3D experiments. The approach demonstrated here is expected to enable the determination of atomic-resolution structures of large protein assemblies, inaccessible by current methodologies. Copyright © 2017. Published by Elsevier Inc.

  10. Solid state structure by X-ray and 13C CP/MAS NMR of new 5-[2-(N,N-dimethylamino)ethoxy]-4,7-dimethylcoumarins

    Science.gov (United States)

    Ostrowska, Kinga; Maciejewska, Dorota; Dobrzycki, Łukasz; Socha, Pawel

    2016-05-01

    5-[2-(N,N-dimethylamino)ethoxy]-4,7-dimethylcoumarin (1) and 6-acetyl-5-[2-(N,N-dimethylamino)ethoxy]-4,7-dimethylcoumarin (2), structurally related, were synthesized using both conventional and microwave-assisted approach. An impact of acetyl groups on the molecular structure of coumarin derivatives has been examined. Crystals of 2 were investigated using single crystal and powder X-ray diffraction techniques. Compound 2 crystallizes forming two polymorphs (denoted as 2_1 and 2_2), both belonging to P21/c space group. Both polymorphs are comparably stable and can be formed simultaneously during crystallization process. The solid state structure was also analysed using the fully resolved 13C CP/MAS NMR. The double signals with the intensity ratio of about 1:1 which were observed in the 13C CP/MAS NMR spectrum of compound 1 must arise due to the presence of two conformers of 1. In contrast, NMR spectrum recorded for powder mixture of two polymorphs of compound 2 displays no signal splitting. This is related to structural similarities of molecules in both polymorphs.

  11. Determining hydrogen-bond interactions in spider silk with 1H-13C HETCOR fast MAS solid-state NMR and DFT proton chemical shift calculations.

    Science.gov (United States)

    Holland, Gregory P; Mou, Qiushi; Yarger, Jeffery L

    2013-07-28

    Two-dimensional (2D) (1)H-(13)C heteronuclear correlation (HETCOR) solid-state NMR spectra collected with fast magic angle spinning (MAS) are used in conjunction with density functional theory (DFT) proton chemical shift calculations to determine the hydrogen-bonding strength for ordered β-sheet and disordered 310-helical structures in spider dragline silk. The hydrogen-bond strength is determined to be identical for both structures in spider silk with a 1.83-1.84 Å NH···OC hydrogen-bond distance.

  12. H/D isotope effect of {sup 1}H MAS NMR spectra and {sup 79}Br NQR frequencies of piperidinium p-bromobenzoate and pyrrolidinium p-bromobenzoate

    Energy Technology Data Exchange (ETDEWEB)

    Honda, Hisashi, E-mail: hhonda@yokohama-cu.ac.jp [Yokohama City University, Graduate School of Nanobioscience (Japan); Kyo, Shinshin [Yokohama City University, Faculty of Sciences (Japan); Akaho, Yousuke [Yokohama City University, Faculty of International College of Arts and Sciences (Japan); Takamizawa, Satoshi [Yokohama City University, Graduate School of Nanobioscience (Japan); Terao, Hiromitsu [Tokushima University, Faculty of Integrated Arts and Sciences (Japan)

    2010-04-15

    H/D isotope effects onto {sup 79}Br NQR frequencies of piperidinium p-bromobenzoate were studied by deuterium substitution of hydrogen atoms which form two kinds of N-H Midline-Horizontal-Ellipsis O type hydrogen bonds, and the isotope shift of ca. 100 kHz were detected for a whole observed temperature range. In addition, {sup 1}H MAS NMR spectra measurements of piperidinium and pyrrolidinium p-bromobenzoate were carried out and little isotope changes of NMR line shape were detected. In order to reveal effects of molecular arrangements into the obtained isotope shift of NQR frequencies, single-crystal X-ray measurement of piperidinium p-bromobenzoate-d2 and density-functional-theory calculation were carried out. Our estimation showed the dihedral-angle change between piperidine and benzene ring contributes to isotope shift rather than those of N-H lengths by deuterium substitution.

  13. The structure of aluminosilicate glasses: High-resolution {sup 17}O and {sup 27}Al MAS and 3QMAS NMR study

    Energy Technology Data Exchange (ETDEWEB)

    Lee, S.K.; Stebbins, J.F.

    2000-05-04

    The authors investigate short-range order and local atomic configuration in charge-balanced aluminosilicate glasses as functions of composition, using {sup 17}O and {sup 27}Al MAS and triple-quantum magic angle spinning (3QMAS) NMR spectroscopy. Enhanced resolution in {sup 17}O and {sup 27}Al 3QMAS spectra, compared to MAS NMR, allows the quantification of the spectra and the extent of disorder using a semiempirical function relating 3QMAS efficiency to a quadrupolar coupling constant (C{sub q}). The variations with the Si/Al ratio (R) in peak positions and widths in the isotropic dimension of {sup 27}Al 3QMAS NMR spectra in both Na and Ca-aluminosilicate glasses can be ascribed to variations in the populations of Al sites with varying numbers of Al vs Si neighbors with composition. In the {sup 17}O 3QMAS spectra, variations of populations of three clearly resolved oxygen sites (Al-O-Al, Si-O-Al, and Si-O-Si) with R and cation field strength are consistent with the predictions given in previous results from {sup 29}Si MAS NMR. The quadrupolar coupling product (P{sub q}) of each oxygen site does not vary significantly with R, but it increases with cation field strength. On the other hand, isotropic chemical shifts ({delta}{sub iso}{sup CS}) increase with decreasing R and increasing cation field strength. These trends suggest that the configuration and framework connectivity in aluminosilicate glasses and melts are relatively constant with R but can be perturbed by high field strength cations with increased Al-O-Al and angular disorder, manifested by the increased variation of {delta}{sub iso}{sup CS} and the formation of non-bridging oxygen (NBO). The extent of disorder in aluminosilicate glasses is reflected in calculated configurational enthalpy, which increases with increasing cation field strength, consistent with the excess enthalpy of mixing data from calorimetry. The method and results given here provide improved prospects for the quantitative application of

  14. Yeast-expressed human membrane protein aquaporin-1 yields excellent resolution of solid-state MAS NMR spectra

    Energy Technology Data Exchange (ETDEWEB)

    Emami, Sanaz; Fan Ying; Munro, Rachel; Ladizhansky, Vladimir; Brown, Leonid S., E-mail: lebrown@uoguelph.ca [University of Guelph, Departments of Physics, and Biophysics Interdepartmental Group (Canada)

    2013-02-15

    One of the biggest challenges in solid-state NMR studies of membrane proteins is to obtain a homogeneous natively folded sample giving high spectral resolution sufficient for structural studies. Eukaryotic membrane proteins are especially difficult and expensive targets in this respect. Methylotrophic yeast Pichia pastoris is a reliable producer of eukaryotic membrane proteins for crystallography and a promising economical source of isotopically labeled proteins for NMR. We show that eukaryotic membrane protein human aquaporin 1 can be doubly ({sup 13}C/{sup 15}N) isotopically labeled in this system and functionally reconstituted into phospholipids, giving excellent resolution of solid-state magic angle spinning NMR spectra.

  15. Transport properties derived from ion-atom collisions: 6Li-6Li+ and 6Li-7Li+ Cases

    Science.gov (United States)

    Bouledroua, Moncef; Bouchelaghem, Fouzia; LPR Team

    2014-10-01

    This investigation treats quantum-mechanically the ion- atom collisions and computes the transport coefficients, such as the coefficients of mobility and diffusion. For the case of lithium, the calculations start by determining the gerade and ungerade potential curves through which ionic lithium approaches ground lithium. Then, by considering the isotopic effects and nuclear spins, the elastic and charge-transfer cross sections are calculated for the case of 6Li+and7Li+ colliding with 6Li. Finally, the temperature-dependent diffusion and mobility coefficients are analyzed, and the results are contrasted with those obtained from literature. The main results of this work have been recently published in. This work has been realized within the frames of the CNEPRU Project D01120110036 of the Algerian Ministry of Higher Education.

  16. MAS NMR, DRIFT, and FT-Raman Characterization of SiO(2)-AlPO(4)-B(2)O(3) Ternary Catalytic Systems.

    Science.gov (United States)

    Aramendía; Boráu; Jiménez; Marinas; Ruiz; Urbano

    1999-09-01

    This work deals with the preparation of SiO(2)-AlPO(4)-B(2)O(3) ternary systems from impregation of a SiO(2)-AlPO(4) solid previously synthesized with B(OH)(3) (0-10% B(OH)(3), by weight). Characterization of the resulting solids has been carried out from adsorption-desorption isotherms of nitrogen, DRIFT, FT-Raman, pyridine adsorption, and (1)H, (11)B, (27)Al, and (31)P MAS NMR. The textural properties are scarcely changed by the impregnation and calcination steps. Moreover, the MAS NMR experiments indicated that the components of the solids do not interact among them. The solids were tested in the dehydration-dehydrogenation of propan-2-ol, widely used to correlate catalytic activity with the surface acid-base properties of the solids. The catalytic results indicate that the effect of boron dopping is an increase in the overall acidity of the solids. Copyright 1999 Academic Press.

  17. High field 27Al MAS NMR and TPD studies of active sites in ethanol dehydration using thermally treated transitional aluminas as catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Jian Zhi; Xu, Suochang; Kwak, Ja Hun; Hu, Mary Y.; Wan, Chuan; Zhao, Zhenchao; Szanyi, Janos; Bao, Xinhe; Han, Xiuwen; Wang, Yong; Peden, Charles H. F.

    2016-04-01

    High field quantitative 27Al MAS NMR and temperature programmed desorption (TPD) of ethanol are used to study the surface and phase transformation of gamma-Al2O3 during calcination in the temperature range of 500 to 1300 degrees C. Following ethanol adsorption, ethylene is generated during TPD with a desorption temperature > 200 degrees C. With increasing calcination temperature prior to TPD, the amount of ethylene produced decreases monotonically. Significantly, 27Al MAS NMR reveals that the amount of penta-coordinate Al3+ ions (Lewis acid sites) also decreases with increasing calcination temperature. In fact, a strong correlation between the amount of penta-coordinate Al3+ ions and the amount of strongly adsorbed ethanol molecules (i.e., the ones that convert to ethylene during TPD) is obtained. This result indicates that the penta-coordinate aluminum sites are the catalytic active sites on alumina surfaces during ethanol dehydration reaction across the entire course of gamma- to alpha-Al2O3 phase transformations.

  18. Separation of small metabolites and lipids in spectra from biopsies by diffusion-weighted HR-MAS NMR: a feasibility study.

    Science.gov (United States)

    Diserens, G; Vermathen, M; Precht, C; Broskey, N T; Boesch, C; Amati, F; Dufour, J-F; Vermathen, P

    2015-01-07

    High Resolution Magic Angle Spinning (HR-MAS) NMR allows metabolic characterization of biopsies. HR-MAS spectra from tissues of most organs show strong lipid contributions that are overlapping metabolite regions, which hamper metabolite estimation. Metabolite quantification and analysis would benefit from a separation of lipids and small metabolites. Generally, a relaxation filter is used to reduce lipid contributions. However, the strong relaxation filter required to eliminate most of the lipids also reduces the signals for small metabolites. The aim of our study was therefore to investigate different diffusion editing techniques in order to employ diffusion differences for separating lipid and small metabolite contributions in the spectra from different organs for unbiased metabonomic analysis. Thus, 1D and 2D diffusion measurements were performed, and pure lipid spectra that were obtained at strong diffusion weighting (DW) were subtracted from those obtained at low DW, which include both small metabolites and lipids. This subtraction yielded almost lipid free small metabolite spectra from muscle tissue. Further improved separation was obtained by combining a 1D diffusion sequence with a T2-filter, with the subtraction method eliminating residual lipids from the spectra. Similar results obtained for biopsies of different organs suggest that this method is applicable in various tissue types. The elimination of lipids from HR-MAS spectra and the resulting less biased assessment of small metabolites have potential to remove ambiguities in the interpretation of metabonomic results. This is demonstrated in a reproducibility study on biopsies from human muscle.

  19. Bonding Preferences of Non-Bridging Oxygens in Calcium Aluminosilicate Glass: Evidence from O-17 MAS and 3QMAS NMR on Calcium Aluminate Glass

    Science.gov (United States)

    Allwardt, J. R.; Lee, S.; Stebbins, J.

    2001-12-01

    Non-bridging oxygens (NBO's) play a significant role in the thermodynamic and transport properties in glasses and silicate melts. Previous oxygen-17 (O-17) triple quantum magic angle spinning (3QMAS NMR) data have shown the presence of NBO's in several calcium aluminosilicate (CAS) glasses on the CaAl2O4-SiO2 join (Stebbins and Xu 1997). The observed chemical shifts of these glasses are similar to those for the NBO in calcium silicate glasses (Stebbins et al. 1997 and Stebbins et al 1999); however, a recent O-17 MAS NMR study of crystalline CaAl2O4 showed that the NBO peak in an associated impurity phase is shifted to a higher frequency by 30 to 40 ppm from that of CAS and Ca-silicate glasses (Stebbins et al. in press). This finding suggests that Si is the preferred network cation for NBO's in aluminosilicate glasses and melts at the glass transition temperature. The preference for Si over that of Al as the network cation host for NBO's has also been suggested by Raman and other spectroscopic techniques (Mysen 1988). To investigate this apparent preference for Si-NBO, O-17 3QMAS and MAS experiments were conducted to examine the location of the NBO peak in the spectra of a calcium aluminate glass. Since the CaAl2O4 glass is difficult to make by conventional cooling methods, the binary eutectic composition (63CaO-37Al2O3) was chosen. The resulting O-17 MAS spectrum shows an intense, relatively narrow peak centered at 72 ppm, which nearly coincides with the peak location and width of the Al-O-Al peak in the crystalline Ca-aluminates (Stebbins et al. in press.) (70 ppm). There is a broader, less intense peak centered at 155 ppm that is assigned to the Al-NBO peak. This peak is in approximately the same location as that for a Ca-aluminate phase reported by Stebbins et al. (in press) (137 ppm). In addition, our 3QMAS data show that the peak maximum of the NBO in the Ca-aluminate (-85 and 150 ppm in isotropic and MAS dimensions, respectively) differs significantly from

  20. Low-power broadband homonuclear dipolar recoupling in MAS NMR by two-fold symmetry pulse schemes for magnetization transfers and double-quantum excitation

    Science.gov (United States)

    Teymoori, Gholamhasan; Pahari, Bholanath; Edén, Mattias

    2015-12-01

    We provide an experimental, numerical, and high-order average Hamiltonian evaluation of an open-ended series of homonuclear dipolar recoupling sequences, SR2 2p 1 with p = 1, 2, 3, … . While operating at a very low radio-frequency (rf) power, corresponding to a nutation frequency of 1/2 of the magic-angle spinning (MAS) rate (ωnut =ωr / 2), these recursively generated double-quantum (2Q) dipolar recoupling schemes offer a progressively improved compensation to resonance offsets and rf inhomogeneity for increasing pulse-sequence order p. The excellent recoupling robustness to these experimental obstacles, as well as to CSA, is demonstrated for 2Q filtering (2QF) experiments and for driving magnetization transfers in 2D NMR correlation spectroscopy, where the sequences may provide either double or zero quantum dipolar Hamiltonians during mixing. Experimental and numerical demonstrations, which mostly target conditions of "ultra-fast" MAS (≳50 kHz) and high magnetic fields, are provided for recoupling of 13C across a wide range of isotropic and anisotropic chemical shifts, as well as dipolar coupling constants, encompassing [2,3-13C2 ]alanine, [1,3-13C2 ]alanine, diammonium [1,4-13C2 ]fumarate, and [U-13 C]tyrosine. When compared at equal power levels, a superior performance is observed for the SR2p 1 sequences with p ⩾ 3 relative to existing and well-established 2Q recoupling techniques. At ultra-fast MAS, proton decoupling is redundant during the homonuclear dipolar recoupling of dilute spins in organic solids, which renders the family of SR2p 1 schemes the first efficient 2Q recoupling option for general applications, such as 2Q-1Q correlation NMR and high-order multiple-quantum excitation, under truly low-power rf conditions.

  1. Formation and decomposition of N,N,N-trimethylanilinium cations on zeolite H-Y investigated by in situ stopped-flow MAS NMR spectroscopy.

    Science.gov (United States)

    Wang, Wei; Seiler, Michael; Ivanova, Irina I; Sternberg, Ulrich; Weitkamp, Jens; Hunger, Michael

    2002-06-26

    Methylation of aniline by methanol on zeolite H-Y has been investigated by in situ (13)C MAS NMR spectroscopy under flow conditions. The in situ (13)C continuous-flow (CF) MAS NMR experiments were performed at reaction temperatures between 473 and 523 K, molar methanol-to-aniline ratios of 1:1 to 4:1, and modified residence times of (13)CH(3)OH between 20 and 100 (g x h)/mol. The methylation reaction was shown to start at 473 K. N,N,N-Trimethylanilinium cations causing a (13)C NMR signal at 58 ppm constitute the major product on the catalyst surface. Small amounts of protonated N-methylaniline ([PhNH(2)CH(3)](+)) and N,N-dimethylaniline ([PhNH(CH(3))(2)](+)) were also observed at ca. 39 and 48 ppm, respectively. After increase of the temperature to 523 K, the contents of N,N-dimethylanilinium cations and ring-alkylated reaction products strongly increased, accompanied by a decrease of the amount of N,N,N-trimethylanilinium cations. With application of the in situ stopped-flow (SF) MAS NMR technique, the decomposition of N,N,N-trimethylanilinium cations on zeolite H-Y to N,N-dimethylanilinium and N-methylanilinium cations was investigated to gain a deeper insight into the reaction mechanism. The results obtained allow the proposal of a mechanism consisting of three steps: (i) the conversion of methanol to surface methoxy groups and dimethyl ether (DME); (ii) the alkylation of aniline with methanol, methoxy groups, or DME leading to an equilibrium mixture of N,N,N-trimethylanilinium, N,N-dimethylanilinium, and N-methylanilinium cations attached to the zeolite surface; (iii) the deprotonation of N,N-dimethylanilinium and N-methylanilinium cations causing the formation of N,N-dimethylaniline (NNDMA) and N-methylaniline (NMA) in the gas phase, respectively. The chemical equilibrium between the anilinium cations carrying different numbers of methyl groups is suggested to play a key role for the products distribution in the gas phase.

  2. 6Li foil thermal neutron detector

    Energy Technology Data Exchange (ETDEWEB)

    Ianakiev, Kiril D [Los Alamos National Laboratory; Swinhoe, Martyn T [Los Alamos National Laboratory; Favalli, Andrea [Los Alamos National Laboratory; Chung, Kiwhan [Los Alamos National Laboratory; Macarthur, Duncan W [Los Alamos National Laboratory

    2010-01-01

    In this paper we report on the design of a multilayer thermal neutron detector based on {sup 6}Li reactive foil and thin film plastic scintillators. The {sup 6}Li foils have about twice the intrinsic efficiency of {sup 10}B films and about four times higher light output due to a unique combination of high energy of reaction particles, low self absorption, and low ionization density of tritons. The design configuration provides for double sided readout of the lithium foil resulting in a doubling of the efficiency relative to a classical reactive film detector and generating a pulse height distribution with a valley between neutron and gamma signals similar to {sup 3}He tubes. The tens of microns thickness of plastic scintillator limits the energy deposited by gamma rays, which provides the necessary neutron/gamma discrimination. We used MCNPX to model a multilayer Li foil detector design and compared it with the standard HLNCC-II (18 {sup 3}He tubes operated at 4 atm). The preliminary results of the {sup 6}Li configuration show higher efficiency and one third of the die-away time. These properties, combined with the very short dead time of the plastic scintillator, offer the potential of a very high performance detector.

  3. Probing the location and distribution of paramagnetic centers in alkali metal-loaded zeolites through (7)Li MAS NMR.

    Science.gov (United States)

    Terskikh, Victor V; Ratcliffe, Christopher I; Ripmeester, John A; Reinhold, Catherine J; Anderson, Paul A; Edwards, Peter P

    2004-09-15

    The nature and surroundings of lithium cations in lithium-exchanged X and A zeolites following loading with the alkali metals Na, K, Rb, and Cs have been studied through (7)Li solid-state NMR spectroscopy. It is demonstrated that the lithium in these zeolites is stable with respect to reduction by the other alkali metals. Even though the lithium cations are not directly involved in chemical interactions with the excess electrons introduced in the doping process, the corresponding (7)Li NMR spectra are extremely sensitive to paramagnetic species that are located inside the zeolite cavities. This sensitivity makes (7)Li NMR a useful probe to study the formation, distribution, and transformation of such species.

  4. Observation of 1H-13C and 1H-1H proximities in a paramagnetic solid by NMR at high magnetic field under ultra-fast MAS

    Science.gov (United States)

    Li, Shenhui; Trébosc, Julien; Lafon, Olivier; Zhou, Lei; Shen, Ming; Pourpoint, Frédérique; Amoureux, Jean-Paul; Deng, Feng

    2015-02-01

    The assignment of NMR signals in paramagnetic solids is often challenging since: (i) the large paramagnetic shifts often mask the diamagnetic shifts specific to the local chemical environment, and (ii) the hyperfine interactions with unpaired electrons broaden the NMR spectra and decrease the coherence lifetime, thus reducing the efficiency of usual homo- and hetero-nuclear NMR correlation experiments. Here we show that the assignment of 1H and 13C signals in isotopically unmodified paramagnetic compounds with moderate hyperfine interactions can be facilitated by the use of two two-dimensional (2D) experiments: (i) 1H-13C correlations with 1H detection and (ii) 1H-1H double-quantum ↔ single-quantum correlations. These methods are experimentally demonstrated on isotopically unmodified copper (II) complex of L-alanine at high magnetic field (18.8 T) and ultra-fast Magic Angle Spinning (MAS) frequency of 62.5 kHz. Compared to 13C detection, we show that 1H detection leads to a 3-fold enhancement in sensitivity for 1H-13C 2D correlation experiments. By combining 1H-13C and 1H-1H 2D correlation experiments with the analysis of 13C longitudinal relaxation times, we have been able to assign the 1H and 13C signals of each L-alanine ligand.

  5. Constant-time 2D and 3D through-bond correlation NMR spectroscopy of solids under 60 kHz MAS

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Rongchun; Ramamoorthy, Ayyalusamy, E-mail: ramamoor@umich.edu [Biophysics and Department of Chemistry, The University of Michigan, Ann Arbor, Michigan 48109-1055 (United States)

    2016-01-21

    Establishing connectivity and proximity of nuclei is an important step in elucidating the structure and dynamics of molecules in solids using magic angle spinning (MAS) NMR spectroscopy. Although recent studies have successfully demonstrated the feasibility of proton-detected multidimensional solid-state NMR experiments under ultrafast-MAS frequencies and obtaining high-resolution spectral lines of protons, assignment of proton resonances is a major challenge. In this study, we first re-visit and demonstrate the feasibility of 2D constant-time uniform-sign cross-peak correlation (CTUC-COSY) NMR experiment on rigid solids under ultrafast-MAS conditions, where the sensitivity of the experiment is enhanced by the reduced spin-spin relaxation rate and the use of low radio-frequency power for heteronuclear decoupling during the evolution intervals of the pulse sequence. In addition, we experimentally demonstrate the performance of a proton-detected pulse sequence to obtain a 3D {sup 1}H/{sup 13}C/{sup 1}H chemical shift correlation spectrum by incorporating an additional cross-polarization period in the CTUC-COSY pulse sequence to enable proton chemical shift evolution and proton detection in the incrementable t{sub 1} and t{sub 3} periods, respectively. In addition to through-space and through-bond {sup 13}C/{sup 1}H and {sup 13}C/{sup 13}C chemical shift correlations, the 3D {sup 1}H/{sup 13}C/{sup 1}H experiment also provides a COSY-type {sup 1}H/{sup 1}H chemical shift correlation spectrum, where only the chemical shifts of those protons, which are bonded to two neighboring carbons, are correlated. By extracting 2D F1/F3 slices ({sup 1}H/{sup 1}H chemical shift correlation spectrum) at different {sup 13}C chemical shift frequencies from the 3D {sup 1}H/{sup 13}C/{sup 1}H spectrum, resonances of proton atoms located close to a specific carbon atom can be identified. Overall, the through-bond and through-space homonuclear/heteronuclear proximities determined from the

  6. Constant-time 2D and 3D through-bond correlation NMR spectroscopy of solids under 60 kHz MAS.

    Science.gov (United States)

    Zhang, Rongchun; Ramamoorthy, Ayyalusamy

    2016-01-21

    Establishing connectivity and proximity of nuclei is an important step in elucidating the structure and dynamics of molecules in solids using magic angle spinning (MAS) NMR spectroscopy. Although recent studies have successfully demonstrated the feasibility of proton-detected multidimensional solid-state NMR experiments under ultrafast-MAS frequencies and obtaining high-resolution spectral lines of protons, assignment of proton resonances is a major challenge. In this study, we first re-visit and demonstrate the feasibility of 2D constant-time uniform-sign cross-peak correlation (CTUC-COSY) NMR experiment on rigid solids under ultrafast-MAS conditions, where the sensitivity of the experiment is enhanced by the reduced spin-spin relaxation rate and the use of low radio-frequency power for heteronuclear decoupling during the evolution intervals of the pulse sequence. In addition, we experimentally demonstrate the performance of a proton-detected pulse sequence to obtain a 3D (1)H/(13)C/(1)H chemical shift correlation spectrum by incorporating an additional cross-polarization period in the CTUC-COSY pulse sequence to enable proton chemical shift evolution and proton detection in the incrementable t1 and t3 periods, respectively. In addition to through-space and through-bond (13)C/(1)H and (13)C/(13)C chemical shift correlations, the 3D (1)H/(13)C/(1)H experiment also provides a COSY-type (1)H/(1)H chemical shift correlation spectrum, where only the chemical shifts of those protons, which are bonded to two neighboring carbons, are correlated. By extracting 2D F1/F3 slices ((1)H/(1)H chemical shift correlation spectrum) at different (13)C chemical shift frequencies from the 3D (1)H/(13)C/(1)H spectrum, resonances of proton atoms located close to a specific carbon atom can be identified. Overall, the through-bond and through-space homonuclear/heteronuclear proximities determined from the 3D (1)H/(13)C/(1)H experiment would be useful to study the structure and dynamics of

  7. Perfil químico de cultivares de feijão (phaseolus vulgaris pela técnica de high resolution magic angle spinning (HR-MAS Chemical profile of beans cultivars (phaseolus vulgaris by ¹h nmr - high resolution magic angle spinning (HR-MAS

    Directory of Open Access Journals (Sweden)

    Luciano Morais Lião

    2010-01-01

    Full Text Available The application of one-dimensional proton high-resolution magic angle spinning (¹H HR-MAS NMR combined with a typical advantages of solid and liquid-state NMR techniques was used as input variables for the multivariate statistical analysis. In this paper, different cultivars of beans (Phaseolus vulgaris developed and in development by Embrapa - Arroz e Feijão were analyzed by ¹H HR-MAS, which have been demonstrated to be a valuable tool in its differentiation according chemical composition and avoid the manipulation of the samples as used in other techniques.

  8. Two-dimensional MAS NMR correlation protocols involving double-quantum filtering of quadrupolar spin-pairs.

    Science.gov (United States)

    Edén, Mattias

    2010-05-01

    Three two-dimensional (2D) NMR homonuclear correlation techniques invoking double-quantum (2Q) filtration of the central transitions of half-integer spins are evaluated numerically and experimentally. They correlate directly detected single-quantum (1Q) coherences in the t(2) domain with either of 1Q, two-spin 2Q or single-spin multiple-quantum coherence-evolutions in the indirect (t(1)) dimension. We employ experimental (23)Na and (27)Al NMR on sodium sulfite and the natural mineral sillimanite (SiAl(2)O(5)), in conjunction with simulated 2D spectra from pairs of dipolar-recoupled spins-3/2 and 5/2 at different external magnetic fields, to compare the correlation strategies from the viewpoints of 2D spectral resolution, signal sensitivity, implementational aspects and their relative merits for establishing internuclear proximities and quadrupolar tensor orientations.

  9. Resolution and measurement of heteronuclear dipolar couplings of a noncrystalline protein immobilized in a biological supramolecular assembly by proton-detected MAS solid-state NMR spectroscopy

    Science.gov (United States)

    Park, Sang Ho; Yang, Chen; Opella, Stanley J.; Mueller, Leonard J.

    2013-12-01

    Two-dimensional 15N chemical shift/1H chemical shift and three-dimensional 1H-15N dipolar coupling/15N chemical shift/1H chemical shift MAS solid-state NMR correlation spectra of the filamentous bacteriophage Pf1 major coat protein show single-site resolution in noncrystalline, intact-phage preparations. The high sensitivity and resolution result from 1H detection at 600 MHz under 50 kHz magic angle spinning using ∼0.5 mg of perdeuterated and uniformly 15N-labeled protein in which the exchangeable amide sites are partially or completely back-exchanged (reprotonated). Notably, the heteronuclear 1H-15N dipolar coupling frequency dimension is shown to select among 15N resonances, which will be useful in structural studies of larger proteins where the resonances exhibit a high degree of overlap in multidimensional chemical shift correlation spectra.

  10. 1H high-resolution magic-angle spinning (HR-MAS) NMR analysis of ligand density on resins using a resin internal standard.

    Science.gov (United States)

    Lucas, Laura H; Cerny, Matthew A; Koen, Yakov M; Hanzlik, Robert P; Larive, Cynthia K

    2004-10-01

    We recently attempted to generate an affinity chromatography adsorbent to purify cytochrome P450 4A1 by coupling 11-(1'-imidazolyl)-3,6,9-trioxaundecanoic acid to Toyopearl AF-Amino 650 M resin. Variations in ligand density for several resin batches were quantified by high-resolution magic-angle spinning (HR-MAS) NMR spectroscopy using a novel resin internal standard. The uniquely designed ImQ internal resin standard yields its signature resonance in a transparent region of the analyte spectrum making suppression of the polymer background unnecessary. This method enabled us to target a reasonable ligand density for enzyme purification and provides an advantageous alternative to quantitation against soluble standards or protonated solvent.

  11. 13C CP MAS NMR and GIAO-CHF/DFT calculations of flavonoids: Morin, kaempferol, tricin, genistein, formononetin and 3,7-dihydroxyflavone

    Science.gov (United States)

    Zielińska, Agnieszka; Paradowska, Katarzyna; Jakowski, Jacek; Wawer, Iwona

    2008-02-01

    13C CP MAS NMR spectra of the flavonoids: morin, kaempferol, 3,7-dihydroxyflavone, tricin and isoflavones: genistein and formononetin were recorded to characterize solid-state conformations. Intramolecular hydrogen bonds forming five-, six- and seven-membered rings are present in the two morin molecules in the crystals - their 13C resonances have been assigned with the aid of the calculated shielding constants. Linear relationships between the calculated shielding constants σDFT (ppm) and chemical shifts ( δCPMAS, ppm) were obtained for all studied compounds. Higher correlation coefficients suggest that the conformation with "clockwise" orientation of both OH groups is more probable in the solid 3,7-dihydroxyflavone, whereas in the solid formononetin the OH and OCH 3 substituents are directed "anticlockwise". The barrier to the rotation of phenyl ring B decreases in the order: morin (2'-OH, 3-OH) > kaempferol (3-OH) > tricin.

  12. 119Sn MAS NMR Study of Probe Molecules Interaction with Sn-BEA: The Origin of Penta- and Hexacoordinated Tin Formation

    DEFF Research Database (Denmark)

    Yakimov, Alexander V.; G. Kolyagin, Yury; Tolborg, Søren

    2016-01-01

    119Sn CPMG MAS NMR was applied to study the adsorption of acetonitrile, methanol, isopropanol, isobutanol and water over Sn-BEA enriched with 119Sn isotope. Two signals observed at ca. -422 and -443 ppm over dehydrated samples were attributed to tetracoordinated framework tin sites with strong...... and weak Lewis acidity, respectively. The adsorption of acetonitrile and methanol resulted in observation of pentacoordinated tin species, due to the formation of 1:1 adsorption complexes over both Sn-sites. Water adsorption led first to formation of pentacoordinated tin species, which were further...... converted into hexacoordinated species at longer reaction times. The latter transformation was found to be kinetically limited and was attributed to chemical interaction of tin sites with water, such as hydrolysis of Si-O-Sn bonds. The adsorption of isopropanol and isobutanol was accompanied...

  13. Structural elucidation of b-(Y,Sc){sub 2}Si{sub 2}O{sub 7} : combined use of {sub 89}Y MAS NMR and powder diffraction.

    Energy Technology Data Exchange (ETDEWEB)

    Allix, M.; Alba, M. D.; Florian, P.; Fernandez-Carrion, A. J.; Suchomel, M. R.; Escudero, A.; Suard, E.; Becerro, A. I. (X-Ray Science Division); (CNRS); (Univ. d' Orleans); (Inst de Ciencia de Materiales de Sevilla); (Inst. Laue-Langevin)

    2011-08-01

    Although the structures of pure Sc{sub 2}Si{sub 2}O{sub 7} and {beta}-Y{sub 2}Si{sub 2}O{sub 7} have been described in the literature using the C2/m space group, {sup 29}Si magic angle spinning (MAS) NMR measurements of the intermediate members of the Sc{sub 2}Si{sub 2}O{sub 7}-{beta}-Y{sub 2}Si{sub 2}O{sub 7} system indicate a lowering of the symmetry to the C2 space group. Indeed, these compositions exhibit a unique Si crystallographic site and an Si-O-Si angle lower than 180{sup o}, incompatible with the C2/m space group. C2 is the only possible alternative. Space group Cm can be discarded with regard to its two different Si sites per unit cell. Moreover, {sup 89}Y MAS NMR data have revealed the existence of two different Y sites in the structure of the intermediate members of the Sc{sub 2}Si{sub 2}O{sub 7}-{beta}-Y{sub 2}Si{sub 2}O{sub 7} system, confirming the lowering of the symmetry to the C2 space group. The viability of the C2 model has therefore been tested and confirmed by refinement of synchrotron and neutron powder diffraction data for the different members of the system. The structural evolutions across the Sc{sub 2}Si{sub 2}O{sub 7}-{beta}-Y{sub 2}Si{sub 2}O{sub 7} system are discussed.

  14. Structural elucidation of {beta}-(Y,Sc){sub 2}Si{sub 2}O{sub 7}. Combined use of {sup 89}Y MAS NMR and powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Allix, M.; Florian, P. [CNRS UPR3079 CEMHTI, Orleans (France); Orleans Univ. (France); Alba, M.D.; Fernandez-Carrion, A.J.; Escudero, A.; Becerro, A.I. [CSIC-Universidad de Sevilla (Spain). Inst. de Ciencia de Materiales de Sevilla; Suchomel, M.R. [Argonne National Laboratory, Argonne, IL (United States). Advanced Photon Source; Suard, E. [Institut Laue-Langevin, Grenoble (France)

    2011-08-15

    Although the structures of pure Sc{sub 2}Si{sub 2}O{sub 7} and {beta}-Y{sub 2}Si{sub 2}O{sub 7} have been described in the literature using the C2/m space group, {sup 29}Si magic angle spinning (MAS) NMR measurements of the intermediate members of the Sc{sub 2}Si{sub 2}O{sub 7}-{beta}-Y{sub 2}Si{sub 2}O{sub 7} system indicate a lowering of the symmetry to the C2 space group. Indeed, these compositions exhibit a unique Si crystallographic site and an Si-O-Si angle lower than 180, incompatible with the C2/m space group. C2 is the only possible alternative. Space group Cm can be discarded with regard to its two different Si sites per unit cell. Moreover, {sup 89}Y MAS NMR data have revealed the existence of two different Y sites in the structure of the intermediate members of the Sc{sub 2}Si{sub 2}O{sub 7}-{beta}-Y{sub 2}Si{sub 2}O{sub 7} system, confirming the lowering of the symmetry to the C2 space group. The viability of the C2 model has therefore been tested and confirmed by refinement of synchrotron and neutron powder diffraction data for the different members of the system. The structural evolutions across the Sc{sub 2}Si{sub 2}O{sub 7}-{beta}-Y{sub 2}Si{sub 2}O{sub 7} system are discussed. (orig.)

  15. Proton-detected MAS NMR experiments based on dipolar transfers for backbone assignment of highly deuterated proteins

    Science.gov (United States)

    Chevelkov, Veniamin; Habenstein, Birgit; Loquet, Antoine; Giller, Karin; Becker, Stefan; Lange, Adam

    2014-05-01

    Proton-detected solid-state NMR was applied to a highly deuterated insoluble, non-crystalline biological assembly, the Salmonella typhimurium type iii secretion system (T3SS) needle. Spectra of very high resolution and sensitivity were obtained at a low protonation level of 10-20% at exchangeable amide positions. We developed efficient experimental protocols for resonance assignment tailored for this system and the employed experimental conditions. Using exclusively dipolar-based interspin magnetization transfers, we recorded two sets of 3D spectra allowing for an almost complete backbone resonance assignment of the needle subunit PrgI. The additional information provided by the well-resolved proton dimension revealed the presence of two sets of resonances in the N-terminal helix of PrgI, while in previous studies employing 13C detection only a single set of resonances was observed.

  16. Investigating the lignocellulosic composition during delignification using confocal raman spectroscopy, cross-polarization magic angle spinning carbon 13 - nuclear magnetic resonance (CP/MAS 13C- NMR) spectroscopy and atomic force microscopy

    CSIR Research Space (South Africa)

    Chunilall, Viren

    2012-03-01

    Full Text Available spectroscopy, Cross-Polarization Magic Angle Spinning Carbon 13 - Nuclear Magnetic Resonance (CP/MAS 13C-NMR) spectroscopy and Atomic Force Microscopy (AFM) in conjunction with image analysis. The confocal Raman results showed that there were differences...

  17. Accurate determination of order parameters from 1H,15N dipolar couplings in MAS solid-state NMR experiments.

    Science.gov (United States)

    Chevelkov, Veniamin; Fink, Uwe; Reif, Bernd

    2009-10-01

    A reliable site-specific estimate of the individual N-H bond lengths in the protein backbone is the fundamental basis of any relaxation experiment in solution and in the solid-state NMR. The N-H bond length can in principle be influenced by hydrogen bonding, which would result in an increased N-H distance. At the same time, dynamics in the backbone induces a reduction of the experimental dipolar coupling due to motional averaging. We present a 3D dipolar recoupling experiment in which the (1)H,(15)N dipolar coupling is reintroduced in the indirect dimension using phase-inverted CP to eliminate effects from rf inhomogeneity. We find no variation of the N-H dipolar coupling as a function of hydrogen bonding. Instead, variations in the (1)H,(15)N dipolar coupling seem to be due to dynamics of the protein backbone. This is supported by the observed correlation between the H(N)-N dipolar coupling and the amide proton chemical shift. The experiment is demonstrated for a perdeuterated sample of the alpha-spectrin SH3 domain. Perdeuteration is a prerequisite to achieve high accuracy. The average error in the analysis of the H-N dipolar couplings is on the order of +/-370 Hz (+/-0.012 A) and can be as small as 150 Hz, corresponding to a variation of the bond length of +/-0.005 A.

  18. 31P MAS-NMR study of flux-grown rare-earth element orthophosphate (monazite/xenotime) solid solutions: Evidence of random cation distribution from paramagnetically shifted NMR resonances

    Energy Technology Data Exchange (ETDEWEB)

    Palke, A. C. [Stanford University; Stebbins, J. F. [Stanford University; Boatner, Lynn A [ORNL

    2013-01-01

    We present 31P magic angle spinning nuclear magnetic resonance (MAS-NMR) spectra of flux-grown solid solutions of La1-xCexPO4 ( x between 0.027 and 0.32) having the monoclinic monazite structure, and of Y1-xMxPO4 (M = Vn+, Ce3+, Nd3+, x between 0.001 and 0.014) having the tetragonal zircon structure. Paramagnetically shifted NMR resonances are observed in all samples due to the presence of paramagnetic Vn+, Ce3+, and Nd3+ in the diamagnetic LaPO4 or YPO4. As a first-order observation, the number and relative intensity of these peaks is related to the symmetry and structure of the diamagnetic host phase. The presence of paramagnetic shifts allows for increased resolution between NMR resonances for distinct atomic species which leads to the observation of low intensity peaks related to PO4 species having more than one paramagnetic neighbor two or four atomic bonds away. Through careful analysis of peak areas and comparison with predictions for simple models, it was determined that solid solutions in the systems examined here are characterized by complete disorder (random distribution) of diamagnetic La3+ or Y3+ with the paramagnetic substitutional species Ce3+ and Nd3+. The increased resolution given by the paramagnetic interactions also leads to the observation of splitting of specific resonances in the 31P NMR spectra that may be caused by local, small-scale distortions from the substitution of ions having dissimilar ionic radii.

  19. Effect of organic matter application on CP-MAS-13C-NMR spectra of humic acids from a brown soil

    Science.gov (United States)

    Dou, S.

    2009-04-01

    The humified SOM or humic substances (HS) composed of humic acid (HA), fulvic acid (FA) and humin (HM) represent the most microbially recalcitrant and stable reservoir of organic carbon in soil (Piccolo et al., 2004). OM applications can influence the amount and structural characteristics of HS(Dou et al., 2008). During the past few decades, there has been much research on HS, but their chemical structure is still not fully understood (Dong, 2006).CP-MAS-13C-NMR spectroscopy was considered as an effective method to study structures of HS without dissolving problem compared with liquid 13C-NMR (Conte et al., 1997; Dou et al., 2008). It can directly measure the carbon framework and reflect the nature of HS transformation after OM application (Spaccini et al., 2000). For that reason, this method was applied in this study. The objective of this paper was to clarify the effect of long term OM application on the changes of structural characteristics in HAs, which provided new information for improving soil fertility by OM application. The experiment was carried out on a brown soil (Paleudalf in USDA Soil Taxonomy) at Shenyang Agricultural University, Liaoning province, China (N41°48'-E123°25'). The experiment included 3 treatments: zero-treatment (CKbr), and two pig manure (PM) treatments (O1 and O2) at the rates of 0.9 t ha-1 and 1.8 t ha-1 of organic carbon, respectively. The samples of the HA fraction were extracted, separated and purified according to the method described by Dou et al. (1991). Elemental composition, Differential thermal analysis (DTA), -lgK value, FT-IR and CP-MAS- 13C-NMR of HAs were performed. Effects on the contents of orgaic carbon and its composition. The contents of TOC were from 8.77 g kg-1 to 12.25 g kg-1. The relative contents in TOC for WSS, HA, and FA were 6.87%, 14.2% and 19.8%. Comparing the CKbr, the contents of WSS, HA and FA for O1 and O2 increased, but relative contents of WSS and FA decreased. The content of the HA increased after

  20. Triple α resonances in the 6Li + 6Li → 3α reaction at low energy

    Directory of Open Access Journals (Sweden)

    A. Tumino

    2015-11-01

    Full Text Available The 6Li + 6Li → 3α reaction has been measured in a kinematically complete experiment at 3.1 MeV of beam energy. The reaction mainly proceeds via intermediate 8Be states. The interaction between any two of the three α particles provides events with one, two or three 8Be interfering levels, with strong enhancement in the α–α coincidence yield. Evidence of three 8Be levels within the same 3α event suggests that one α particle is exchanged between the other two. This is a condition for Efimov states to occur in nuclei, for which no observation exists yet. The hyperspherical formalism for the low-energy three-body problem has been applied to point out the 3α particle correlation.

  1. Diffusion of $^{6}$Li in Ta and W

    CERN Document Server

    Vacik, J

    2006-01-01

    The objective of this work was the study of 6Li diffusion in the Ta and W refractory metals. The samples were prepared by ion implantation of 380 keV 6Li+ ions into W and Ta thin foils (up to the fluence of 1016 ions/cm2) and annealed up to the temperature 1940 °C. The depth profiles of 6Li were determined using the Thermal Neutron Depth Profiling (TNDP) technique. The results showed that diffusion of 6Li in both W and Ta foils is very complex and cannot be described by simple Fick’s laws. Trapping centers (in the subsurface layers of both W and Ta metals) were supposed in a trial to explain the 6Li diffusion behaviour. However, the 6Li depth profiles were only partly explained. Other aspects are necessary to take into account for more proper quantification; such as spatially dependent diffusion coefficients, etc.

  2. Identification of Streptococcus pneumoniae serotype 11E, serovariant 11Av and mixed populations by high-resolution magic angle spinning nuclear magnetic resonance (HR-MAS NMR spectroscopy and flow cytometric serotyping assay (FCSA.

    Directory of Open Access Journals (Sweden)

    Romina Camilli

    Full Text Available BACKGROUND: Recent studies have identified Streptococcus pneumoniae serotype 11E and serovariant 11Av among isolates previously typed as 11A by classical serotyping methods. Serotype 11E and serovariant 11Av differ from serotype 11A by having totally or partially inactive wcjE, a gene in cps locus coding for an O-acetyl transferase. Serotype 11E is rare among carriage isolates but common among invasive isolates suggesting that it survives better during invasion. Aim of this work was to investigate the epidemiology of serotype 11A in a pneumococcal collection using a new serotyping approach based on High-Resolution Magic Angle Spinning Nuclear Magnetic Resonance (HR-MAS NMR spectroscopy to distinguish serotypes 11A and 11E. METHODS: A collection of 48 (34 invasive and 14 carriage S. pneumoniae isolates from Italy, previously identified as serotype 11A by the Quellung reaction, were investigated by wcjE sequencing, HR-MAS NMR spectroscopy and the reference flow cytometric serotyping assay (FCSA based on monoclonal antibodies. RESULTS: HR-MAS NMR spectra from serotypes 11A and 11E showed different NMR peaks indicating that HR-MAS NMR could be used to distinguish these serotypes, although HR-MAS NMR could not distinguish serotype 11Av from serotype 11E unambiguously. Thirty-eight isolates were confirmed to be serotype 11A, 8 isolates with a mutated wcjE were serotype 11E, 1 isolate belonged to serovariant 11Av, and 1 isolate was a mixed population 11A/11Av. All 11E isolates were identified among invasive isolates. CONCLUSIONS: We proved that HR-MAS NMR can be of potential use for pneumococcal serotyping. The detection of serotype 11E among invasive isolates in our collection, supports previous epidemiological studies suggesting that mutations in wcjE can represent a mechanism promoting pneumococcal survival during invasion. The discovery of a spectrum of immunochemical diversity within established serotypes should stimulate efforts to develop new

  3. 6^Li in the atmosphere of GJ 117

    CERN Document Server

    Christian, D J; Jevremovic, D; Hauschildt, P H; Baron, E

    2005-01-01

    We present high resolution VLT UVES observations of the active K dwarf GJ 117. 6^Li enhancement has been shown for energetic solar events, one chromospherically active binary, and several dwarf halo stars. Our analysis reveals the detection of 6^Li on this source with 6^Li/7^Li = 0.030+/-0.010. We found no significant contribution from other lines, including Ti I, in the Li profile of GJ 117 and a template star of similar spectral type and metallicity. We discuss the possibility for 6^Li production by spallation and find it to be consistent with the activity levels of the object.

  4. I: Low Frequency NMR and NQR Using a dc SQUID. II: Variable-temperature 13C CP/MAS of Organometallics

    Energy Technology Data Exchange (ETDEWEB)

    Ziegeweid, Marcia A. [Univ. of California, Berkeley, CA (United States)

    1995-11-01

    NMR and NQR at low frequencies are difficult prospects due to small nuclear spin polarization. Furthermore, the sensitivity of the inductive pickup circuitry of standard spectrometers is reduced as the frequency is lowered. I have used a cw-SQUID (Superconducting Quantum Interference Device) spectrometer, which has no such frequency dependence, to study the local atomic environment of 14N via the quadrupolar interaction. Because 14N has spin I = 1 and a 0-6 MHz frequency range, it is not possible to obtain well-resolved spectra in high magnetic fields. I have used a technique to observe 14N NQR resonances via their effect on neighboring protons mediated by the heteronuclear dipolar interaction to study peptides and narcotics. The sensitivity of the SQUID is not enough to measure low-frequency surface (or other low spin density) systems. The application of spin-polarized xenon has been previously used to enhance polarization in conventional NMR experiments. Because xenon only polarizes spins with which it is in contact, it is surface selective. While differences in chemical shifts between surface and bulk spins are not large, it is expected that the differences in quadrupole coupling constant should be very large due to the drastic change of the electric field gradient surrounding spins at the surface. With this in mind, I have taken preliminary steps to measure SQUID detected polarization transfer from Xe to another spin species at 4.2 K and in small magnetic fields (<50 G). In this regime, the spin-lattice relaxation of xenon is dependent on the applied magnetic field. The results of our efforts to characterize the relaxation of xenon are presented. The final section describes the solid-state variable-temperature (VT) one- and two-dimensional 13C cross polarization (CP)/magic angle spinning (MAS) NMR of Hf(η5-C5H5)21-C5H5)2, Zr

  5. I: Low Frequency NMR and NQR Using a dc SQUID. II: Variable-temperature 13C CP/MAS of Organometallics

    Energy Technology Data Exchange (ETDEWEB)

    Ziegeweid, M.A.

    1995-11-29

    NMR and NQR at low frequencies are difficult prospects due to small nuclear spin polarization. Furthermore, the sensitivity'of the inductive pickup circuitry of standard spectrometers is reduced as the frequency is lowered. I have used a cw-SQUID (Superconducting QUantum Interference Device) spectrometer, which has no such frequency dependence, to study the local atomic environment of {sup 14}N via the quadrupolar interaction. Because {sup 14}N has spin I = 1 and a 0-6 MHz frequency range, it is not possible to obtain well-resolved spectra in high magnetic fields. I have used a technique to observe {sup 14}N NQR resonances via their effect on neighboring protons mediated by the heteronuclear dipolar interaction to study peptides and narcotics. The sensitivity of the SQUID is not enough to measure low-frequency surface (or other low spin density) systems. The application of spin-polarized xenon has been previously used to enhance polarization in conventional NMR experiments. Because xenon only polarizes spins with which it is in contact, it is surface selective. While differences in chemical shifts between surface and bulk spins are not large, it is expected that the differences in quadrupole coupling constant should be very large due to the drastic change of the electric field gradient surrounding spins at the surface. With this in mind, I have taken preliminary steps to measure SQUID detected polarization transfer from Xe to another spin species at 4.2 K and in small magnetic fields (<50 G). In this regime, the spin-lattice relaxation of xenon is dependent on the applied magnetic field. The results of our efforts to characterize the relaxation of xenon are presented. The final section describes the solid-state variable-temperature (VT) one- and two-dimensional {sup 13}C cross polarization (CP)/magic angle spinning (MAS) NMR of Hf({eta}{sup 5}-C{sub 5}H{sub 5}){sub 2}({eta}{sup 1}-C{sub 5}H{sub 5}){sub 2}, Zr({eta}{sup 5}-C{sub 5}H{sub 5}){sub 3}({eta}{sup 1

  6. Four-body dynamics in 6Li elastic scattering

    CERN Document Server

    Watanabe, Shin; Ogata, Kazuyuki; Yahiro, Masanobu

    2015-01-01

    We analyze 6Li elastic scattering in a wide range of incident energies (Ein), assuming the n + p + alpha + target four-body model and solving the dynamics with the four-body version of the continuum-discretized coupled-channels method (CDCC). Four-body CDCC well reproduces the experimental data with no adjustable parameter for 6Li + 209Bi scattering at Ein = 24-50 MeV and 6Li + 208Pb scattering at Ein = 29-210 MeV. In the wide Ein range, 6Li breakup is significant and provides repulsive corrections to the folding potential. As an interesting property, d breakup is strongly suppressed in 6Li-breakup processes independently of Ein. We investigate what causes the d-breakup suppression.

  7. {sup 1}H and {sup 23}Na MAS NMR spectroscopy of cationic species in CO{sub 2} selective alkaline earth metal porous silicoaluminophosphates prepared via liquid and solid state ion exchange

    Energy Technology Data Exchange (ETDEWEB)

    Arevalo-Hidalgo, Ana G. [Department of Chemical Engineering, University of Puerto Rico-Mayagueez Campus, Mayagueez, PR 00681-9000 (Puerto Rico); Dugar, Sneha; Fu, Riqiang [National High Magnetic Field Laboratory, Florida State University, Tallahassee, FL 32310 (United States); Hernandez-Maldonado, Arturo J., E-mail: arturoj.hernandez@upr.edu [Department of Chemical Engineering, University of Puerto Rico-Mayagueez Campus, Mayagueez, PR 00681-9000 (Puerto Rico)

    2012-07-15

    The location of extraframework cations in Sr{sup 2+} and Ba{sup 2+} ion-exchanged SAPO-34 was estimated by means of {sup 1}H and {sup 23}Na MAS NMR spectroscopy and spectral deconvolution. Incorporation of the alkaline earth metal cations onto the SAPO framework was achieved via liquid state ion exchange, coupled partial detemplation/solid-state ion exchange, and combination of both techniques. MAS NMR revealed that the level of ion exchange was limited by the presence of protons and sodium cations near hexagonal prisms (site SI), which are relatively difficult to exchange with the alkaline earth metal due to steric and charge repulsion criteria. In addition, the presence of ammonium cations in the supercages facilitated the exchange of otherwise tenacious hydrogen as corroborated by unit cell compositional data as well as enhanced CO{sub 2} adsorption at low partial pressures. The extraframework ammonium species were produced from partial detemplation of the structure-directing agent employed for the SAPO-34 synthesis, tetraethylammonium. - Graphical abstract: MAS NMR was used to elucidate the position the cationic species in alkaline earth metal exchanged silicoaluminophosphates. These species played a significant role during the ion exchange process and, therefore, the materials ultimate CO{sub 2} adsorption performance. Highlights: Black-Right-Pointing-Pointer Location of extraframework Sr{sup 2+} or Ba{sup 2+} cations was estimated by means of {sup 1}H and {sup 23}Na MAS NMR. Black-Right-Pointing-Pointer Level of Sr{sup 2+} or Ba{sup 2+} ion exchange was limited by the presence of protons and sodium cations. Black-Right-Pointing-Pointer Presence of ammonium cations in the supercages facilitated the exchange. Black-Right-Pointing-Pointer Sr{sup 2+} and Ba{sup 2+} ion exchanged SAPOs are outstanding CO{sub 2} adsorbents.

  8. One-Pot Synthesis, X-Ray Diffraction and MAS NMR Spectroscopic Study of Gallosilicate Nitrate Cancrinite Na8[GaSiO4]6(NO34(H2O6

    Directory of Open Access Journals (Sweden)

    Ashok V. Borhade

    2010-01-01

    Full Text Available One-pot synthetic gallosilicate nitrate cancrinite (CAN framework topology have been synthesized under hydrothermal conditions at 100 °C. The synthesized product was characterized by, X-ray powder diffraction, IR, Raman and 29Si, 23Na MAS NMR spectroscopy, SEM and thermogravimetry. The crystal structure refinement of pure nitrate cancrinite has been carried out from X-ray data using Rietveld refinement method. Gallosilicate cancrinite Na8[GaSiO4]6(NO34(H2O6 crystalline hexagonal with space group P63 and a = 12.77981 Å (2, c = 5.20217 Å (1, (Rwp = 0.0696 Rp = 0.0527. The results by MAS NMR spectroscopy confirmed the alternating Si, Ga ordering of the gallosilicate framework for a Si/Ga ratio of 1.0. A distribution of the quadrupolar interaction of the sodium cations caused by the enclatherated water molecules and motional effects can be suggested from the 23Na MAS NMR. Thermogravimetric investigation shows the extent of nitrate entrapment, stability within the cancrinite cage and decomposition properties. SEM clearly shows the hexagonal needle shaped crystals of nitrate cancrinite.

  9. Metabolic profiling of ob/ob mouse fatty liver using HR-MAS (1)H-NMR combined with gene expression analysis reveals alterations in betaine metabolism and the transsulfuration pathway.

    Science.gov (United States)

    Gogiashvili, Mikheil; Edlund, Karolina; Gianmoena, Kathrin; Marchan, Rosemarie; Brik, Alexander; Andersson, Jan T; Lambert, Jörg; Madjar, Katrin; Hellwig, Birte; Rahnenführer, Jörg; Hengstler, Jan G; Hergenröder, Roland; Cadenas, Cristina

    2017-02-01

    Metabolic perturbations resulting from excessive hepatic fat accumulation are poorly understood. Thus, in this study, leptin-deficient ob/ob mice, a mouse model of fatty liver disease, were used to investigate metabolic alterations in more detail. Metabolites were quantified in intact liver tissues of ob/ob (n = 8) and control (n = 8) mice using high-resolution magic angle spinning (HR-MAS) (1)H-NMR. In addition, after demonstrating that HR-MAS (1)H-NMR does not affect RNA integrity, transcriptional changes were measured by quantitative real-time PCR on RNA extracted from the same specimens after HR-MAS (1)H-NMR measurements. Importantly, the gene expression changes obtained agreed with those observed by Affymetrix microarray analysis performed on RNA isolated directly from fresh-frozen tissue. In total, 40 metabolites could be assigned in the spectra and subsequently quantified. Quantification of lactate was also possible after applying a lactate-editing pulse sequence that suppresses the lipid signal, which superimposes the lactate methyl resonance at 1.3 ppm. Significant differences were detected for creatinine, glutamate, glycine, glycolate, trimethylamine-N-oxide, dimethylglycine, ADP, AMP, betaine, phenylalanine, and uridine. Furthermore, alterations in one-carbon metabolism, supported by both metabolic and transcriptional changes, were observed. These included reduced demethylation of betaine to dimethylglycine and the reduced expression of genes coding for transsulfuration pathway enzymes, which appears to preserve methionine levels, but may limit glutathione synthesis. Overall, the combined approach is advantageous as it identifies changes not only at the single gene or metabolite level but also deregulated pathways, thus providing critical insight into changes accompanying fatty liver disease. Graphical abstract A Evaluation of RNA integrity before and after HR-MAS (1)H-NMR of intact mouse liver tissue. B Metabolite concentrations and gene

  10. Big Bang 6Li nucleosynthesis studied deep underground (LUNA collaboration)

    Science.gov (United States)

    Trezzi, D.; Anders, M.; Aliotta, M.; Bellini, A.; Bemmerer, D.; Boeltzig, A.; Broggini, C.; Bruno, C. G.; Caciolli, A.; Cavanna, F.; Corvisiero, P.; Costantini, H.; Davinson, T.; Depalo, R.; Elekes, Z.; Erhard, M.; Ferraro, F.; Formicola, A.; Fülop, Zs.; Gervino, G.; Guglielmetti, A.; Gustavino, C.; Gyürky, Gy.; Junker, M.; Lemut, A.; Marta, M.; Mazzocchi, C.; Menegazzo, R.; Mossa, V.; Pantaleo, F.; Prati, P.; Rossi Alvarez, C.; Scott, D. A.; Somorjai, E.; Straniero, O.; Szücs, T.; Takacs, M.

    2017-03-01

    The correct prediction of the abundances of the light nuclides produced during the epoch of Big Bang Nucleosynthesis (BBN) is one of the main topics of modern cosmology. For many of the nuclear reactions that are relevant for this epoch, direct experimental cross section data are available, ushering the so-called "age of precision". The present work addresses an exception to this current status: the 2H(α,γ)6Li reaction that controls 6Li production in the Big Bang. Recent controversial observations of 6Li in metal-poor stars have heightened the interest in understanding primordial 6Li production. If confirmed, these observations would lead to a second cosmological lithium problem, in addition to the well-known 7Li problem. In the present work, the direct experimental cross section data on 2H(α,γ)6Li in the BBN energy range are reported. The measurement has been performed deep underground at the LUNA (Laboratory for Underground Nuclear Astrophysics) 400 kV accelerator in the Laboratori Nazionali del Gran Sasso, Italy. The cross section has been directly measured at the energies of interest for Big Bang Nucleosynthesis for the first time, at Ecm = 80, 93, 120, and 133 keV. Based on the new data, the 2H(α,γ)6Li thermonuclear reaction rate has been derived. Our rate is even lower than previously reported, thus increasing the discrepancy between predicted Big Bang 6Li abundance and the amount of primordial 6Li inferred from observations.

  11. Insight into the local magnetic environments and deuteron mobility in jarosite (AFe3(SO4)2(OD)6, A = K, Na, D3O) and hydronium alunite ((D3O)Al3(SO4)2(OD,OD2)6), from variable temperature 2H MAS NMR spectroscopy

    DEFF Research Database (Denmark)

    Nielsen, Ulla Gro; Heinmaa, Ivo; Samoson, Ago

    2011-01-01

    Detailed insight into the magnetic properties and mobility of the different deuteron species in jarosites (AFe3(SO4)2(OD)6, A = K, Na, D3O) is obtained from variable temperature 2H MAS NMR spectroscopy from 40 K to 300 K. Fast MAS results in high resolution spectra of these paramagnetic compounds...

  12. Investigating the Surface Structure of γ-Al 2 O 3 Supported WO X Catalysts by High Field 27 Al MAS NMR and Electronic Structure Calculations

    Energy Technology Data Exchange (ETDEWEB)

    Wan, Chuan; Hu, Mary Y.; Jaegers, Nicholas R.; Shi, Dachuan; Wang, Huamin; Gao, Feng; Qin, Zhaohai; Wang, Yong; Hu, Jian Zhi

    2016-10-13

    The metal-support interaction in γ-Al2O3 supported WOX catalysts is investigated by a combination of high field quantitative single pulse (SP) 27Al MAS NMR spectroscopy, 2D MQMAS, 1H-27Al CP/MAS, and electronic structure calculations. NMR allows the observation of at least seven different Al sites, including a pentahedral Al site, three different tetrahedral Al sites, and three octahedral Al sites. It is found that the penta-coordinated Al (AlP) site density decreases monotonically with an increased WOX loading while the octahedral Al (AlO) site density increases concurrently. This suggests that the Alp sites are the preferred surface anchoring positions for the WOX species. Importantly, the AlP site isotropic chemical shift observed for the unsupported γ-Al2O3 at about 38 ppm migrates into the octahedral region with a new isotropic chemical shift value appearing near 7 ppm when the Alp site is anchored by WOX species. Density functional theory (DFT) computational modeling of the NMR parameters on proposed cluster models is carried out to accurately interpret the dramatic chemical shift changes from which the detailed anchoring mechanisms are obtained. It is found that tungsten dimers and monomers are the preferred supported surface species on γ-Al2O3, wherein one monomeric and several dimeric structures are identified as the most likely surface anchoring structures.

  13. Structure determination of uniformly {sup 13}C, {sup 15}N labeled protein using qualitative distance restraints from MAS solid-state {sup 13}C-NMR observed paramagnetic relaxation enhancement

    Energy Technology Data Exchange (ETDEWEB)

    Tamaki, Hajime [Hokkaido University, Graduate School of Life Science (Japan); Egawa, Ayako [Osaka University, Institute for Protein Research (Japan); Kido, Kouki [Hokkaido University, Graduate School of Life Science (Japan); Kameda, Tomoshi [National Institute of Advanced Industrial Science and Technology, Biotechnology Research Institute for Drug Discovery (Japan); Kamiya, Masakatsu; Kikukawa, Takashi; Aizawa, Tomoyasu [Hokkaido University, Faculty of Advanced Life Science (Japan); Fujiwara, Toshimichi [Osaka University, Institute for Protein Research (Japan); Demura, Makoto, E-mail: demura@sci.hokudai.ac.jp [Hokkaido University, Faculty of Advanced Life Science (Japan)

    2016-01-15

    Magic angle spinning (MAS) solid-state nuclear magnetic resonance (NMR) is a powerful method for structure determination of insoluble biomolecules. However, structure determination by MAS solid-state NMR remains challenging because it is difficult to obtain a sufficient amount of distance restraints owing to spectral complexity. Collection of distance restraints from paramagnetic relaxation enhancement (PRE) is a promising approach to alleviate this barrier. However, the precision of distance restraints provided by PRE is limited in solid-state NMR because of incomplete averaged interactions and intermolecular PREs. In this report, the backbone structure of the B1 domain of streptococcal protein G (GB1) has been successfully determined by combining the CS-Rosetta protocol and qualitative PRE restraints. The derived structure has a Cα RMSD of 1.49 Å relative to the X-ray structure. It is noteworthy that our protocol can determine the correct structure from only three cysteine-EDTA-Mn{sup 2+} mutants because this number of PRE sites is insufficient when using a conventional structure calculation method based on restrained molecular dynamics and simulated annealing. This study shows that qualitative PRE restraints can be employed effectively for protein structure determination from a limited conformational sampling space using a protein fragment library.

  14. Buffer-gas-assisted polarization spectroscopy of 6Li.

    Science.gov (United States)

    Ohtsubo, Nozomi; Aoki, Takatoshi; Torii, Yoshio

    2012-07-15

    We report on the demonstration of Doppler-free polarization spectroscopy of the D2 line of (6)Li atoms. Counterintuitively, the presence of an Ar buffer gas, in a certain pressure range, causes a drastic enhancement of the polarization rotation signal. The observed dependence of the signal amplitude on the Ar buffer pressure and the pump laser power is reproduced by calculations based on simple rate equations. We performed stable laser frequency locking using a dispersion signal obtained by polarization spectroscopy for laser cooling of (6)Li atoms.

  15. Metabolic Profiles in Temporal Cortex,Hippocampus and Entorhinal Cortex in Rats Measuredby HR-MAS 1H NMR Spectroscopy%HR-MAS NMR研究大鼠颞叶、海马和内嗅皮质的生理代谢表征

    Institute of Scientific and Technical Information of China (English)

    刘慧浪; 朱航; 夏圣安; 刘买利

    2008-01-01

    颞叶结构参与了多种中枢退行性疾病的发牛和发展.了解生理状念下大鼠的这些脑区的代谢特征可以为动物模型的病理研究提供基础数据和参考.本文采用高分辨魔角旋转核磁共振(HR-MAS NMR)波谱技术和主成分分析(PCA)方法对S.D.大鼠双侧颞叶、海马和内嗅皮质的代谢物进行了分析,结果发现这3个脑区的代谢表征存在显著差异.颞叶区的N-乙酰天门冬氨酸和牛磺酸的浓度最高,肌醇和肌酸的浓度最低;海马区的甘氨酸和胆碱的浓度最高;而在内嗅皮质区则是谷氨酰氨的浓度最高.另外,还证实了HR-MAS NMR-PCA技术是研究生理和病理状态下脑组织各亚结构代谢表征的一种有效的手段.

  16. Pressure induced structural and density changes in Ca and Mg aluminosilicate glasses (MO/Al2O3≤1) recovered from 1-3 GPa: 27Al, 17O, 29Si MAS NMR and density

    Science.gov (United States)

    Bista, S.; Stebbins, J. F.

    2016-12-01

    Numerous studies have shown that at least in Na and K aluminosilicate melts and glasses, the presence of NBO facilitates the increase in Al coordination with pressure, for example albite and jadeite compositions show little structural change at 2-3 GPa. Much less is known about higher field strength cations such as Ca and Mg, despite their importance in mafic magmas. Therefore, in this study, we have studied several compositions of Ca and Mg aluminosilicate glasses with little to no NBO in the metaluminous and peraluminous regions. Our 27Al MAS NMR on the glasses recovered from high T and P show surprisingly rapid increases in average Al coordination with pressure, with the largest increases recorded in the Mg system. In Ca aluminosilicate glasses, the average Al coordination increase in peralkaline and peraluminous glasses follow a much more rapid rise compared to the metaluminous, although the metaluminous composition also shows a significant change in Al coordination unlike the Na aluminosilicate glasses of similar composition. In Mg aluminosilicate glasses, the average Al coordination increase in both peralkaline and metaluminous compositions are similar. Our study shows that the mechanism of the coordination increase with pressure is more complex than the simple consumption of NBO, especially with the high field strength and smaller size modifier cations like Mg. We also observed shifts in 29Si and 17O MAS NMR spectra suggesting increase in high coordinated Al neighbors, but these changes are harder to uniquely interpret.

  17. Reaction mechanisms in the 6Li+ 52Cr system

    Directory of Open Access Journals (Sweden)

    Pandey Bhawna

    2015-01-01

    Full Text Available Reactions induced by the weakly bound 6Li projectile interacting with the intermediate mass target 52Cr are investigated. The choice of this particular reaction in our study is because it is proposed as a surrogate reaction [6Li(52Cr, d56Fe*] for the measurement of 55Fe(n,p reaction cross-section, which has been found to be very important in fusion reactor studies. All the conditions which have to be satisfied for using the surrogate method have been checked. The energy of 6Li beam is selected in a way so as to get equivalent neutron energy in the region of 9-14 MeV, which is of primary interest in fusion reactor application. In the present work, statistical model calculations PACE (Projection-Angular-Momentum-Coupled-Evaporation, ALICE and Continuum-Discretized–Coupled-Channel (CDCC: FRESCO have been used to provide information for the 6Li + 52Cr system and the respective contributions of different reaction mechanisms. The present theoretical work is an important step in the direction towards studying the cross-section of the 55Fe(n, p55Mn reaction by surrogate method.

  18. Photo-Cross-Linked Poly(DL-lactide)-Based Networks. Structural Characterization by HR-MAS NMR Spectroscopy and Hydrolytic Degradation Behavior

    NARCIS (Netherlands)

    Melchels, Ferry P. W.; Velders, Aldrik H.; Feijen, Jan; Grijpma, Dirk W.

    2010-01-01

    To date, biodegradable networks and particularly their kinetic chain lengths have been characterized by analysis of their degradation products in solution. We characterize the network itself by NMR analysis in the solvent-swollen state under magic angle spinning conditions. The networks were prepare

  19. Photo-Cross-Linked Poly(dl-lactide)-Based Networks. Structural Characterization by HR-MAS NMR Spectroscopy and Hydrolytic Degradation Behavior

    NARCIS (Netherlands)

    Melchels, Ferry P.W.; Velders, Aldrik H.; Feijen, Jan; Grijpma, Dirk W.

    2010-01-01

    To date, biodegradable networks and particularly their kinetic chain lengths have been characterized by analysis of their degradation products in solution. We characterize the network itself by NMR analysis in the solvent-swollen state under magic angle spinning conditions. The networks were prepare

  20. Unusual Threshold Anomaly in the 6Li+208Pb System

    Institute of Scientific and Technical Information of China (English)

    ZHANG Chun-Lei; JIA Hui-Ming; WU Zhen-Dong; XU Xin-Xing; BAI Chun-Lin; ZHANG Huan-Qiao; LIN Cheng-Jian; RUAN Ming; LIU Zu-Hua; YANG Feng; WU Xiu-Kun; ZHOU Ping; AN Guang-Peng

    2006-01-01

    @@ The angular distributions of elastic scattering for the 6Li +208Pb system have been measured at several energies around the Coulomb barrier. The parameters of optical potential are extracted by means of a phenomenological optical model analysis. It is found that the real and imaginal potentials show a pronounced energy dependence.The behaviour of the potential at the nearly especially sub-barrier energies in the 6Li+208Pb system is quite different from the results of some previous reports observed in other systems, such as 19 F +208 Pb and 16 O+208 Pb.This unusual threshold phenomenon indicates that breakup channel is strongly coupled with the elastic channel and has obvious effects on optical potential.

  1. Solid state structural analysis of new pentamidine analogs designed as chemotherapeutics that target DNA by X-ray diffraction and 13C, 15N CP/MAS NMR methods

    Science.gov (United States)

    Żabiński, Jerzy; Maciejewska, Dorota; Wolska, Irena

    2010-12-01

    The paper presents the solid-state analysis of the crystalline form of 1,5- bis[(4-cyanophenyl)- N-methylamino]pentane ( 1) and polycrystalline powder sample of 1,5- bis[(4-amidinophenyl)- N-methylamino]pentane dihydrochloride ( 2). The methods used are X-ray diffraction technique and 13C, 15N CP/MAS NMR spectroscopy in an attempt to detect the effects of possible polymorphism. Both methods indicate that only single conformers exist in the solid-state for 1 and 2. 1,5- Bis[(4-cyanophenyl)- N-methylamino]pentane 1, crystallizes in the orthorhombic space group P2 12 12. The asymmetric unit contains one half of the ordered molecule. Only weak intermolecular interactions were found in solid-state, in which methyl groups are engaged.

  2. Triple α resonances in the {sup 6}Li + {sup 6}Li → 3α reaction at low energy

    Energy Technology Data Exchange (ETDEWEB)

    Tumino, A., E-mail: tumino@lns.infn.it [Facoltà di Ingegneria e Architettura, Università degli Studi di Enna “Kore”, Enna (Italy); INFN, Laboratori Nazionali del Sud, Catania (Italy); Bonasera, A.; Giuliani, G. [INFN, Laboratori Nazionali del Sud, Catania (Italy); Cyclotron Laboratory, Texas A& M University, College Station, TX (United States); Lattuada, M. [INFN, Laboratori Nazionali del Sud, Catania (Italy); Dipartimento di Fisica e Astronomia, Università di Catania, Catania (Italy); Milin, M. [Faculty of Science, University of Zagreb, Zagreb (Croatia); Pizzone, R.G. [INFN, Laboratori Nazionali del Sud, Catania (Italy); Spitaleri, C. [INFN, Laboratori Nazionali del Sud, Catania (Italy); Dipartimento di Fisica e Astronomia, Università di Catania, Catania (Italy); Tudisco, S. [INFN, Laboratori Nazionali del Sud, Catania (Italy)

    2015-11-12

    The {sup 6}Li + {sup 6}Li → 3α reaction has been measured in a kinematically complete experiment at 3.1 MeV of beam energy. The reaction mainly proceeds via intermediate {sup 8}Be states. The interaction between any two of the three α particles provides events with one, two or three {sup 8}Be interfering levels, with strong enhancement in the α–α coincidence yield. Evidence of three {sup 8}Be levels within the same 3α event suggests that one α particle is exchanged between the other two. This is a condition for Efimov states to occur in nuclei, for which no observation exists yet. The hyperspherical formalism for the low-energy three-body problem has been applied to point out the 3α particle correlation.

  3. Interface Induced Growth and Transformation of Polymer-Conjugated Proto-Crystalline Phases in Aluminosilicate Hybrids: A Multiple-Quantum (23)Na-(23)Na MAS NMR Correlation Spectroscopy Study.

    Science.gov (United States)

    Brus, Jiri; Kobera, Libor; Urbanova, Martina; Doušová, Barbora; Lhotka, Miloslav; Koloušek, David; Kotek, Jiří; Čuba, Pavel; Czernek, Jiri; Dědeček, Jiří

    2016-03-22

    Nanostructured materials typically offer enhanced physicochemical properties because of their large interfacial area. In this contribution, we present a comprehensive structural characterization of aluminosilicate hybrids with polymer-conjugated nanosized zeolites specifically grown at the organic-inorganic interface. The inorganic amorphous Al-O-Si framework is formed by alkali-activated low-temperature transformation of metakaoline, whereas simultaneous copolymerization of organic comonomers creates a secondary epoxide network covalently bound to the aluminosilicate matrix. This secondary epoxide phase not only enhances the mechanical integrity of the resulting hybrids but also introduces additional binding sites accessible for compensating negative charge on the aluminosilicate framework. This way, the polymer network initiates growth and subsequent transformation of protocrystalline short-range ordered zeolite domains that are located at the organic-inorganic interface. By applying an experimental approach based on 2D (23)Na-(23)Na double-quantum (DQ) MAS NMR spectroscopy, we discovered multiple sodium binding sites in these protocrystalline domains, in which immobilized Na(+) ions form pairs or small clusters. It is further demonstrated that these sites, the local geometry of which allows for the pairing of sodium ions, are preferentially occupied by Pb(2+) ions during the ion exchange. The proposed synthesis protocol thus allows for the preparation of a novel type of geopolymer hybrids with polymer-conjugated zeolite phases suitable for capturing and storage of metal cations. The demonstrated (23)Na-(23)Na DQ MAS NMR combined with DFT calculations represents a suitable approach for understanding the role of Na(+) ions in aluminositicate solids and related inorganic-organic hybrids, particularly their specific arrangement and clustering at interfacial areas.

  4. Solid state NMR of proteins at high MAS frequencies: symmetry-based mixing and simultaneous acquisition of chemical shift correlation spectra

    Energy Technology Data Exchange (ETDEWEB)

    Bellstedt, Peter [Fritz Lipmann Institute, Biomolecular NMR spectroscopy, Leibniz Institute for Age Research (Germany); Herbst, Christian [Ubon Ratchathani University, Department of Physics, Faculty of Science (Thailand); Haefner, Sabine; Leppert, Joerg; Goerlach, Matthias; Ramachandran, Ramadurai, E-mail: raman@fli-leibniz.de [Fritz Lipmann Institute, Biomolecular NMR spectroscopy, Leibniz Institute for Age Research (Germany)

    2012-12-15

    We have carried out chemical shift correlation experiments with symmetry-based mixing sequences at high MAS frequencies and examined different strategies to simultaneously acquire 3D correlation spectra that are commonly required in the structural studies of proteins. The potential of numerically optimised symmetry-based mixing sequences and the simultaneous recording of chemical shift correlation spectra such as: 3D NCAC and 3D NHH with dual receivers, 3D NC Prime C and 3D C Prime NCA with sequential {sup 13}C acquisitions, 3D NHH and 3D NC Prime H with sequential {sup 1}H acquisitions and 3D CANH and 3D C'NH with broadband {sup 13}C-{sup 15}N mixing are demonstrated using microcrystalline samples of the {beta}1 immunoglobulin binding domain of protein G (GB1) and the chicken {alpha}-spectrin SH3 domain.

  5. Spin-transfer pathways in paramagnetic lithium transition-metal phosphates from combined broadband isotropic solid-state MAS NMR spectroscopy and DFT calculations.

    Science.gov (United States)

    Clément, Raphaële J; Pell, Andrew J; Middlemiss, Derek S; Strobridge, Fiona C; Miller, Joel K; Whittingham, M Stanley; Emsley, Lyndon; Grey, Clare P; Pintacuda, Guido

    2012-10-17

    Substituted lithium transition-metal (TM) phosphate LiFe(x)Mn(1-x)PO(4) materials with olivine-type structures are among the most promising next generation lithium ion battery cathodes. However, a complete atomic-level description of the structure of such phases is not yet available. Here, a combined experimental and theoretical approach to the detailed assignment of the (31)P NMR spectra of the LiFe(x)Mn(1-x)PO(4) (x = 0, 0.25, 0.5, 0.75, 1) pure and mixed TM phosphates is developed and applied. Key to the present work is the development of a new NMR experiment enabling the characterization of complex paramagnetic materials via the complete separation of the individual isotropic chemical shifts, along with solid-state hybrid DFT calculations providing the separate hyperfine contributions of all distinct Mn-O-P and Fe-O-P bond pathways. The NMR experiment, referred to as aMAT, makes use of short high-powered adiabatic pulses (SHAPs), which can achieve 100% inversion over a range of isotropic shifts on the order of 1 MHz and with anisotropies greater than 100 kHz. In addition to complete spectral assignments of the mixed phases, the present study provides a detailed insight into the differences in electronic structure driving the variations in hyperfine parameters across the range of materials. A simple model delimiting the effects of distortions due to Mn/Fe substitution is also proposed and applied. The combined approach has clear future applications to TM-bearing battery cathode phases in particular and for the understanding of complex paramagnetic phases in general.

  6. Anéis aromáticos condensados e relação E4/E6: estudo de ácidos húmicos de gleissolos por RMN de 13C no estado sólido utilizando a técnica CP/MAS desacoplamento defasado Condensed aromatic rings and E4/E6 ratio: humic acids in gleysoils studied by NMR CP/MAS13C, and dipolar dephasing

    Directory of Open Access Journals (Sweden)

    Sérgio da Costa Saab

    2007-04-01

    Full Text Available In this work, seven samples of humic acids extracted from gleysoils were investigated. These studies, using NMR CP/MAS 13C techniques, did not show significant correlation between the E4/E6 ratio and the degree of aromaticity. However, dipolar dephasing (DD measurements of condensed aromatic or substituted carbons showed a negative correlation of 0.94. Also, there was a good correlation between the amount of semiquinone free radicals measured by the EPR technique and condensed aromatic rings measured by NMR CP/MAS 13C with the DD technique. The content of semiquinone free radicals was quantified by EPR spectroscopy and was correlated with the humification (degree of aromaticity of the humic substances. The results indicated that the E4/E6 ratio identifies the degree of aromatic rings condensation. It was also found that the degree of aromaticity, measured by NMR, as frequently presented in the literature (by conventional CP/MAS, underestimates aromatic rings in condensed structures.

  7. Condensed aromatic rings and E{sub 4}/E{sub 6} ratio: humic acids in gleysoils studied by NMR CP/MAS{sup 13}C, and dipolar dephasing; Aneis aromaticos condensados e relacao E{sub 4}/E{sub 6}: estudo de acidos humicos de gleissolos por RMN de {sup 13}C no estado solido utilizando a tecnica CP/MAS desacoplamento defasado

    Energy Technology Data Exchange (ETDEWEB)

    Saab, Sergio da Costa [Universidade Estadual de Ponta Grossa, PR (Brazil). Dept. de Fisica]. E-mail: scsaab@uepg.br; Martin-Neto, Ladislau [Empresa Brasileira de Pesquisa Agropecuaria, Sao Carlos, SP (Brazil)

    2007-03-15

    In this work, seven samples of humic acids extracted from gleysoils were investigated. These studies, using NMR CP/MAS {sup 13}C techniques, did not show significant correlation between the E{sub 4}/E{sub 6} ratio and the degree of aromaticity. However, dipolar dephasing (DD) measurements of condensed aromatic or substituted carbons showed a negative correlation of 0.94. Also, there was a good correlation between the amount of semiquinone free radicals measured by the EPR technique and condensed aromatic rings measured by NMR CP/MAS {sup 13}C with the DD technique. The content of semiquinone free radicals was quantified by EPR spectroscopy and was correlated with the humification (degree of aromaticity) of the humic substances. The results indicated that the E{sub 4}/E{sub 6} ratio identifies the degree of aromatic rings condensation. It was also found that the degree of aromaticity, measured by NMR, as frequently presented in the literature (by conventional CP/MAS), underestimates aromatic rings in condensed structures. (author)

  8. Substitution of lithium for magnesium, zinc, and aluminum in Li{sub 15}Si{sub 4}: crystal structures, thermodynamic properties, as well as {sup 6}Li and {sup 7}Li NMR spectroscopy of Li{sub 15}Si{sub 4} and Li{sub 15-x}M{sub x}Si{sub 4} (M=Mg, Zn, and Al)

    Energy Technology Data Exchange (ETDEWEB)

    Baran, Volodymyr; Faessler, Thomas F. [Department Chemie, Technische Universitaet Muenchen, Garching (Germany); Wuellen, Leo van [Department of Physics, University of Augsburg (Germany)

    2016-05-04

    An investigation into the substitution effects in Li{sub 15}Si{sub 4}, which is discussed as metastable phase that forms during electrochemical charging and discharging cycles in silicon anode materials, is presented. The novel partial substitution of lithium by magnesium and zinc is reported and the results are compared to those obtained for aluminum substitution. The new lithium silicides Li{sub 14}MgSi{sub 4} (1) and Li{sub 14.05}Zn{sub 0.95}Si{sub 4} (2) were synthesized by high-temperature reactions and their crystal structures were determined from single-crystal data. The magnetic properties and thermodynamic stabilities were investigated and compared with those of Li{sub 14.25}Al{sub 0.75}Si{sub 4} (3). The substitution of a small amount of Li in metastable Li{sub 15}Si{sub 4} for more electron-rich metals, such as Mg, Zn, or Al, leads to a vast increase in the thermodynamic stability of the resulting ternary compounds{sub .} The {sup 6,7}Li NMR chemical shift and spin relaxation time T{sub 1}-NMR spectroscopy behavior at low temperatures indicate an increasing contribution of the conduction electrons to these NMR spectroscopy parameters in the series for 1-3. However, the increasing thermal stability of the new ternary phases is accompanied by a decrease in Li diffusivity, with 2 exhibiting the lowest activation energy for Li mobility with values of 56, 60, and 62 kJ mol{sup -1} for 2, Li{sub 14.25}Al{sub 0.75}Si{sub 14}, and 1, respectively. The influence of the metastable property of Li{sub 15}Si{sub 4} on NMR spectroscopy experiments is highlighted. (copyright 2016 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  9. Elastic and inelastic scattering of {sup 6}Li + {sup 18}O versus {sup 7}Li + {sup 18}O and {sup 6}Li + {sup 16}O

    Energy Technology Data Exchange (ETDEWEB)

    Rudchik, Adam T., E-mail: rudchik@kinr.kiev.ua [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Kliczewski, Stanislaw [H. Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, ul. Radzikowskiego 152, PL-31-342 Cracow (Poland); Chercas, Kostyantyn A. [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Kemper, Kirby W. [Physics Department, Florida State University, Tallahassee, FL 32306-4350 (United States); Koshchy, Evgeniy I. [Kharkiv National University, pl. Svobody 4, 61077 Kharkiv (Ukraine); Rusek, Krzysztof [National Centre for Nuclear Research, ul. Hoża 69, PL-00-681 Warsaw (Poland); Heavy Ion Laboratory of Warsaw University, ul. L. Pasteura 5A, PL-02-093 Warsaw (Poland); Rudchik, Andryi A.; Mezhevych, Sergyi Yu.; Pirnak, Valeryi M. [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Plujko, Volodymyr A. [Taras Shevchenko Kyiv National University, vul. Volodymyrs' ka 64, 01033 Kyiv (Ukraine); Ponkratenko, Oleg A. [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Choiński, Jaroslaw [Heavy Ion Laboratory of Warsaw University, ul. L. Pasteura 5A, PL-02-093 Warsaw (Poland); Czech, Bronislaw; Siudak, Regina; Szczurek, Antoni [H. Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, ul. Radzikowskiego 152, PL-31-342 Cracow (Poland); Stolarz, Anna [Heavy Ion Laboratory of Warsaw University, ul. L. Pasteura 5A, PL-02-093 Warsaw (Poland); Zelinskyi, Ruslan M. [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine)

    2014-02-15

    Inverse kinematics scattering of {sup 18}O on {sup 6}Li at E{sub lab}({sup 18}O) = 114 MeV was measured to obtain elastic and inelastic scattering cross sections. In this way cross sections for excited states in {sup 6}Li and {sup 18}O were determined. The data were analyzed within the optical model and coupled reaction channel method. The {sup 6}Li + {sup 18}O optical potential as well as the {sup 6}Li and {sup 18}O deformation parameters were deduced. Contributions of different nuclear processes to the {sup 6}Li + {sup 18}O elastic and inelastic scattering were explored. The isotopic differences between the {sup 6,7}Li + {sup 18}O and {sup 6}Li + {sup 16,18}O potential parameters were determined.

  10. Direct Observation of Lattice Aluminum Environments in Li Ion Cathodes LiNi1-y-zCoyAlzO2 and Al-Doped LiNixMnyCozO2 via (27)Al MAS NMR Spectroscopy.

    Science.gov (United States)

    Dogan, Fulya; Vaughey, John T; Iddir, Hakim; Key, Baris

    2016-07-06

    Direct observations of local lattice aluminum environments have been a major challenge for aluminum-bearing Li ion battery materials, such as LiNi1-y-zCoyAlzO2 (NCA) and aluminum-doped LiNixMnyCozO2 (NMC). (27)Al magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy is the only structural probe currently available that can qualitatively and quantitatively characterize lattice and nonlattice (i.e., surface, coatings, segregation, secondary phase etc.) aluminum coordination and provide information that helps discern its effect in the lattice. In the present study, we use NMR to gain new insights into transition metal (TM)-O-Al coordination and evolution of lattice aluminum sites upon cycling. With the aid of first-principles DFT calculations, we show direct evidence of lattice Al sites, nonpreferential Ni/Co-O-Al ordering in NCA, and the lack of bulk lattice aluminum in aluminum-"doped" NMC. Aluminum coordination of the paramagnetic (lattice) and diamagnetic (nonlattice) nature is investigated for Al-doped NMC and NCA. For the latter, the evolution of the lattice site(s) upon cycling is also studied. A clear reordering of lattice aluminum environments due to nickel migration is observed in NCA upon extended cycling.

  11. Surface characteristics of the iron-oxyhydroxide layer formed during brick coatings by ESEM/EDS, {sup 23}Na and {sup 1}H MAS NMR, and ToF-SIMS

    Energy Technology Data Exchange (ETDEWEB)

    Allahdin, O. [Chaire Unesco « Sur la gestion de l' eau », Laboratoire Hydrosciences Lavoisier, Université de Bangui, Faculté des Sciences, B.P. 908 (Central African Republic); Wartel, M. [Université Lille1, Laboratoire LASIR (UMR CNRS 8516), Equipe Physico-chimie de l' Environnement, Bât. C8, 2" è" m" e étage, 59655 Villeneuve d' Ascq cedex (France); Mabingui, J. [Chaire Unesco « Sur la gestion de l' eau », Laboratoire Hydrosciences Lavoisier, Université de Bangui, Faculté des Sciences, B.P. 908 (Central African Republic); Revel, B. [Université Lille1, Service RMN, Bât. C4, 59655 Villeneuve d' Ascq cedex (France); Nuns, N. [Université Lille1, Institut Chevreul, 59655 Villeneuve d' Ascq cedex (France); Boughriet, A., E-mail: abdel.boughriet@univ-lille1.fr [Université Lille1, Laboratoire LASIR (UMR CNRS 8516), Equipe Physico-chimie de l' Environnement, Bât. C8, 2" è" m" e étage, 59655 Villeneuve d' Ascq cedex (France)

    2015-09-01

    Brick made locally by craftsmen in Bangui (Central African Republic) was modified first by HCl activation and second by iron-oxyhydroxide impregnation through the precipitation of ferric ions by NaOH at various fixed pH values (ranging from 3 to 13). The elemental analyses of synthesized compounds were performed using ICP-AES, and their surface chemistry/properties were investigated by environmental scanning electron microscopy (ESEM/EDS), {sup 1}H and {sup 23}Na MAS NMR spectroscopy, and time-of-flight secondary ion mass spectrometry (ToF-SIMS). The evidence of different {sup 23}Na chemical environments and the coexistence of Si and Al bound to ferrihydrite were made. The surface properties of this material which was found to be dependent upon synthesis pH, contributed to enhance metal uptake from water. - Highlights: • HCl-activated brick was coated at different Fe(III)-precipitation pH. • Surface properties were determined by ESEM, NMR and ToF-SIMS. • Al- and Si-bearing ferrihydrite and different Na environments were detected. • The pH used for modified-brick synthesis influenced metal uptake from water.

  12. Coulomb Breakup of Nucleus 6 Li on Ion 208Pb

    OpenAIRE

    Irgaziev, B. F.; ERGASHBAEV, H. T.

    1998-01-01

    In the framework of the three-body approach the A(a,bc)A Coulomb breakup has been investigated. The three-body Coulomb dynamic is taken into account to derive the expression for the reaction matrix element. The mechanism of the breakup includes the direct process and the excitation of resonance state of the particle a. The calculation of the triple differential cross section of the 208Pb(6Li, a d)208Pb Coulomb dissociation have been performed in the energy region Ea d < 1MeV. Cal...

  13. Proton-detected 3D (15)N/(1)H/(1)H isotropic/anisotropic/isotropic chemical shift correlation solid-state NMR at 70kHz MAS.

    Science.gov (United States)

    Pandey, Manoj Kumar; Yarava, Jayasubba Reddy; Zhang, Rongchun; Ramamoorthy, Ayyalusamy; Nishiyama, Yusuke

    2016-01-01

    Chemical shift anisotropy (CSA) tensors offer a wealth of information for structural and dynamics studies of a variety of chemical and biological systems. In particular, CSA of amide protons can provide piercing insights into hydrogen-bonding interactions that vary with the backbone conformation of a protein and dynamics. However, the narrow span of amide proton resonances makes it very difficult to measure (1)H CSAs of proteins even by using the recently proposed 2D (1)H/(1)H anisotropic/isotropic chemical shift (CSA/CS) correlation technique. Such difficulties due to overlapping proton resonances can in general be overcome by utilizing the broad span of isotropic chemical shifts of low-gamma nuclei like (15)N. In this context, we demonstrate a proton-detected 3D (15)N/(1)H/(1)H CS/CSA/CS correlation experiment at fast MAS frequency (70kHz) to measure (1)H CSA values of unresolved amide protons of N-acetyl-(15)N-l-valyl-(15)N-l-leucine (NAVL).

  14. Photoassociative creation of ultracold heteronuclear 6Li40K* molecules

    CERN Document Server

    Ridinger, Armin; Salez, Thomas; Fernandes, Diogo Rio; Bouloufa, Nadia; Dulieu, Olivier; Salomon, Christophe; Chevy, Frederic

    2011-01-01

    We investigate the formation of weakly bound, electronically excited, heteronuclear 6Li40K* molecules by single-photon photoassociation in a magneto-optical trap. We performed trap loss spectroscopy within a range of 325 GHz below the Li(2S_(1/2))+K(4P_(3/2)) and Li(2S_(1/2))+K(4P_(1/2)) asymptotic states and observed more than 60 resonances, which we identify as rovibrational levels of 7 of 8 attractive long-range molecular potentials. The long-range dispersion coefficients and rotational constants are derived. We find large molecule formation rates of up to ~3.5x10^7s^(-1), which are shown to be comparable to those for homonuclear 40K_2*. Using a theoretical model we infer decay rates to the deeply bound electronic ground-state vibrational level X^1\\Sigma^+(v'=3) of ~5x10^4s^(-1). Our results pave the way for the production of ultracold bosonic ground-state 6Li40K molecules which exhibit a large intrinsic permanent electric dipole moment.

  15. Three-body parameter for Efimov states in 6Li

    Science.gov (United States)

    Huang, Bo; O'Hara, Kenneth M.; Grimm, Rudolf; Hutson, Jeremy M.; Petrov, Dmitry S.

    2014-10-01

    We present a state-of-the-art reanalysis of experimental results on Efimov resonances in the three-fermion system of 6Li. We discuss different definitions of the three-body parameter (3BP) for Efimov states and adopt a definition that excludes effects due to deviations from universal scaling for low-lying states. We develop a finite-temperature model for the case of three distinguishable fermions and apply it to the excited-state Efimov resonance to obtain the most accurate determination to date of the 3BP in an atomic three-body system. Our analysis of ground-state Efimov resonances in the same system yields values for the three-body parameter that are consistent with the excited-state result. Recent work has suggested that the reduced 3BP for atomic systems is a near-universal quantity, almost independent of the particular atom involved. However, the value of the 3BP obtained for 6Li is significantly (˜20 % ) different from that previously obtained from the excited-state resonance in Cs. The difference between these values poses a challenge for theory.

  16. MAS NMR Study of the Metastable Solid Solutions Found in the LiFePO4/FePO4 System

    Energy Technology Data Exchange (ETDEWEB)

    Cabana, Jordi; Shirakawa, Junichi; Chen, Guoying; Richardson, Thomas; Grey, Clare P.

    2009-10-09

    Li and 3IP NMR experiments were conducted on a series of single- or two-phase samples in the LiFePCvFePCM system with different overall lithium contents, and containing the two end-members and/or two metastable solid solution hases, Lio.6FeP04 or Lio.34FeP04. These experiments were carried out at different temperatures in order to search for vacancy/charge ordering and ion/electron mobility in the metastable phases. Evidence for Li+-Fe2+ interactions was bserved for both Lio.6FeP04 and Lio.34FePC>4. The strength of this interaction leads to the formation of LiFePCvlike clusters in the latter, as shown by the room temperature data. Different motional processes are proposed to exist as the temperature is increased and various scenarios are discussed. While concerted lithium-electron hopping and/or correlations explains the data below 125C, evidence for some uncorrelated motion is found at higher temperatures, together with the onset of phase mixing.

  17. A generalized theoretical framework for the description of spin decoupling in solid-state MAS NMR: Offset effect on decoupling performance.

    Science.gov (United States)

    Tan, Kong Ooi; Agarwal, Vipin; Meier, Beat H; Ernst, Matthias

    2016-09-01

    We present a generalized theoretical framework that allows the approximate but rapid analysis of residual couplings of arbitrary decoupling sequences in solid-state NMR under magic-angle spinning conditions. It is a generalization of the tri-modal Floquet analysis of TPPM decoupling [Scholz et al., J. Chem. Phys. 130, 114510 (2009)] where three characteristic frequencies are used to describe the pulse sequence. Such an approach can be used to describe arbitrary periodic decoupling sequences that differ only in the magnitude of the Fourier coefficients of the interaction-frame transformation. It allows a ∼100 times faster calculation of second-order residual couplings as a function of pulse sequence parameters than full spin-dynamics simulations. By comparing the theoretical calculations with full numerical simulations, we show the potential of the new approach to examine the performance of decoupling sequences. We exemplify the usefulness of this framework by analyzing the performance of commonly used high-power decoupling sequences and low-power decoupling sequences such as amplitude-modulated XiX (AM-XiX) and its super-cycled variant SC-AM-XiX. In addition, the effect of chemical-shift offset is examined for both high- and low-power decoupling sequences. The results show that the cross-terms between the dipolar couplings are the main contributions to the line broadening when offset is present. We also show that the SC-AM-XIX shows a better offset compensation.

  18. Efimov Physics in a 6Li-133Cs Atomic Mixture

    Science.gov (United States)

    Johansen, Jacob; Feng, Lei; Parker, Colin; Chin, Cheng; Wang, Yujun

    2015-05-01

    We investigate Efimov physics based on three-body recombination in an atomic mixture of 6Li and 133Cs in the vicinity of interspecies Feshbach resonances at 843 and 889 G. This allows us to compare the loss spectra near different resonances and test the universality of Efimov states. Theoretically the Efimov spectrum near 889 G is expected to be similar to that near 843 G, except that the first resonance is absent near the former Feshbach resonance. This is due to the difference in the Cs-Cs scattering length near the two resonances: At 843 G it is negative, whereas at 889 G it is positive. Although it is primarily the Li-Cs interactions that lead to Efimov resonances, the Cs-Cs scattering length is expected to influence the spectrum. This work is supported by NSF and Chicago MRSEC.

  19. Theoretical calculations and analysis for n + 6Li reaction

    Science.gov (United States)

    Tao, Xi; Wang, Jimin; Chen, Guochang; Shen, Qingbiao

    2017-09-01

    R-matrix theory is an important methodology for applications on light, medium and heavy mass nuclides nuclear reaction in the resonance energy range. Full R-matrix formalism contains the diagonal elements of the energy levels matrix and it is a rigorous theory. Because of different assumptions and approximations, many kinds of R-matrix derived methods are obtained. The new R-matrix code FDRR is presented and includes 4 kinds of R-matrix applications. It can be used for calculating integral cross sections and angular distributions of 2-bodies reactions. The cross sections and angular distributions of n+ 6Li reaction are calculated and analyzed by FDRR code. The results are in good agreement with experimental data below 20 MeV.

  20. Lithium Ion Mobility in Lithium Phosphidosilicates: Crystal Structure, (7) Li, (29) Si, and (31) P MAS NMR Spectroscopy, and Impedance Spectroscopy of Li8 SiP4 and Li2 SiP2.

    Science.gov (United States)

    Toffoletti, Lorenzo; Kirchhain, Holger; Landesfeind, Johannes; Klein, Wilhelm; van Wüllen, Leo; Gasteiger, Hubert A; Fässler, Thomas F

    2016-12-05

    The need to improve electrodes and Li-ion conducting materials for rechargeable all-solid-state batteries has drawn enhanced attention to the investigation of lithium-rich compounds. The study of the ternary system Li-Si-P revealed a series of new compounds, two of which, Li8 SiP4 and Li2 SiP2 , are presented. Both phases represent members of a new family of Li ion conductors that display Li ion conductivity in the range from 1.15(7)×10(-6) Scm(-1) at 0 °C to 1.2(2)×10(-4) Scm(-1) at 75 °C (Li8 SiP4 ) and from 6.1(7)×10(-8) Scm(-1) at 0 °C to 6(1)×10(-6) Scm(-1) at 75 °C (Li2 SiP2 ), as determined by impedance measurements. Temperature-dependent solid-state (7) Li NMR spectroscopy revealed low activation energies of about 36 kJ mol(-1) for Li8 SiP4 and about 47 kJ mol(-1) for Li2 SiP2 . Both compounds were structurally characterized by X-ray diffraction analysis (single crystal and powder methods) and by (7) Li, (29) Si, and (31) P MAS NMR spectroscopy. Both phases consist of tetrahedral SiP4 anions and Li counterions. Li8 SiP4 contains isolated SiP4 units surrounded by Li atoms, while Li2 SiP2 comprises a three-dimensional network based on corner-sharing SiP4 tetrahedra, with the Li ions located in cavities and channels.

  1. An evaluation of microwave-driven stannylation followed by in situ {sup 119}Sn MAS n.m.r. spectroscopy as a probe for hydroxyl functionality in medium-rank British coals and macerals

    Energy Technology Data Exchange (ETDEWEB)

    Manak, H.; Monsef-Mirzai, P.; McWhinnie, W.R.; Hamor, T.A. [Aston University, Birmingham (United Kingdom). Dept. of Chemical Engineering and Applied Chemistry

    1997-07-01

    The paper describes the derivatization of hydroxyl groups in coals and coal macerals by stannylation. Stannylation of a range of phenolic compounds with Me{sub 3}SnCl, Bu{sub 3}SnCl and (Bu{sub 3}Sn){sub 2}O (TMTO) was carried out under both microwave-driven and conventional conditions. The degree of Stannylation was influenced by the steric environment of the OH group, implying that stannylation in comparison with, say trimethylsilylation of OH groups could help to map the steric environments of phenolic groups in coals. Good maceral separations of Creswell coal and acceptable separation of Cottonwood coal were achieved. The whole coals and the macerals were stannylated with TBTO under microwave-enhanced conditions and the products were examined by {sup 119}Sn MAS n.m.r. and X-ray photoelectron spectroscopy. The reaction was confined to surface regions. Differences were found in the behaviour of the macerals. The crystal and molecular structures of the trimethylstannyl derivative of 2,6-diphenylphenol were determined, to establish the validity of the claim to have stannylated model compounds. Molecular parameters were compared with related systems. 18 refs., 3 figs., 5 tabs.

  2. Characterization of polysulfone and polysulfone/vanillin microcapsules by 1H NMR spectroscopy, solid-state 13C CP/MAS-NMR spectroscopy, and N2 adsorption-desorption analyses.

    Science.gov (United States)

    Peña, Brisa; de Ménorval, Louis-Charles; Garcia-Valls, Ricard; Gumí, Tània

    2011-11-01

    Textile detergent and softener industries have incorporated perfume microencapsulation technology to improve their products. Perfume encapsulation allows perfume protection until use and provides a long-lasting fragrance release. But, certain industrial microcapsules show low encapsulation capacity and low material stability. Polysulfone capsules have been already proposed to solve these drawbacks. Among them, PSf/Vanillin capsules were considered as a desirable system. They present both good material stability and high encapsulation capacity. However, several factors such as the final location of the perfume in the polymeric matrix, the aggregation state that it has in the capsule and its interaction with the capsule components have not been studied yet. These factors can provide vast information about the capsule performance and its improvement. With the aim to characterize these parameters, the physical and chemical properties of PSf/Vanillin capsules have been investigated by nuclear magnetic resonance (NMR) spectroscopy, scanning electron microscopy (SEM), atomic force microscopy (AFM), and N(2) adsorption-desorption measurements. AFM micrograph and N(2) isotherms confirm that the presence of vanillin modify the physical structure of PSf/Vanillin microcapsules as it is trapped in the capsule porosity. NMR results show that vanillin is present in solid state in PSf/Vanillin microcapsules.

  3. High-energy break-up of 6Li as a tool to study the Big-Bang nucleosynthesis reaction 2H(alpha,gamma)6Li

    CERN Document Server

    Hammache, F; Typel, S; Galaviz, D; Sümmerer, K; Coc, A; Uhlig, F; Attallah, F; Caamano, M; Cortina, D; Geissel, H; Hellström, M; Iwasa, N; Kiener, J; Koczon, P; Kohlmeyer, B; Mohr, P; Schwab, E; Schwarz, K; Schümann, F; Senger, P; Sorlin, O; Tatischeff, V; Thibaud, J P; Vangioni, E; Wagner, A; Walus, W

    2010-01-01

    The recently claimed observations of non-negligible amounts of 6Li in old halo stars have renewed interest in the Big-Bang Nucleosynthesis (BBN) of 6Li. One important ingredient in the predicted BBN abundance of 6Li is the low-energy 2H(alpha,gamma)6Li cross section. Up to now, the only available experimental result for this cross section showed an almost constant astrophysical S-factor below 400 keV, contrary to theoretical expectations. We report on a new measurement of the 2H(alpha,gamma)6Li reaction using the break-up of 6Li at 150 A MeV. Even though we cannot separate experimentally the Coulomb contribution from the nuclear one, we find clear evidence for Coulomb-nuclear interference by analyzing the scattering-angular distributions. This is in-line with our theoretical description which indicates a drop of the S_24-factor at low energies as predicted also by most other models. Consequently, we find even lower upper limits for the calculated primordial 6Li abundance than before.

  4. Study on Effects of Acidic Extraction on Yield and Structure of Tobacco Pectin by CP/MAS 13C NMR Spectroscopy%CP/MAS 13C NMR技术分析酸提取对烟草果胶产率和结构的影响

    Institute of Scientific and Technical Information of China (English)

    李东亮; 谭兰兰; 高芸; 朱晓兰; 戴亚

    2015-01-01

    In order to investigate the fine structure of tobacco pectin and the key factors in extraction, the effects of extraction conditions (including pH, temperature and extraction time) on the yield, purity and structure of pectin were studied by cross-polarization/magic angle spinning 13C nuclear magnetic resonance (CP/MAS 13C NMR) spectroscopy. The results showed that: 1) The highest pectin yield (10.87%) achieved after extracting for 1.5 hours at pH 1.5 and 85 ℃; while polygalacturonic acid(PGA)reached its highest purity (78.4%) after extracting for 1.5 hours at pH 2.0 and 95 ℃. 2) The extraction conditions influenced the structure of pectin to a certain extent, the degrees of methylation (DM) and acetylation (DA) of pectin increased as pH value increased from 1.5 to 2.5, while decreased with the rise of temperature and the prolongation of extraction time significantly.%为研究烟草果胶的精细结构和掌握果胶提取的关键因素,采用交叉极化/魔角旋转固态核磁光谱技术(CP/MAS 13C NMR)考察了酸提取条件(pH、温度和提取时间)对烟草果胶产率、纯度(质量分数)及结构的影响。结果表明:①在pH 1.5和85℃条件下提取1.5 h时,烟草果胶得率最高,为10.87%,但在pH 2.0和95℃条件下提取1.5 h时,聚半乳糖醛酸(PGA)的纯度最高,为78.4%。②提取条件对烟草果胶的结构也有一定的影响,pH=1.5~2.5时,果胶的甲酯度(DM)和乙酰度(DA)均随pH升高而增大,随温度升高而降低,随提取时间延长而显著下降。

  5. THE 2H(alpha, gamma6LI REACTION AT LUNA AND BIG BANG NUCLEOSYNTHETIS

    Directory of Open Access Journals (Sweden)

    Carlo Gustavino

    2013-12-01

    Full Text Available The 2H(α, γ6Li reaction is the leading process for the production of 6Li in standard Big Bang Nucleosynthesis. Recent observations of lithium abundance in metal-poor halo stars suggest that there might be a 6Li plateau, similar to the well-known Spite plateau of 7Li. This calls for a re-investigation of the standard production channel for 6Li. As the 2H(α, γ6Li cross section drops steeply at low energy, it has never before been studied directly at Big Bang energies. For the first time the reaction has been studied directly at Big Bang energies at the LUNA accelerator. The preliminary data and their implications for Big Bang nucleosynthesis and the purported 6Li problem will be shown.

  6. All-optical production of 6Li quantum gases

    Science.gov (United States)

    Burchianti, A.; Seman, J. A.; Valtolina, G.; Morales, A.; Inguscio, M.; Zaccanti, M.; Roati, G.

    2015-03-01

    We report efficient production of quantum gases of 6Li using a sub-Doppler cooling scheme based on the D1 transition. After loading in a standard magneto-optical trap, an atomic sample of 109 atoms is cooled at a temperature of 40 μK by a bichromatic D1 gray-molasses. More than 2×107 atoms are then transferred into a high-intensity optical dipole trap, where a two-spin state mixture is evaporatively cooled down to quantum degeneracy. We observe that D1 cooling remains effective in the deep trapping potential, allowing an effective increase of the atomic phase-space density before starting the evaporation. In a total experimental cycle of 11 s, we produce weakly-interacting degenerate Fermi gases of 7×105 atoms at T/TF molecules. We further describe a simple and compact optical system both for high-resolution imaging and for imprinting a thin optical barrier on the atomic cloud; this represents a first step towards the study of quantum tunneling in strongly interacting superfluid Fermi gases.

  7. 6Li/7Li estimates for metal-poor stars

    CERN Document Server

    Perez, A E Garcia; Inoue, S; Ryan, S G; Suzuki, T K; Chiba, M

    2009-01-01

    The presence of the lithium-6 isotope in some metal-poor stars is a matter of surprise because of the high values observed. Non-standard models of Big Bang nucleosynthesis and pre-Galactic cosmic ray fusion and spallation have been proposed to explain these values. However, the observations of this light isotope are challenging which may make some detections disputable. The goal was to determine 6Li/7Li for a sample of metal-poor stars; three of them have been previously studied and the remaining two are new for this type of study. The purpose was to increase, if possible, the number of lithium-6 detections and to confirm previously published results. Spectra of the resonance doublet line of neutral lithium Li I 670.78nm were taken with the High Dispersion Spectrograph at the Subaru 8.2m-telescope for a sample of five metal-poor stars (-3.12 < [Fe/H] < -2.19). The contribution of lithium-6 to the total observed line profile was estimated from the 1D-LTE analysis of the line asymmetry. Observed asymmetri...

  8. MAS NMR study of the photoreceptor phytochrome

    NARCIS (Netherlands)

    Rohmer, Thierry

    2009-01-01

    Plants, algae and bacteria respond to light in various manners. The effect of light on the growth of plants is called photomorphogenesis and is regulated by the photoreceptor protein named phytochrome. Phytochrome is formed in the dark in its inactive red-absorbing (Pr) state and transformed upon ab

  9. {sup 6}Li foil scintillation sandwich thermal neutron detector

    Energy Technology Data Exchange (ETDEWEB)

    Ianakiev, K.D., E-mail: ianakiev@lanl.gov [Los Alamos National Laboratory, MS E540, Los Alamos, NM 87545 (United States); Swinhoe, M.T.; Favalli, A.; Chung, K.; MacArthur, D.W. [Los Alamos National Laboratory, MS E540, Los Alamos, NM 87545 (United States)

    2011-10-01

    Increasing needs for neutron detection and limited supply of {sup 3}He have led to the need for replacement neutron detection technology. This paper presents the design and initial results for a neutron detector ({sup 6}Li foil scintillator sandwich) that uses lithium metal foil to detect thermal neutrons. The reaction products, primarily triton, deposit most of their energy in thin scintillator films and create light pulses. Gamma rays can deposit only a small amount of energy in the thin films and so produce only very small light pulses. Lithium is preferable to boron in this application because triton escapes from lithium more easily than does the alpha particle from boron, allowing the use of thicker films and hence greater efficiency. In addition, triton has a higher light output in the scintillator than the boron alpha particle. Lithium metal is preferable to a lithium compound, such as lithium fluoride, because the number of tritons that escape from the metal is greater for the same amount of lithium. Monte Carlo simulations show that good efficiency values can be achieved with reasonably sized detectors, values that are greater than that of comparable {sup 3}He systems for portal monitors. In addition, simulations of a neutron coincidence counting concept show high counting efficiency and short die-away time (16 {mu}s), which imply better performance than that of the high-level neutron coincidence counter (HLNCC)-II. Initial experimental measurements on a prototype detector using alpha particles (having similar light output to the expected tritons) show good light collection and transport properties.

  10. Basic technology for 6Li enrichment using an ionic-liquid impregnated organic membrane

    Science.gov (United States)

    Hoshino, Tsuyoshi; Terai, Takayuki

    2011-10-01

    The tritium needed as a fuel for fusion reactors is produced by the neutron capture reaction of lithium-6 ( 6Li) in tritium breeding materials. However, natural Li contains only about 7.6 at.% 6Li. In this paper, a new lithium isotope separation technique using an ionic-liquid impregnated organic membrane is proposed. In order to separate and concentrate lithium isotopes, only lithium ions are able to move through the membrane by electrodialysis between the cathode and the anode in lithium solutions. Preliminary experiments of lithium isotope separation were conducted using this phenomenon. Organic membranes impregnated with TMPA-TFSI and PP13-TFSI as ionic liquids were prepared, and the relationship between the 6Li separation coefficient and the applied electrodialytic conditions was evaluated using them. The results showed that the 6Li isotope separation coefficient in this method (about 1.1-1.4) was larger than that in the mercury amalgam method (about 1.06).

  11. Search for the Halo Effect in the 1H(6He, 6Li)n Peaction

    Institute of Scientific and Technical Information of China (English)

    李志宏; 柳卫平; 白希祥; 王友宝; 连钢; 李志常; 申庆彪; 林承键; 曾晟; 符长波

    2002-01-01

    The angular distributions of the charge exchange reaction 1 H(6He, 6Li)n were measured in reverse kinematics with a secondary 6He beam at the energy of4.17 AMeV. The data were analysed in the context ora microscopic calculation. It is shown that both the ground state of6He and the second excited state of6Li (3.563 MeV, 0+) have a halo structure.

  12. 6LiF oleic acid capped nanoparticles entrapment in siloxanes for thermal neutron detection

    Science.gov (United States)

    Carturan, S.; Maggioni, G.; Marchi, T.; Gramegna, F.; Cinausero, M.; Quaranta, A.; Palma, M. Dalla

    2016-07-01

    The good light output of siloxane based scintillators as displayed under γ-rays and α particles has been exploited here to obtain clear and reliable response toward thermal neutrons. Sensitization towards thermal neutrons has been pursued by adding 6LiF, in form of nanoparticles. Aiming at the enhancement of compatibility between the inorganic nanoparticles and the low polarity, siloxane based surrounding medium, oleic acid-capped 6LiF nanoparticles have been synthesized by thermal decomposition of Li trifluoroacetate. Thin pellets siloxane scintillator maintained their optical transmittance up to weight load of 2% of 6Li. Thin samples with increasing 6Li concentration and thicker ones with fixed 6Li amount have been prepared and tested with several sources (α, γ-rays, moderated neutrons). Light output as high as 80% of EJ212 under α irradiation was measured with thin samples, and negligible changes have been observed as a result of 6LiF addition. In case of thick samples, severe light loss has been observed, as induced by opacity. Nevertheless, thermal neutrons detection has been assessed and the data have been compared with GS20, based on Li glass, taken as a reference material.

  13. Ultra-low temperature MAS-DNP

    Science.gov (United States)

    Lee, Daniel; Bouleau, Eric; Saint-Bonnet, Pierre; Hediger, Sabine; De Paëpe, Gaël

    2016-03-01

    Since the infancy of NMR spectroscopy, sensitivity and resolution have been the limiting factors of the technique. Regular essential developments on this front have led to the widely applicable, versatile, and powerful spectroscopy that we know today. However, the Holy Grail of ultimate sensitivity and resolution is not yet reached, and technical improvements are still ongoing. Hence, high-field dynamic nuclear polarization (DNP) making use of high-frequency, high-power microwave irradiation of electron spins has become very promising in combination with magic angle sample spinning (MAS) solid-state NMR experiments. This is because it leads to a transfer of the much larger polarization of these electron spins under suitable irradiation to surrounding nuclei, greatly increasing NMR sensitivity. Currently, this boom in MAS-DNP is mainly performed at minimum sample temperatures of about 100 K, using cold nitrogen gas to pneumatically spin and cool the sample. This Perspective deals with the desire to improve further the sensitivity and resolution by providing "ultra"-low temperatures for MAS-DNP, using cryogenic helium gas. Different designs on how this technological challenge has been overcome are described. It is shown that stable and fast spinning can be attained for sample temperatures down to 30 K using a large cryostat developed in our laboratory. Using this cryostat to cool a closed-loop of helium gas brings the additional advantage of sample spinning frequencies that can greatly surpass those achievable with nitrogen gas, due to the differing fluidic properties of these two gases. It is shown that using ultra-low temperatures for MAS-DNP results in substantial experimental sensitivity enhancements and according time-savings. Access to this temperature range is demonstrated to be both viable and highly pertinent.

  14. Determining the 6Li Doped Side of a Glass Scintillator for Ultra Cold Neutrons

    CERN Document Server

    Jamieson, Blair

    2015-01-01

    Ultracold neutron (UCN) detectors using two visually very similar, to the microscopic level, pieces of optically contacted Cerium doped lithium glasses have been proposed for high rate UCN experiments. The chief difference between the two glass scintillators is that one side is 6Li depleted and the other side Li doped. This note outlines a method to determine which side of the glass stack is doped with 6Li using AmBe and 252Cf neutron sources, and a Si surface barrier detector. The method sees an excess of events around the alpha and triton energies of neutron capture on 6Li when the enriched side is facing the Si surface barrier detector.

  15. Out-and-back {sup 13}C-{sup 13}C scalar transfers in protein resonance assignment by proton-detected solid-state NMR under ultra-fast MAS

    Energy Technology Data Exchange (ETDEWEB)

    Barbet-Massin, Emeline; Pell, Andrew J. [University of Lyon, CNRS/ENS Lyon/UCB Lyon 1, Centre de RMN a Tres Hauts Champs (France); Jaudzems, Kristaps [Latvian Institute of Organic Synthesis (Latvia); Franks, W. Trent; Retel, Joren S. [Leibniz-Institut fuer Molekulare Pharmakologie (Germany); Kotelovica, Svetlana; Akopjana, Inara; Tars, Kaspars [Biomedical Research and Study Center (Latvia); Emsley, Lyndon [University of Lyon, CNRS/ENS Lyon/UCB Lyon 1, Centre de RMN a Tres Hauts Champs (France); Oschkinat, Hartmut [Leibniz-Institut fuer Molekulare Pharmakologie (Germany); Lesage, Anne; Pintacuda, Guido, E-mail: guido.pintacuda@ens-lyon.fr [University of Lyon, CNRS/ENS Lyon/UCB Lyon 1, Centre de RMN a Tres Hauts Champs (France)

    2013-08-15

    We present here {sup 1}H-detected triple-resonance H/N/C experiments that incorporate CO-CA and CA-CB out-and-back scalar-transfer blocks optimized for robust resonance assignment in biosolids under ultra-fast magic-angle spinning (MAS). The first experiment, (H)(CO)CA(CO)NH, yields {sup 1}H-detected inter-residue correlations, in which we record the chemical shifts of the CA spins in the first indirect dimension while during the scalar-transfer delays the coherences are present only on the longer-lived CO spins. The second experiment, (H)(CA)CB(CA)NH, correlates the side-chain CB chemical shifts with the NH of the same residue. These high sensitivity experiments are demonstrated on both fully-protonated and 100 %-H{sup N} back-protonated perdeuterated microcrystalline samples of Acinetobacter phage 205 (AP205) capsids at 60 kHz MAS.

  16. Cosmic Ray Production of $^6$Li by Structure Formation Shocks in the Early Galaxy

    CERN Document Server

    Inoue, S; Inoue, Susumu; Suzuki, Takeru Ken

    2003-01-01

    We discuss the production of the element $^6$Li in the early Galaxy by cosmic rays accelerated at structure formation shocks, driven by the hierarchical merging of sub-Galactic halos during Galaxy formation. The salient features of this scenario are discussed and compared with observations of $^6$Li in metal-poor halo stars, including a recent Subaru HDS result on the star HD140283. Some unique predictions of the model are clearly testable by future observations and may also provide important insight into how the Galaxy formed.

  17. Properties of 4He and 6Li with improved chiral EFT interactions

    Directory of Open Access Journals (Sweden)

    Maris P.

    2016-01-01

    Full Text Available We present recent results for 4He and 6Li obtained with improved NN interactions derived from chiral effective field theory up to N4LO. The many-body calculations are performed order-by-order in the chiral expansion. At N3LO and N4LO additional renormalization using the Similarity Renormalization Group is adopted to improve numerical convergence of the many-body calculations. We discuss results for the ground state energies, as well as the magnetic moment and the low-lying spectrum of 6Li.

  18. Properties of 4He and 6Li with improved chiral EFT interactions

    Science.gov (United States)

    Maris, P.; Binder, S.; Calci, A.; Epelbaum, E.; Furnstahl, R. J.; Golak, J.; Hebeler, K.; Kamada, H.; Krebs, H.; Langhammer, J.; Liebig, S.; Meißner, U.-G.; Minossi, D.; Nogga, A.; Potter, H.; Roth, R.; Skibiński, R.; Topolnicki, K.; Vary, J. P.; Witala, H.

    2016-03-01

    We present recent results for 4He and 6Li obtained with improved NN interactions derived from chiral effective field theory up to N4LO. The many-body calculations are performed order-by-order in the chiral expansion. At N3LO and N4LO additional renormalization using the Similarity Renormalization Group is adopted to improve numerical convergence of the many-body calculations. We discuss results for the ground state energies, as well as the magnetic moment and the low-lying spectrum of 6Li.

  19. Resonant, direct, and transfer breakup of 6Li by 112Sn

    Science.gov (United States)

    Chattopadhyay, D.; Santra, S.; Pal, A.; Kundu, A.; Ramachandran, K.; Tripathi, R.; Sarkar, D.; Sodaye, S.; Nayak, B. K.; Saxena, A.; Kailas, S.

    2016-12-01

    Projectile breakup cross sections in the 6Li+112Sn reaction have been measured at two beam energies, 30 and 22 MeV. Cross sections for sequential breakup of 6Li into α +d via its resonant state of 1+ (5.65 MeV) in the continuum have been measured for the first time along with two other dominant resonant states of 3+ (2.18 MeV) and 2+ (4.31 MeV) at Ebeam=30 MeV. However, at 22 MeV, the α +d breakup is found to be only due to direct breakup process. Cross sections measured for sequential breakup via two transfer channels, (6Li,5Li ) and (6Li,8Be ), into α +p and α +α , respectively, and the above α +d breakup channels compared with the results of coupled-channels calculations unravel the reaction mechanisms involving a weakly bound projectile and different processes leading to large inclusive α -particle production.

  20. Hyperfine structure in photoassociative spectra of 6Li2 and 7Li2

    NARCIS (Netherlands)

    Abraham, E.R.I.; McAlexander, W.I.; Stoof, H.T.C.; Hulet, R.G.

    1996-01-01

    We present spectra of hyperfine resolved vibrational levels of the A1Σu+and 1 3Σg+ states of 6Li2 and 7Li2 obtained via photoassociation of colliding ultracold atoms in a magneto-optical trap. A simple first-order perturbation theory analysis accurately accounts for the frequency splittings and rela

  1. Basic technology for {sup 6}Li enrichment using an ionic-liquid impregnated organic membrane

    Energy Technology Data Exchange (ETDEWEB)

    Hoshino, Tsuyoshi, E-mail: hoshino.tsuyoshi@jaea.go.jp [Blanket Irradiation and Analysis Group, Fusion Research and Development Directorate, Japan Atomic Energy Agency, 4002, Narita-cho, Oarai-machi, Higashi Ibaraki-gun, Ibaraki 311-1393 (Japan); Terai, Takayuki [The Institute of Engineering Innovation and Department of Nuclear Engineering and Management School of Engineering, The University of Tokyo, 2-11-16 Yayoi, Bunkyo-ku, Tokyo 113-8656 (Japan)

    2011-10-01

    The tritium needed as a fuel for fusion reactors is produced by the neutron capture reaction of lithium-6 ({sup 6}Li) in tritium breeding materials. However, natural Li contains only about 7.6 at.% {sup 6}Li. In this paper, a new lithium isotope separation technique using an ionic-liquid impregnated organic membrane is proposed. In order to separate and concentrate lithium isotopes, only lithium ions are able to move through the membrane by electrodialysis between the cathode and the anode in lithium solutions. Preliminary experiments of lithium isotope separation were conducted using this phenomenon. Organic membranes impregnated with TMPA-TFSI and PP13-TFSI as ionic liquids were prepared, and the relationship between the {sup 6}Li separation coefficient and the applied electrodialytic conditions was evaluated using them. The results showed that the {sup 6}Li isotope separation coefficient in this method (about 1.1-1.4) was larger than that in the mercury amalgam method (about 1.06).

  2. A quantum degenerate Bose-Fermi mixture of 41K and 6Li

    Science.gov (United States)

    Wu, Yu-Ping; Yao, Xing-Can; Chen, Hao-Ze; Liu, Xiang-Pei; Wang, Xiao-Qiong; Chen, Yu-Ao; Pan, Jian-Wei

    2017-05-01

    We report a new apparatus for the study of two-species quantum degenerate mixture of 41K and 6Li atoms. We develop and combine several advanced cooling techniques to achieve both a large atom number and high phase space density of the two-species atom clouds. Furthermore, we build a high efficiency two-species magnetic transport system to transfer atom clouds from the 3D magneto-optical-trap chamber to a full glass science chamber of an extreme high vacuum environment and good optical access. We perform a forced radio-frequency evaporative cooling for 41K atoms while the 6Li atoms are sympathetically cooled in an optically plugged magnetic trap. Finally, we achieve the simultaneous quantum degeneracy for the 41K and 6Li atoms. The Bose-Einstein condensate of 41K has 1.4 × 105 atoms with a condensate fraction of about 62%, while the degenerate Fermi gas of 6Li has a total atom number of 5.4 × 105 at 0.25 Fermi temperature.

  3. VL51ES (Generation 6 Li-Ion Cell for Satellites

    Directory of Open Access Journals (Sweden)

    Defer M.

    2017-01-01

    Full Text Available This paper presents the design of Saft’s VL51ES (Generation 6 Li-Ion cell, the main challenges in the course of the development, the main BOL characteristics and performances achieved during the development program. Finally, it also describes how this cell fits in Saft’s battery range and the benefits of it.

  4. A refined model of the chlorosomal antennae of the green bacterium chlorobium tepidum from proton chemical shift constraints obtained with high-field 2-D and 3-D MAS NMR dipolar correlation spectroscopy

    NARCIS (Netherlands)

    Rossum, van B.E.J.; Steengaard, D.B.; Boender, G.J.; Schaffner, K.; Holzwarth, A.R.; Groot, de H.J.M.

    2001-01-01

    Heteronuclear 2-D and 3-D magic-angle spinning NMR dipolar correlation spectroscopy was applied to determine solid-state 1H shifts for aggregated bacteriochlorophyll c (BChl c) in uniformly 13C-enriched light harvesting chlorosomes of the green photosynthetic bacterium Chlorobium tepidum. A complete

  5. A refined model of the chlorosomal antennae of the green bacterium chlorobium tepidum from proton chemical shift constraints obtained with high-field 2-D and 3-D MAS NMR dipolar correlation spectroscopy

    NARCIS (Netherlands)

    Rossum, van B.E.J.; Steengaard, D.B.; Boender, G.J.; Schaffner, K.; Holzwarth, A.R.; Groot, de H.J.M.

    2001-01-01

    Heteronuclear 2-D and 3-D magic-angle spinning NMR dipolar correlation spectroscopy was applied to determine solid-state 1H shifts for aggregated bacteriochlorophyll c (BChl c) in uniformly 13C-enriched light harvesting chlorosomes of the green photosynthetic bacterium Chlorobium tepidum. A complete

  6. Gamow shell model description of radiative capture reactions $^6$Li$(p,\\gamma)$$^7$Be and $^6$Li$(n,\\gamma)$$^7$Li

    CERN Document Server

    Dong, G X; Fossez, K; Płoszajczak, M; Jaganathen, Y; Betan, R M Id

    2016-01-01

    According to standard stellar evolution, lithium abundance is believed to be a useful indicator of the stellar age. However, many evolved stars like red giants show huge fluctuations around expected theoretical abundances that are not yet fully understood. The better knowledge of nuclear reactions that contribute to the creation and destruction of lithium can help to solve this puzzle. In this work we apply the Gamow shell model (GSM) formulated in the coupled-channel representation (GSM-CC) to investigate the mirror radiative capture reactions $^6$Li$(p,\\gamma)$$^7$Be and $^6$Li$(n,\\gamma)$$^7$Li. The cross-sections are calculated using a translationally invariant Hamiltonian with the finite-range interaction which is adjusted to reproduce spectra, binding energies and one-nucleon separation energies in $^{6-7}$Li, $^7$Be. All relevant $E1$, $M1$, and $E2$ transitions from the initial continuum states to the final bound states $J={3/2}_1^-$ and $J={1/2}^-$ of $^7$Li and $^7$Be are included. We demonstrate th...

  7. Nuclear reactions of the system {sup 6} Li on {sup 58} Ni near the Coulomb barrier; Reacciones nucleares del sistema {sup 6} Li sobre {sup 58} Ni cerca de la barrera de Coulomb

    Energy Technology Data Exchange (ETDEWEB)

    Lizcano, D.; Aguilera, E.F.; Garcia M, H.; Martinez Q, E. [ININ, 52045 Ocoyoacac, Estado de Mexico (Mexico)

    2004-07-01

    Protons, alpha particles and deuterons coming from the reactions {sup 6} Li + {sup 58} Ni are detected to three different energy around the Coulomb barrier. The possible effects of the weakly bound character of the projectile are studied and the results are compared with previous data for the system {sup 6} Li + {sup 59} Co. (Author)

  8. Importance of $1n$-stripping process in the $^{6}$Li+$^{159}$Tb reaction

    CERN Document Server

    Pradhan, M K; Roy, Subinit; Basu, P; Goswami, A; Kshetri, R; Palit, R; Parkar, V V; Ray, M; Sarkar, M Saha; Santra, S

    2013-01-01

    The inclusive cross sections of the $\\alpha$-particles produced in the reaction $^{6}$Li+$^{159}$Tb have been measured at energies around the Coulomb barrier. The measured cross sections are found to be orders of magnitude larger than the calculated cross sections of $^{6}$Li breaking into $\\alpha$ and $d$ fragments, thus indicating contributions from other processes. The experimental cross sections of $1n$-stripping and $1n$-pickup processes have been determined from an entirely different measurement, reported earlier. Apart from incomplete fusion and/ $d$-transfer processes, the $1n$-stripping process is found to be a significant contributor to the inclusive $\\alpha$-particle cross sections in this reaction.

  9. Narrow-linewidth cooling of $^{6}$Li atoms using the 2S-3P transition

    CERN Document Server

    Chen, Hao-Ze; Wu, Yu-Ping; Liu, Xiang-Pei; Wang, Xiao-Qiong; Chen, Yu-Ao; Pan, Jian-Wei

    2016-01-01

    We report on a narrow-linewidth cooling of $^{6}$Li atoms using the $2S_{1/2}\\to 3P_{3/2}$ transition in the ultraviolet (UV) wavelength regime. By combining the traditional red magneto-optical trap (MOT) at 671 nm and the UV MOT at 323 nm, we obtain a cold sample of $1.3\\times10^9$ atoms with a temperature of 58 $\\mu$K. Furthermore, we demonstrate a high efficiency magnetic transport for $^{6}$Li atoms with the help of the UV MOT. Finally, we obtain $8.1\\times10^8$ atoms with a temperature of 296 $\\mu$K at a magnetic gradient of 198 G/cm in the science chamber with a good vacuum environment and large optical access.

  10. Scintillation properties of semiconducting 6LiInSe2 crystals to ionizing radiation

    Science.gov (United States)

    Wiggins, Brenden; Groza, Michael; Tupitsyn, Eugene; Lukosi, Eric; Stassun, Keivan; Burger, Arnold; Stowe, Ashley

    2015-11-01

    6LiInSe2 has gained attention recently as a semiconducting thermal neutron detector. As presented herein, the chalcogenide compound semiconductor also detects incident neutrons via scintillation, making 6LiInSe2 the only lithium containing semiconductor to respond to neutrons via both detection mechanisms. Both yellow and red crystals, which appear in the literature, were investigated. Only the yellow crystal responded favorably to ionizing radiation, similar to the semiconducting operation utilizing electrodes. The obtained light yield for yellow crystals is 4400 photons/MeV, referenced to Bi4Ge3O12 (BGO).The estimated thermal neutron light yield was 21,000 photons/thermal neutron. The two measured decay time components were found to be 31±1 ns (49%) and 143±9 ns (51%).This crystal provides efficient, robust detection of neutrons via scintillation with respectable light yield and rapid response, enabling its use for a broad array of neutron detection applications.

  11. Optimization of a sup 6 LiF bolometric neutron detector

    CERN Document Server

    Silver, C S; Piccirillo, L; Timbie, P T; Zhou, J W

    2002-01-01

    The optimization of a sup 6 LiF bolometer for neutron spectroscopy applications has been accomplished with a series of 12 different detectors. This type of detector is similar to X-ray bolometers, which have been extensively studied, and the absorber has a high neutron capture cross-section. Each bolometer was irradiated with alpha particles to investigate its response to thermal pulses. The best resolution obtained with this series of bolometers was 39 keV FWHM at 5.3 MeV. One of the bolometers was calibrated with monoenergetic neutrons, and its thermal properties are derived from measurements over a range of temperatures. We discuss the considerations involved in optimizing a sup 6 LiF bolometer for different types of neutron applications.

  12. Autler-Townes splitting in two-color photoassociation of 6Li

    CERN Document Server

    Schloeder, U; Silber, C; Zimmermann, C; Schloeder, Ulrike; Deuschle, Thomas; Silber, Christian; Zimmermann, Claus

    2003-01-01

    We report on high-resolution two-color photoassociation spectroscopy in the triplet system of magneto-optically trapped 6Li. The absolute transition frequencies have been measured. Strong optical coupling of the bound molecular states has been observed as Autler-Townes splitting in the photoassociation signal. The spontaneous bound-bound transition rate is determined and the molecule formation rate is estimated. The observed lineshapes are in good agreement with the theoretical model.

  13. Formation of eta'(958) Meson Bound States by the 6Li(gamma,d) reaction

    CERN Document Server

    Miyatani, M; Nagahiro, H; Hirenzaki, S

    2016-01-01

    We have investigated the 6Li(gamma,d) reaction theoretically for the formation of the eta'(958) mesic nucleus close to the recoilless kinematics. We have developed the theoretical formula and reported the quantitative results of the formation spectra for various cases in this article. We have found that the formation cross sections are reduced by the effects of the fragile deuteron form factor.

  14. Optimization of {sup 6}LiF:ZnS(Ag) Scintillator Light Yield Using Geant4

    Energy Technology Data Exchange (ETDEWEB)

    Yehuda-Zada, Y. [Nuclear Research Center Negev, Beer-Sheva (Israel); Ben-Gurion University (Israel); Pritchard, K.; Ziegler, J.B.; Cooksey, C.; Siebein, K. [National Institute of Standards and Technology, Gaithersburg, Maryland (United States); Jackson, M.; Hurlbut, C. [Eljen Technology, Sweetwater Texas (United States); Kadmon, Y.; Cohen, Y.; Maliszewskyj, N.C. [Nuclear Research Center Negev, Beer-Sheva (Israel); Ibberson, R.M.; Majkrzak, C.F. [National Institute of Standards and Technology, Gaithersburg, Maryland (United States); Orion, Y. [Ben-Gurion University (Israel); Osovizky, A. [National Institute of Standards and Technology, Gaithersburg, Maryland (United States); Rotem Industries Ltd, Rotem Industrial Park (Israel); University of Maryland (United States)

    2015-07-01

    Neutrons provide an effective tool to probe materials structure. Neutron diffraction is a method to determine the atomic and magnetic structure of a material based on neutron scattering. By this method a collimated incident beam of thermal neutrons heat the examined sample and based on the obtained diffraction pattern information on the structure of the material is provided. Research for developing a novel cold neutron detector for Chromatic Analysis Neutron Diffractometer Or Reflectometer (CANDOR) is underway at the NIST center for neutron research. The system unique design is aimed to provide over ten times fold faster analysis of materials than conventional system. In order to achieve the fast analysis a large number of neutron detectors is required. A key design constraint for this detector is the thickness of the neutron sensitive element. This is met using {sup 6}LiF:ZnS(Ag) scintillation material with embedded wavelength shifting (WLS) fibers conducting scintillation light to silicon photomultiplier photo-sensors. The detector sensitivity is determined by both the neutron capture probability ({sup 6}Li density) and the detectable light output produced by the ZnS(Ag) ionization, the latter of which is hindered by the fluorescence absorption of the scintillation light by the ZnS. Tradeoffs between the neutron capture probability, stimulated light production and light attenuation for determining the optimal stoichiometry of the {sup 6}LiF and ZnS(Ag) as well as the volume ratio of scintillator and fiber. Simulations performed using the GEANT4 Monte Carlo package were made in order to optimize the detector design. GEANT4 enables the investigation of the neutron interaction with the detector, the ionization process and the light transfer process following the nuclear process. The series of conversions required for this detector were modelled: - A cold neutron enters the sensor and is captured by {sup 6}Li in the scintillator mixture ({sup 6}Li (n,α) {sup 3}H

  15. {sup 6}Li breakup and suppression of complete fusion above the Coulomb barrier

    Energy Technology Data Exchange (ETDEWEB)

    Elmahdy, N.A. [Modern Academy for Engineering and Technology, Cairo (Egypt); Denikin, A.S. [Dubna International University, Dubna (Russian Federation); JINR, Flerov Laboratory of Nuclear Reactions, Dubna (Russian Federation); Ismail, M.; Ellithi, A.Y. [Cairo University, Cairo (Egypt)

    2015-05-15

    We study the role of the projectile breakup in the fusion process by example of the {sup 6}Li reactions with the {sup 59}Co, {sup 144}Sm and {sup 209}Bi targets in vicinity of the Coulomb barrier. The coupled channel and distorted wave approaches are employed in order to calculate the complete fusion and the breakup cross sections, respectively. The partial cross sections in both the channels are compared in order to estimate the breakup fraction responsible for the suppression of complete fusion. The calculations are compared with available experimental data. The conclusions and recommendations are made. (orig.)

  16. Model Calculation of n + 6Li Reactions Below 20 MeV

    Institute of Scientific and Technical Information of China (English)

    ZHANG Jing-Shang; HAN Yin-Lu

    2001-01-01

    Based on the unified Hauser-Feshbach and exciton model for light nuclei, the calculations of reaction cross sections and the double-differential cross sections for n + 6Li are performed. Since all of the first-particle emissions are from the compound nucleus to the discrete levels, the angular momentum coupling effect in pre-equilibrium mechanism must be taken into account. The fitting of the measured data indicates that the three-body break-up process needs to be involved, and the pre-equilibrium reaction mechanism dominates the reaction processes. In light nucleus reactions the recoil effect must be taken into account.``

  17. Characterization of the silicon+6LiF thermal neutron detection technique

    Science.gov (United States)

    Pappalardo, A.; Barbagallo, M.; Cosentino, L.; Marchetta, C.; Musumarra, A.; Scirè, C.; Scirè, S.; Vecchio, G.; Finocchiaro, P.

    2016-02-01

    The worldwide need to replace 3He for neutron detection has triggered research and development on new technologies and methods. A promising one is based on commercial solid state silicon detectors coupled with thin neutron converter layers containing 6Li. After proving the feasibility of this technique, we characterized the behavior of such a detector with different converter layer thicknesses. In this paper we also disentangle other contributions to the overall spectrum shape observed with this kind of detector, proving that its detection efficiency can be made reasonably high and that the gamma/neutron discrimination capability is comparable to that of 3He tubes.

  18. Characterization of the silicon+6LiF thermal neutron detection technique

    CERN Document Server

    Pappalardo, A; Cosentino, L; Marchetta, C; Musumarra, A; Scirè, C; Scirè, S; Vecchio, G; Finocchiaro, P

    2015-01-01

    The worldwide need to replace 3He for the neutron detection has triggered R&D on new technologies and methods. A promising one is based on commercial solid state silicon detectors coupled with thin neutron converter layers containing 6Li. After proving the feasibility of this technique, we characterized the behavior of such a detector with different converter layer thicknesses. In this paper we also disentangle other contributions to the overall spectrum shape observed with this kind of detector, proving that its detection efficiency can be made reasonably high and that the gamma/neutron discrimination capability is comparable to the one of 3He tubes.

  19. Comparative analysis of pulse shape discrimination methods in a {sup 6}Li loaded plastic scintillator

    Energy Technology Data Exchange (ETDEWEB)

    Balmer, Matthew J.I., E-mail: m.balmer@lancaster.ac.uk [Department of Engineering, Lancaster University, LA1 4YR (United Kingdom); Gamage, Kelum A.A. [Department of Engineering, Lancaster University, LA1 4YR (United Kingdom); Taylor, Graeme C. [Neutron Metrology Group, National Physical Laboratory, Teddington, TW11 0LW (United Kingdom)

    2015-07-11

    Three algorithms for discriminating between fast neutrons, thermal neutrons and gamma rays in a {sup 6}Li loaded plastic scintillator have been compared. Following a literature review of existing pulse shape discrimination techniques, the performance of the charge comparison method, triangular filtering and frequency gradient analysis were investigated in this work. The scintillator was exposed to three different mixed gamma/neutron radiation fields. The figure of merit of neutron/gamma separation was investigated over a broad energy range, as well as for the neutron capture energy region. After optimisation, all three methods were found to perform similarly in terms of neutron/gamma separation.

  20. Study of silicon+6LiF thermal neutron detectors: GEANT4 simulations versus real data

    Science.gov (United States)

    Meo, S. Lo; Cosentino, L.; Mazzone, A.; Bartolomei, P.; Finocchiaro, P.

    2017-09-01

    Research and development on alternative thermal neutron detection technologies and methods are nowadays needed as a possible replacement of 3He-based ones. Commercial solid state silicon detectors, coupled with neutron converter layers containing 6Li, have been proved to represent a viable solution for several applications as present in the literature. In order to better understand the detailed operation and the response and efficiency of such detectors, a series of dedicated GEANT4 simulations were performed and compared with real data collected in a few different configurations. The results show an excellent agreement between data and simulations, indicating that the behavior of the detector is fully understood.

  1. Characterization of the silicon+{sup 6}LiF thermal neutron detection technique

    Energy Technology Data Exchange (ETDEWEB)

    Pappalardo, A. [INFN Laboratori Nazionali del Sud, Catania (Italy); Barbagallo, M. [INFN Sezione di Bari (Italy); Cosentino, L.; Marchetta, C. [INFN Laboratori Nazionali del Sud, Catania (Italy); Musumarra, A. [INFN Laboratori Nazionali del Sud, Catania (Italy); Università di Catania (Italy); Scirè, C.; Scirè, S.; Vecchio, G.; Finocchiaro, P. [INFN Laboratori Nazionali del Sud, Catania (Italy)

    2016-02-21

    The worldwide need to replace {sup 3}He for neutron detection has triggered research and development on new technologies and methods. A promising one is based on commercial solid state silicon detectors coupled with thin neutron converter layers containing {sup 6}Li. After proving the feasibility of this technique, we characterized the behavior of such a detector with different converter layer thicknesses. In this paper we also disentangle other contributions to the overall spectrum shape observed with this kind of detector, proving that its detection efficiency can be made reasonably high and that the gamma/neutron discrimination capability is comparable to that of {sup 3}He tubes.

  2. Astrophysical S factor for the radiative-capture reaction p{sup 6}Li {yields} {sup 7}Be{gamma}

    Energy Technology Data Exchange (ETDEWEB)

    Dubovichenko, S. B., E-mail: sergey@dubovichenko.ru [National Space Agency of the Republic of Kazakhstan, Fessenkov Astrophysical Institute, National Center of Space Research and Technology (Kazakhstan); Burtebaev, N., E-mail: burteb@inp.kz; Zazulin, D. M.; Kerimkulov, Zh. K. [National Nuclear Center of Republic of Kazakhstan, Institute of Nuclear Physics (Kazakhstan); Amar, A. S. A. [Al-Farabi Kazakh National University (Kazakhstan)

    2011-07-15

    A new measurement of differential cross sections for elastic p{sup 6}Li scattering in the energy range 0.35-1.2 MeV was performed. A partial-wave analysis of the data obtained in this way was carried out, and potentials simulating the p{sup 6}Li interaction were constructed. Various experiments devoted to studying elastic p{sup 6}Li scattering over the broad energy range of 0.5-50 MeV were analyzed on the basis of the optical model. By using the potentials obtained from the partial-wave analysis, the possibility of describing the astrophysical S factor for radiative proton capture on {sup 6}Li at low energies was considered within the potential cluster model involving forbidden states.

  3. Solvent signal suppression for high-resolution MAS-DNP

    Science.gov (United States)

    Lee, Daniel; Chaudhari, Sachin R.; De Paëpe, Gaël

    2017-05-01

    Dynamic nuclear polarization (DNP) has become a powerful tool to substantially increase the sensitivity of high-field magic angle spinning (MAS) solid-state NMR experiments. The addition of dissolved hyperpolarizing agents usually results in the presence of solvent signals that can overlap and obscure those of interest from the analyte. Here, two methods are proposed to suppress DNP solvent signals: a Forced Echo Dephasing experiment (FEDex) and TRAnsfer of Populations in DOuble Resonance Echo Dephasing (TRAPDORED) NMR. These methods reintroduce a heteronuclear dipolar interaction that is specific to the solvent, thereby forcing a dephasing of recoupled solvent spins and leaving acquired NMR spectra free of associated resonance overlap with the analyte. The potency of these methods is demonstrated on sample types common to MAS-DNP experiments, namely a frozen solution (of L-proline) and a powdered solid (progesterone), both containing deuterated glycerol as a DNP solvent. The proposed methods are efficient, simple to implement, compatible with other NMR experiments, and extendable past spectral editing for just DNP solvents. The sensitivity gains from MAS-DNP in conjunction with FEDex or TRAPDORED then permits rapid and uninterrupted sample analysis.

  4. Pulse-Shape Analysis of Neutron-Induced Scintillation Light in Ni-doped 6LiF/ZnS

    Energy Technology Data Exchange (ETDEWEB)

    Cowles, Christian C.; Behling, Richard S.; Imel, G. R.; Kouzes, Richard T.; Lintereur, Azaree; Robinson, Sean M.; Stave, Sean C.; Siciliano, Edward R.; Wang, Zheming

    2016-10-06

    Abstract–Alternatives to 3He are being investigated for gamma-ray insensitive neutron detection applications, including plutonium assay. One promising material is lithium-6 fluoride with silver activated zinc sulfide 6LiF/ZnS(Ag) in conjunction with a wavelength shifting plastic. Doping the 6LiF/ZnS(Ag) with nickel (Ni) has been proposed as a means of reducing the decay time of neutron signal pulses. This research performed a pulse shape comparison between Ni-doped and non-doped 6LiF/ZnS(Ag) neutron pulses. The Ni-doped 6LiF/ZnS(Ag) had a 32.7% ± 0.3 increase in neutron pulse height and a 32.4% ± 0.3 decrease in neutron pulse time compared to the non-doped 6LiF/ZnS(Ag). Doping 6LiF/ZnS(Ag) with nickel may allow neutron detector operation with improved signal to noise ratios, and reduced pulse pileup affects, increasing the accuracy and range of source activities with which such a detector could operate.

  5. On the nuclear $(n;t)-$reaction in the three-electron ${}^{6}$Li atom

    CERN Document Server

    Frolov, Alexei M

    2012-01-01

    The nuclear $(n;t)-$reaction of the three-electron ${}^{6}$Li atom with thermal/slow neutrons is considered. An effective method has been developed for determining the probabilities of formation of various atoms and ions in different bound states. We discuss a number of fundamental questions directly related to numerical computations of the final state atomic probabilities. A few appropriate variational expansions for atomic wave functions of the incident lithium atom and final helium atom and/or tritium negatively charged ion are discussed. It appears that the final ${}^4$He atom arising during the nuclear $(n,{}^{6}$Li; ${}^4$He$,t)$-reaction in the three-electron Li atom can also be created in its triplet states. The formation of the quasi-stable three-electron $e^{-}_3$ during the nuclear $(n; t)-$reaction at the Li atom is briefly discussed. Bremsstrahlung emitted by atomic electrons accelerated by the rapidly moving fragments from this reaction is analyzed. The frequency spectrum of the emitted radiatio...

  6. Scintillation properties of semiconducting {sup 6}LiInSe{sub 2} crystals to ionizing radiation

    Energy Technology Data Exchange (ETDEWEB)

    Wiggins, Brenden [Y-12 National Security Complex, Oak Ridge, TN (United States); Vanderbilt University, Nashville, TN (United States); Groza, Michael; Tupitsyn, Eugene [Fisk University, Nashville, TN (United States); Lukosi, Eric [University of Tennessee, Knoxville, TN (United States); Stassun, Keivan; Burger, Arnold [Vanderbilt University, Nashville, TN (United States); Fisk University, Nashville, TN (United States); Stowe, Ashley [Y-12 National Security Complex, Oak Ridge, TN (United States); Vanderbilt University, Nashville, TN (United States); University of Tennessee, Knoxville, TN (United States)

    2015-11-21

    {sup 6}LiInSe{sub 2} has gained attention recently as a semiconducting thermal neutron detector. As presented herein, the chalcogenide compound semiconductor also detects incident neutrons via scintillation, making {sup 6}LiInSe{sub 2} the only lithium containing semiconductor to respond to neutrons via both detection mechanisms. Both yellow and red crystals, which appear in the literature, were investigated. Only the yellow crystal responded favorably to ionizing radiation, similar to the semiconducting operation utilizing electrodes. The obtained light yield for yellow crystals is 4400 photons/MeV, referenced to Bi{sub 4}Ge{sub 3}O{sub 12} (BGO).The estimated thermal neutron light yield was 21,000 photons/thermal neutron. The two measured decay time components were found to be 31±1 ns (49%) and 143±9 ns (51%).This crystal provides efficient, robust detection of neutrons via scintillation with respectable light yield and rapid response, enabling its use for a broad array of neutron detection applications.

  7. Optimizing ZnS/6LiF scintillators for wavelength-shifting-fiber neutron detectors

    Energy Technology Data Exchange (ETDEWEB)

    Crow, Lowell [ORNL; Funk, Loren L [ORNL; Hannan, Bruce W [ORNL; Hodges, Jason P [ORNL; Riedel, Richard A [ORNL; Wang, Cai-Lin [ORNL

    2016-01-01

    In this paper we compare the performance of grooved and flat ZnS/6LiF scintillators in a wavelength shifting-fiber (WLSF) detector. Flat ZnS/6LiF scintillators with the thickness L=0.2-0.8 mm were characterized using photon counting and pulse-height analysis and compared to a grooved scintillator of approximately 0.8 mm thick. While a grooved scintillator considerably increases the apparent thickness of the scintillator to neutrons for a given coating thickness, we find that the flat scintillators perform better than the grooved scintillators in terms of both light yield and neutron detection efficiency. The flat 0.8-mm-thick scintillator has the highest light output, and it is 52% higher compared with a grooved scintillator of same thickness. The lower light output of the grooved scintillator as compared to the flat scintillator is consistent with the greater scintillator-WLSF separation and the much larger average emission angle of the grooved scintillator. We also find that the average light cone width, or photon travel-length as measured using time-of-flight powder diffraction of diamond and vanadium, decreases with increasing L in the range of L=0.6-0.8 mm. This result contrasts with the traditional Swank diffusion model for micro-composite scintillators, and could be explained by a decrease in photon diffusion-coefficient or an increase in micro-particle content in the flat scintillator matrix for the thicker scintillators.

  8. Line shift, line asymmetry, and the 6Li/7Li isotopic ratio determination

    CERN Document Server

    Cayrel, Roger; Chand, Hum; Bonifacio, Piercarlo; Spite, Monique; Spite, François; Petitjean, Patrick; Ludwig, Hans-Günter; Caffau, Elisabetta

    2007-01-01

    Context: Line asymmetries are generated by convective Doppler shifts in stellar atmospheres, especially in metal-poor stars, where convective motions penetrate to higher atmospheric levels. Such asymmetries are usually neglected in abundance analyses. The determination of the 6Li/7Li isotopic ratio is prone to suffering from such asymmetries, as the contribution of 6Li is a slight blending reinforcement of the red wing of each component of the corresponding 7Li line, with respect to its blue wing. Aims: The present paper studies the halo star HD 74000 and estimates the impact of convection-related asymmetries on the Li isotopic ratio determination. Method: Two methods are used to meet this aim. The first, which is purely empirical, consists in deriving a template profile from another element that can be assumed to originate in the same stellar atmospheric layers as Li I, producing absorption lines of approximately the same equivalent width as individual components of the 7Li I resonance line. The second metho...

  9. Two-proton pickup studies with the (6Li,8B) reaction

    Energy Technology Data Exchange (ETDEWEB)

    Weisenmiller, R.B.

    1976-12-03

    The (/sup 6/Li,/sup 8/B) reaction has been investigated on targets of /sup 26/Mg, /sup 24/Mg, /sup 16/O, /sup 13/C, /sup 12/C, /sup 11/B, /sup 10/B, and /sup 9/Be at a bombarding energy of 80.0 MeV, and on targets of /sup 16/O, /sup 12/C, /sup 9/Be, /sup 7/Li, and /sup 6/Li at a bombarding energy of 93.3 MeV. Only levels consistent with direct, single-step two-proton pickup reaction mechanisms were observed to be strongly populated. On T/sub z/ = 0 targets, the spectroscopic selectivity of this reaction resembles that of the analogous (p,t) reaction. Additionally, these data demonstrate the dominance of spatially symmetric transfer of the two protons. On T/sub z/ greater than 0 targets the (/sup 6/Li,/sup 8/B) reaction was employed to locate two previously unreported levels (at 7.47 +- 0.05 MeV and 8.86 +- 0.07 MeV) in the T/sub z/ = 2 nuclide /sup 24/Ne and to establish the low-lying 1p-shell states in the T/sub z/ = /sup 3///sub 2/ nuclei /sup 11/Be, /sup 9/Li, and /sup 7/He. However, no evidence was seen for any narrow levels in the T/sub z/ = /sup 3///sub 2/ nuclide /sup 5/H nor for any narrow excited states in /sup 7/He. The angular distributions reported here are rather featureless and decrease monotonically with increasing angle. This behavior can be shown by a semi-classical reaction theory to be a consequence of the reaction kinematics. A semi-classical approach also suggests that the kinematic term in the transition matrix element is only weakly dependent upon the angular momentum transfer (which is consistent with simple Distorted Wave Born Approximation calculations). However, only qualitative agreement was obtained between the observed relative transition yields and semi-classical predictions, using the two-nucleon coefficients of fractional parentage of Cohen and Kurath, probably due to the limitations of the semi-classical reaction theory.

  10. Fusion excitation function measurement for 6Li+64Ni at near-barrier energies

    Directory of Open Access Journals (Sweden)

    Shaikh Md. Moin

    2015-01-01

    Full Text Available Total fusion excitation function has been measured for the reaction of weakly bound 6Li projectile on medium mass 64Ni target at energies near the Coulomb barrier of the system. Online characteristic γ-ray detection method has been used to identify and determine the cross sections of the residues. No suppression of total fusion cross section (σTF is observed at above barrier energies. But enhancement of measured cross section with respect to the one-dimensional barrier penetration model (1-DBPM calculation is observed at below barrier energies. The enhancement can not be explained by coupled channels calculation with dominant projectile and target excitations as well as one-neutron stripping reaction.

  11. MeV Neutron Production from Thermal Neutron Capture in {6}^Li Simulated with Geant4

    CERN Document Server

    Santoro, Valentina; Bentley, Phillip M

    2015-01-01

    Various Li compounds are commonly used at neutron facilities as neutron absorbers. These compounds provide one of the highest ratios of neutron attenuation to $\\gamma$-ray production. Unfortunately, the usage of these compounds can also give rise to fast neutron emission with energies up to almost 16 MeV. Historically, some details in this fast neutron production mechanism can be absent from some modeling packages under some optimization scenarios. In this work, we tested Geant4 to assess the performance of this simulation toolkit for the fast neutron generation mechanism. We compare the results of simulations performed with Geant4 to available measurements. The outcome of our study shows that results of the Geant4 simulations are in good agreement with the available measurements for $^6$Li fast neutron production, and suitable for neutron instrument background evaluation at spallation neutron sources.

  12. Reaction mechanisms in the {sup 6}Li + {sup 59}Co system

    Energy Technology Data Exchange (ETDEWEB)

    Souza, F.A. [Instituto de Fisica - Universidade de Sao Paulo, Departamento de Fisica Nuclear, C.P. 66318, 05315-970 Sao Paulo, SP (Brazil)], E-mail: fsouza@dfn.if.usp.br; Beck, C. [Institut Pluridisciplinaire Hubert Curien, UMR 7178, CNRS-IN2P3 et Universite Louis Pasteur, Boite Postale 28, F-67037 Strasbourg, Cedex 2 (France); Carlin, N. [Instituto de Fisica - Universidade de Sao Paulo, Departamento de Fisica Nuclear, C.P. 66318, 05315-970 Sao Paulo, SP (Brazil); Keeley, N. [CEA-Saclay DSM/IRFU/SPhN, F-91191 Gif sur Yvette Cedex (France); Neto, R. Liguori; Moura, M.M. de; Munhoz, M.G.; Del Santo, M.G.; Suaide, A.A.P.; Szanto, E.M.; Szanto de Toledo, A. [Instituto de Fisica - Universidade de Sao Paulo, Departamento de Fisica Nuclear, C.P. 66318, 05315-970 Sao Paulo, SP (Brazil)

    2009-04-15

    The reactions induced by the weakly bound {sup 6}Li projectile interacting with the intermediate mass target {sup 59}Co were investigated. Light charged particles singles and {alpha}-d coincidence measurements were performed at the near barrier energies E{sub lab}=17.4, 21.5, 25.5 and 29.6 MeV. The main contributions of the different competing mechanisms are discussed. A statistical model analysis, Continuum-Discretized Coupled-Channels (CDCC) calculations and two-body kinematics were used as tools to provide information to disentangle the main components of these mechanisms. A significant contribution of the direct breakup was observed through the difference between the experimental sequential breakup cross section and the CDCC prediction for the non-capture breakup cross section.

  13. alpha. - d resonances and the low-lying states of sup 6 Li

    Energy Technology Data Exchange (ETDEWEB)

    Eskandarian, A.; Afnan, I.R. (School of Physical Sciences, The Flinders University of South Australia, Bedford Park, South Australia 5042 (Australia))

    1992-12-01

    The low-lying states (below the {sup 3}He-{sup 3}H threshold) of the {sup 6}Li nucleus are generated using three-body models with two-body nonlocal separable interactions between the constituent particles. The positions and widths of the states are determined by searching for the eigenvalues of the kernel of the Faddeev equations in the complex energy plane. When appropriate (for {ital T}=0 states only), the results are compared with a separate determination of these quantities from the {alpha}-{ital d} scattering process. All experimentally observed levels are found. Given that the Coulomb interaction is not included in our calculations, agreement with experiment is favorable for both the positions and the widths of the resonances.

  14. α-d resonances and the low-lying states of 6Li

    Science.gov (United States)

    Eskandarian, A.; Afnan, I. R.

    1992-12-01

    The low-lying states (below the 3-3H threshold) of the 6Li nucleus are generated using three-body models with two-body nonlocal separable interactions between the constituent particles. The positions and widths of the states are determined by searching for the eigenvalues of the kernel of the Faddeev equations in the complex energy plane. When appropriate (for T=0 states only), the results are compared with a separate determination of these quantities from the α-d scattering process. All experimentally observed levels are found. Given that the Coulomb interaction is not included in our calculations, agreement with experiment is favorable for both the positions and the widths of the resonances.

  15. Time-of-flight calibration of a 6Li glass epithermal neutron detector

    Science.gov (United States)

    Livingston; Saleh; Block; Brand

    2000-10-01

    The curing of Portland cement concrete involves the conversion of water from a free to a bound state. The process can be monitored nondestructively by measuring the shift in the neutron energy spectrum in the epithermal range (0.025-1 eV). A tuned array of 6Li glass detectors has been constructed with varying efficiencies over the epithermal energy range. To determine the efficiency of each detector as a function of neutron energy, it is necessary to calibrate it against a reference neutron spectrum. This was accomplished using a time-of-flight approach with a pulsed neutron beam produced at the Gaerttner LINAC Laboratory at Rensselaer Polytechnic Institute. With a neutron flight path of 25 m it was possible to determine the neutron detector efficiencies to an energy resolution of 11 microeV. The data showed good agreement with the detector design calculations.

  16. Thermal neutron detection by entrapping 6LiF nanocrystals in siloxane scintillators

    Science.gov (United States)

    Carturan, S. M.; Marchi, T.; Maggioni, G.; Gramegna, F.; Degerlier, M.; Cinausero, M.; Dalla Palma, M.; Quaranta, A.

    2015-06-01

    Exploiting the long experience in design and production of scintillating mixtures based on siloxane matrices with combinations of primary dye and waveshifter, a first set of 6LiF loaded scintillator disks has been produced. The synthesis is herein described and reported, as well as preliminary results on their light response towards thermal neutrons. The preservation of transparency and mechanical integrity of the scintillator material is challenging when introducing the inorganic salt LiF which is a "foreign body" to the organic polysiloxane host matrix Different strategies such as synthesis of nanoparticles and surface functionalization have been pursued to succeed in the entrapment of the neutron converter whilst maintaining moderate light output, optical transparency and flexibility of the base scintillator.

  17. MeV Neutron Production from Thermal Neutron Capture in 6Li Simulated With Geant4

    Science.gov (United States)

    Santoro, Valentina; DiJulio, Douglas D.; Bentley, Phillip M.

    2016-09-01

    Various Li compounds are commonly used at neutron facilities as neutron absorbers. These compounds provide one of the highest ratios of neutron attenuation to y- ray production. Unfortunately, the usage of these compounds can also give rise to fast neutron emission with energies up to almost 16 MeV. Historically, some details in this fast neutron production mechanism can be absent from some modeling packages under some optimization scenarios. In this work, we tested Geant4 to assess the performance of this simulation toolkit for the fast neutron generation mechanism. We compare the results of simulations performed with Geant4 to available measurements. The outcome of our study shows that results of the Geant4 simulations are in good agreement with the available measurements for 6 Li fast neutron production, and suitable for neutron instrument background evaluation at spallation neutron sources.

  18. Observation of repulsive Fermi polarons in a resonant mixture of ultracold ${}^6$Li atoms

    CERN Document Server

    Scazza, F; Massignan, P; Recati, A; Amico, A; Burchianti, A; Fort, C; Inguscio, M; Zaccanti, M; Roati, G

    2016-01-01

    We employ radio-frequency spectroscopy to investigate a polarized spin-mixture of ultracold ${}^6$Li atoms close to a broad Feshbach scattering resonance. Focusing on the regime of strong repulsive interactions, we observe well-defined coherent quasiparticles even for unitarity-limited interactions. We characterize the many-body system by extracting the key properties of repulsive Fermi polarons: the energy $E_+$, the effective mass $m^*$, the residue $Z$ and the decay rate $\\Gamma$. Above a critical interaction, $E_+$ is found to exceed the Fermi energy of the bath while $m^*$ diverges and even turns negative. Such findings reveal that the paramagnetic Fermi liquid state becomes thermodynamically unstable towards an energetically favored ferromagnetic phase.

  19. Investigation of α-cluster states in 13C via the (6Li,d) reaction

    CERN Document Server

    Rodrigues, M R D; Horodynski-Matsushigue, L B; Cunsolo, A; Cappuzzello, F; Duarte, J L M; Rodrigues, C L; Ukita, G M; Souza, M A; Miyake, H

    2010-01-01

    The 9Be(6Li,d)13C reaction was used to investigate possible α-cluster states in 13C. The reaction was measured at 25.5 MeV incident energy, employing the São Paulo Pelletron-Enge-Spectrograph facility and the nuclear emulsion detection technique. Ten out of sixteen known levels of 13C, up to 11 MeV of excitation, were observed and, due to the much improved energy resolution of 50 keV, at least three doublets could be resolved. This work presents a preliminary analysis of five of the most intensely populated states, also in comparison with the results of former transfer studies.

  20. Alpha cluster states in light nuclei populated through the (6Li,d) reaction

    Energy Technology Data Exchange (ETDEWEB)

    Borello-Lewin, Thereza; Rodrigues, M.R.D.; Horodynski-Matsushigue, L.B.; Duarte, J.L.M.; Rodrigues, C.L.; Souza, M.A. [Universidade de Sao Paulo (IF/USP), SP (Brazil). Inst. de Fisica; Cunsolo, A.; Cappuzzello, F. [Universita di Catania (Italy). Istituto Nazionale di Fisica Nucleare. Lab. Nazionali del Sud; Ukita, Gilberto Mitsuo [Universidade de Santo Amaro (UNISA), Sao Paulo, SP (Brazil). Fac. de Psicologia

    2011-07-01

    Full text: The alpha cluster correlation is an important concept in the nuclear physics of light nuclei. The main purpose of the research program in progress is the investigation of the alpha clustering phenomenon in (x{alpha}) and(x{alpha}+{nu}) nuclei through the ({sup 6}Li,d) alpha transfer reaction. In fact, there is scarce experimental information on the subject, in particular associated with resonant states predicted near (x{alpha}) and (x{alpha}+{nu}) thresholds. Measurements of the {sup 12},{sup 13}C({sup 6}Li,d) {sup 16},{sup 17}O reactions, at an incident energy of 25.5 MeV, have been performed employing the Sao Paulo Pelletron-Enge Split-Pole facility and the nuclear emulsion detection technique. The work is under way and an experimental energy resolution of 30 keV was obtained. Near the (4{alpha}) breakup threshold in {sup 16}O, three narrow alpha resonances, not previously measured, were detected, revealing important {alpha} + {sup 12}C(G.S.) components. One of these resonances corresponds to the known 0{sup +} state at 15.1 MeV[5] of excitation that has probably, according to Funaki et al., the gas like configuration of the 4{alpha} condensate state, with a very dilute density and a large component of {alpha} + {sup 12}C(Hoyle) configuration. As was already mentioned, our experimental information points to the necessity of including the {alpha} + {sup 12}C(G.S.) component in the wave function. (author)

  1. Fast neutron measurements with 7Li and 6Li enriched CLYC scintillators

    Science.gov (United States)

    Giaz, A.; Blasi, N.; Boiano, C.; Brambilla, S.; Camera, F.; Cattadori, C.; Ceruti, S.; Gramegna, F.; Marchi, T.; Mattei, I.; Mentana, A.; Million, B.; Pellegri, L.; Rebai, M.; Riboldi, S.; Salamida, F.; Tardocchi, M.

    2016-07-01

    The recently developed Cs2LiYCl6:Ce (CLYC) crystals are interesting scintillation detectors not only for their gamma energy resolution (<5% at 662 keV) but also for their capability to identify and measure the energy of both gamma rays and fast/thermal neutrons. The thermal neutrons were detected by the 6Li(n,α)t reaction while for the fast neutrons the 35Cl(n,p)35S and 35Cl(n,α)32P neutron-capture reactions were exploited. The energy of the outgoing proton or α particle scales linearly with the incident neutron energy. The kinetic energy of the fast neutrons can be measured using both the Time Of Flight (TOF) technique and using the CLYC energy signal. In this work, the response to monochromatic fast neutrons (1.9-3.8 MeV) of two CLYC 1″×1″ crystals was measured using both the TOF and the energy signal. The observables were combined to identify fast neutrons, to subtract the thermal neutron background and to identify different fast neutron-capture reactions on 35Cl, in other words to understand if the detected particle is an α or a proton. We performed a dedicated measurement at the CN accelerator facility of the INFN Legnaro National Laboratories (Italy), where the fast neutrons were produced by impinging a proton beam (4.5, 5.0 and 5.5 MeV) on a 7LiF target. We tested a CLYC detector 6Li-enriched at about 95%, which is ideal for thermal neutron measurements, in parallel with another CLYC detector 7Li-enriched at more than 99%, which is suitable for fast neutron measurements.

  2. Fast neutron measurements with {sup 7}Li and {sup 6}Li enriched CLYC scintillators

    Energy Technology Data Exchange (ETDEWEB)

    Giaz, A., E-mail: agnese.giaz@mi.infn.it [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Blasi, N.; Boiano, C.; Brambilla, S. [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Camera, F. [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Università degli Studi di Milano, Physics Department, Via Celoria 16, 20133 Milano (Italy); Cattadori, C. [INFN sezione di Milano Bicocca, Piazza della Scienza 3, 20125 Milano (Italy); Ceruti, S. [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Università degli Studi di Milano, Physics Department, Via Celoria 16, 20133 Milano (Italy); Gramegna, F.; Marchi, T. [INFN Laboratori Nazionali di Legnaro, Viale dell’Università, 2, 35020 Legnaro, PD (Italy); Mattei, I. [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Mentana, A. [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Università degli Studi di Milano, Physics Department, Via Celoria 16, 20133 Milano (Italy); Million, B.; Pellegri, L. [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Rebai, M. [Università degli Studi di Milano Bicocca, Physics Department, Piazza della Scienza 3, 20126 Milano (Italy); Riboldi, S. [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Università degli Studi di Milano, Physics Department, Via Celoria 16, 20133 Milano (Italy); Salamida, F. [INFN sezione di Milano Bicocca, Piazza della Scienza 3, 20125 Milano (Italy); Tardocchi, M. [Istituto di Fisica del Plasma, Associazione EURATOM-ENEA-CNR, Via R. Cozzi 53, 2015 Milano (Italy)

    2016-07-21

    The recently developed Cs{sub 2}LiYCl{sub 6}:Ce (CLYC) crystals are interesting scintillation detectors not only for their gamma energy resolution (<5% at 662 keV) but also for their capability to identify and measure the energy of both gamma rays and fast/thermal neutrons. The thermal neutrons were detected by the {sup 6}Li(n,α)t reaction while for the fast neutrons the {sup 35}Cl(n,p){sup 35}S and {sup 35}Cl(n,α){sup 32}P neutron-capture reactions were exploited. The energy of the outgoing proton or α particle scales linearly with the incident neutron energy. The kinetic energy of the fast neutrons can be measured using both the Time Of Flight (TOF) technique and using the CLYC energy signal. In this work, the response to monochromatic fast neutrons (1.9–3.8 MeV) of two CLYC 1″×1″ crystals was measured using both the TOF and the energy signal. The observables were combined to identify fast neutrons, to subtract the thermal neutron background and to identify different fast neutron-capture reactions on {sup 35}Cl, in other words to understand if the detected particle is an α or a proton. We performed a dedicated measurement at the CN accelerator facility of the INFN Legnaro National Laboratories (Italy), where the fast neutrons were produced by impinging a proton beam (4.5, 5.0 and 5.5 MeV) on a {sup 7}LiF target. We tested a CLYC detector {sup 6}Li-enriched at about 95%, which is ideal for thermal neutron measurements, in parallel with another CLYC detector {sup 7}Li-enriched at more than 99%, which is suitable for fast neutron measurements.

  3. The Astrophysical S-factor for the 2H(, )6Li Nuclear Reaction at Low-Energies

    Indian Academy of Sciences (India)

    H. Sadeghi; A. Moghadasi; M. Ghamary

    2014-12-01

    The alpha radiative capture reactions are the key to understand about primordial nucleosynthesis and the observed abundance of light nucleus in stars. The astrophysical S-factor for the process 2H(, )6Li has been calculated at the low-energies relevant to big-bang nucleosynthesis and in comparison with laboratory data. On the basis of the model, the alpha radiative capture process is studied by using the two-and three-body electromagnetic currents. The bound and resonance states of 6Li are calculated via an inverse process, deuteron- photodisintegration of a 6Li nucleus. In comparison with other theoretical approaches and available laboratory data, excellent agreement is achieved for the astrophysical S-factor of this process.

  4. Photoassociation spectroscopy of long-range molecular states below the 2s + 3p 6Li2 asymptote

    Science.gov (United States)

    Gross, Christian; Chaudhuri, Saptarishi; Gan, Jaren; Dieckmann, Kai

    2015-05-01

    We present photoassociation spectra of high-lying vibrational states of the interatomic potentials correlating to the 2s + 3p asymptote of 6Li2 . Starting from an atomic cloud in a magneto-optical trap we first drive a free-to-bound transition into a molecular bound state using a tunable ultra-violet laser. Thereafter we ionize these long-range molecules using a 532 nm laser and detect the resulting ions with a channeltron. We determine the absolute positions of the transitions with MHz precision utilizing a frequency comb based calibration. Lithium dimers are extensively studied theoretically using various models and methods. Spectroscopic measurements are crucial to test and benchmark these methods and are available for various electronic states and inter-nuclear distances of 6Li2 molecule. Our study provides the first experimental observation of long-range states of the 2s + 3p asymptote of 6Li2 .

  5. Tritium production in a sphere of /sup 6/LiD irradiated by 14-MeV neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Hemmendinger, A.; Ragan, C.E.; Shunk, E.R.; Ellis, A.N.; Anaya, J.M.; Wallace, J.M.

    1978-10-01

    The specific production of tritium in samples of /sup 6/LiH and /sup 7/LiH embedded in a 600-mm-diam sphere of /sup 6/LiD irradiated by a central source of 14-MeV neutrons was determined by measuring the activity of the hydrogen evolved from the samples of each isotope at each of five different radii in the /sup 6/LiD assembly. The entire process of decomposing the LiH, transferring the evolved gas into counters, and determining the decay rate was standardized by processing LiH samples irradiated by thermal neutrons for which the /sup 6/Li(n,..cap alpha..) cross section is well known. The specific production of tritium in /sup 6/LiH and /sup 7/LiH (embedded samples) and the activation of radiochemical detector foils of /sup 45/Sc, /sup 89/Y, /sup 90/Zr, /sup 169/Tm, /sup 191/Ir /sub 373/, /sup 193/Ir /sub 627/, /sup 197/Au, /sup 235/U, and /sup 238/U placed at various positions in the /sup 6/LiD sphere were calculated and compared with the experimental data. One- and three-dimensional Monte Carlo and S/sub n/ neutron-transport calculations were performed. The most reliable (three-dimensional Monte Carlo) calculation is in reasonable agreement with both the tritium-production and the radiochemical-activation data. The existing discrepancies between calculation and experiment appear largely attributable to uncertainties in some tritium-production and radiochemical-activation cross sections. 15 references.

  6. An atomic beam of 6Li — 7Li for high resolution spectroscopy from matrix isolation sublimation

    Science.gov (United States)

    Oliveira, A. N.; Sacramento, R. L.; Silva, B. A.; Uhlmann, F. O.; Wolff, W.; Cesar, C. L.

    2016-07-01

    We propose the Matrix Isolation Sublimation (MlSu) technique for generating cold lithium atoms for the measurement of the 6Li - 7Li isotope shift in D1 and D2 transitions. The technique is capable of generating cold 6Li and 7Li beams at 4 K with forward velocity of 125 m/s. Using this beam we offer a distinguished source of lithium atoms for transitions measurements, adding a new possibility to make high resolution spectroscopy towards improving the experimental checks of the theory.

  7. TiO{sub 2} colloidal nanocrystals surface modification by V{sub 2}O{sub 5} species: Investigation by {sup 47,49}Ti MAS-NMR and H{sub 2}, CO and NO{sub 2} sensing properties

    Energy Technology Data Exchange (ETDEWEB)

    Epifani, Mauro, E-mail: mauro.epifani@le.imm.cnr.it [Consiglio Nazionale delle Ricerche—Istituto per la Microelettronica e Microsistemi (CNR–IMM), via Monteroni c/o Campus Universitario, I-73100 Lecce (Italy); Comini, Elisabetta [SENSOR Lab, Department of Information Engineering, Brescia University and CNR-INO, via Valotti 9, 25133 Brescia (Italy); Díaz, Raül [Electrochemical Processes Unit, IMDEA Energy Institute, Avda. Ramón de la Sagra 3, 28935 Móstoles (Spain); Force, Carmen [NMR Unit, Centro de Apoyo Tecnológico, Universidad Rey Juan Carlos, c/Tulipán, s/n, 28933 Móstoles (Spain); Siciliano, Pietro [Consiglio Nazionale delle Ricerche—Istituto per la Microelettronica e Microsistemi (CNR–IMM), via Monteroni c/o Campus Universitario, I-73100 Lecce (Italy); Faglia, Guido [SENSOR Lab, Department of Information Engineering, Brescia University and CNR-INO, via Valotti 9, 25133 Brescia (Italy)

    2015-10-01

    Highlights: • Novel sensing architecture is presented, made by V{sub 2}O{sub 5} modification of TiO{sub 2} surface. • MAS NMR techniques are a powerful tool for studying the influence of the V{sub 2}O{sub 5} layer. • The V{sub 2}O{sub 5} surface deposition enhanced the adsorption properties with respect to pure TiO{sub 2}. - Abstract: TiO{sub 2} and TiO{sub 2}–V{sub 2}O{sub 5} nanocrystals were prepared by coupling sol–gel and solvothermal methods, followed by heat-treatment at 400 °C, after which the mean nanocrystal size was about 5 nm. The materials were characterized by X-ray diffraction, transmission electron microscopy and solid state nuclear magnetic resonance spectroscopy. It was shown that while the TiO{sub 2} phase was always anatase even after heat-treatment at 500 °C, the presence of the vanadium oxide species enhanced the surface re-configuration of the Ti ions. Hence the coordination environment of surface Ti atoms was drastically changed, by formation of further bonds and imposition of a given local geometry. The final hypothesis was that in pure titania surface rearrangement occurs, leading to the new NMR signal, but this modification was favored in the TiO{sub 2}–V{sub 2}O{sub 5} sample, where the Ti surface atoms were forced into the final configurations by the bonding with V atoms through oxygen. The materials heat-treated at 400 °C were used to process chemoresistive sensors, which were tested to hydrogen, CO and NO{sub 2}, as examples of gases with peculiar sensing mechanisms. The results evidenced that the surface deposition of V{sub 2}O{sub 5} onto the anatase TiO{sub 2} nanocrystals was effective in modifying the adsorption properties of the anatase nanocrystals.

  8. In situ MAS NMR Study on Propane Activation over Ga-modified H-ZSM-5 Under Mild Condition%原位固体核磁共振研究温和条件下丙烷在镓改性H-ZSM-5上的活化

    Institute of Scientific and Technical Information of China (English)

    邹雁; 石磊; 马卓娜; 朱卡克; 贺鹤勇

    2003-01-01

    @@ 将价格低廉、储量丰富的低碳烷烃(C1~C5)转化为高附加值的工业产品是多相催化研究中的一个重要领域[1~6]. 镓改性的H-ZSM-5催化剂已被广泛应用于丙烷芳构化的工业化生产中[7,8]. 然而, 由于低碳烷烃中碳碳和碳氢键的高稳定性, 低碳烷烃的转化通常需要较高的反应温度, 因此开发可在温和条件下工作的低碳烷烃功能化反应的催化剂是一个重要的研究方向. 使用原位魔角旋转核磁共振(MAS NMR)技术和13C标记的反应物在研究低碳烷烃的活化中具有独特的优越性[9,10]. Derouane等[11]首次采用MAS NMR技术研究2-13C-丙烷在温和条件下(573 K)在镓负载的H-ZSM-5的酸性和氧化还原双功能活性位上转化为1份2-13C-丙烷和2份1-13C-丙烷反应, 提出了质子化准环丙烷(PPCP)中间体的丙烷活化机理. 为温和条件下丙烷活化和功能化开拓了一条新路. 但Derouane等[11]使用的催化剂中含有离子型镓及分布在分子筛外表面和内孔道中的氧化镓等多种镓组分, 未详细讨论何种镓组分为活性物种, 而此类催化剂中活性物种的研究对于开发温和条件下进行丙烷功能化的高活性催化剂具有重要意义. 本文采用MAS NMR技术和13C标记的丙烷, 研究温和条件下(573 K)丙烷在含有不同类型镓物种的H-ZSM-5上的活化, 探索活化丙烷的镓物种.

  9. Projectile-breakup-induced fission-fragment angular distributions in the 6Li+232Th reaction

    Science.gov (United States)

    Pal, A.; Santra, S.; Chattopadhyay, D.; Kundu, A.; Ramachandran, K.; Tripathi, R.; Roy, B. J.; Nag, T. N.; Sawant, Y.; Sarkar, D.; Nayak, B. K.; Saxena, A.; Kailas, S.

    2017-08-01

    Background: Experimental anisotropy in fission-fragment (FF) angular distribution in reactions involving weakly bound stable projectiles with actinide targets are enhanced compared to statistical saddle-point model (SSPM) predictions. Contributions from breakup- or transfer-induced fission to total fission are cited as possible reasons for such enhancement. Purpose: To identify the breakup- or transfer-induced fission channels in 6Li+232Th reaction and to investigate their effects on FF angular anisotropy. Methods: The FF angular distributions have been measured exclusively at three beam energies (28, 32, and 36 MeV) around the Coulomb barrier in coincidence with projectile breakup fragments like α , d , and p using Si strip detectors. The angular anisotropy obtained for different exclusive breakup- or transfer-induced fission channels are compared with that for total fission. SSPM and pre-equilibrium fission models have been employed to obtain theoretical FF angular anisotropy. Results: Angular anisotropy of the fission fragments produced by different transfer- or breakup-induced fission reactions have been obtained separately in the rest frame of respective recoiling nuclei. Some of these anisotropies were found to be stronger than those of the inclusive fission. Overall angular distributions of transfer or breakup fission, integrated over all possible recoil angles with weight factor proportional to differential cross section of the complementary breakup fragment emitted in coincidence in all possible directions, were obtained. It was observed that the overall FF angular anisotropy for each of these fission channels is less than or equal to the anisotropy of total fission at all the measured energies. Assuming isotropic out-of-plane correlations between the fission fragments and light-charged particles, the overall breakup- or transfer-induced fission fragment angular distributions do not explain the observed enhancement in FF anisotropy of total fission. Pre

  10. 6LiF Semiconductor Sandwich Spectrometer for Fast Neutron Spectrum Measurement%用于快中子能谱测量的6LiF夹心半导体谱仪

    Institute of Scientific and Technical Information of China (English)

    蒋勇; 李俊杰; 张涛; 范晓强; 郑春

    2012-01-01

    A detector of 6LiF semiconductor sandwich spectrometer was designed and manufactured. Characteristics of the spectrometer were tested in the fast neutron critical assembly. Measurement principle, configuration of detector and electronic circuit were introduced. Fast neutron spectrum was measured using the 6LiF semiconductor sandwich spectrometer. When the detector's 6 LiF mass thickness is 186 μg/cm2, the spectrometer's energy resolution is 363 keV in the thermal neutron field. For this spectrometer, the optimal fathomable neutron energy range is 0. 3-7. 5 MeV, and the background counts only take possession of 1 % in this area.%本文介绍了6 LiF夹心谱仪的测量原理、自行设计研制的6LiF夹心半导体谱仪探头结构及电子学系统组成等.在热中子场中测试了夹心谱仪的性能,获得了α粒子峰、T粒子峰及“和”峰在多道上的位置与能量分辨率,并用T粒子与“和”峰两个能量点的峰位对谱仪系统进行了能量刻度.分别用效应探头和本底探头测量了临界装置表面的效应谱和本底谱,当效应探头采用的6 LiF镀层质量厚度为186 μg/cm2时,6 LiF夹心谱仪对热中子的能量分辨率为363 keY,测量中子最佳能区为0.3~7.5 MeV,在该能区内,本底谱约占1%.

  11. Development of a 6LiF/ZnS-based Neutron Multiplicity Counter

    Energy Technology Data Exchange (ETDEWEB)

    Stave, Sean C.; Behling, Richard S.; Bernacki, Bruce E.; Bliss, Mary; Cowles, Christian C.; Kouzes, Richard T.; Lintereur, Azaree; Robinson, Sean M.; Siciliano, Edward R.

    2016-10-06

    Abstract–Neutron multiplicity counters are used in safeguards to provide rapid assay of samples which contain an unknown amount of plutonium in a potentially unknown configuration. A project at PNNL is using regular and nickel-quenched 6LiF/ZnS neutron-scintillator sheets and wavelength shifting plastic for light pipes in place of 3He. A combination of laboratory and modeling work predicts a LiF/ZnS-based system to be able to match or exceed the performance of the best 3He-based systems available. Also, the Ni-quenched material is expected to allow for improved neutron/gamma-ray discrimination at twice the event rate relative to the non-Ni-quenched LiF/ZnS. A new system based on the LiF/ZnS material is under construction and components are being used to optimize the detection efficiency and neutron/gamma-ray discrimination properties. Components of the new system are partially constructed and undergoing performance testing utilizing high-speed digitizers with field programmable gate arrays to perform the neutron/gamma-ray discrimination. The expected performance of the full-scale system is expected to be nearly the same as for 3He-based systems and is due for completion in 2016.

  12. Systematics of the breakup probability function for {sup 6}Li and {sup 7}Li projectiles

    Energy Technology Data Exchange (ETDEWEB)

    Capurro, O.A., E-mail: capurro@tandar.cnea.gov.ar [Laboratorio TANDAR, Comisión Nacional de Energía Atómica, Av. General Paz 1499, B1650KNA San Martín, Buenos Aires (Argentina); Pacheco, A.J.; Arazi, A. [Laboratorio TANDAR, Comisión Nacional de Energía Atómica, Av. General Paz 1499, B1650KNA San Martín, Buenos Aires (Argentina); CONICET, Av. Rivadavia 1917, C1033AAJ Buenos Aires (Argentina); Carnelli, P.F.F. [CONICET, Av. Rivadavia 1917, C1033AAJ Buenos Aires (Argentina); Instituto de Investigación e Ingeniería Ambiental, Universidad Nacional de San Martín, 25 de Mayo y Francia, B1650BWA San Martín, Buenos Aires (Argentina); Fernández Niello, J.O. [Laboratorio TANDAR, Comisión Nacional de Energía Atómica, Av. General Paz 1499, B1650KNA San Martín, Buenos Aires (Argentina); CONICET, Av. Rivadavia 1917, C1033AAJ Buenos Aires (Argentina); Instituto de Investigación e Ingeniería Ambiental, Universidad Nacional de San Martín, 25 de Mayo y Francia, B1650BWA San Martín, Buenos Aires (Argentina); and others

    2016-01-15

    Experimental non-capture breakup cross sections can be used to determine the probability of projectile and ejectile fragmentation in nuclear reactions involving weakly bound nuclei. Recently, the probability of both type of dissociations has been analyzed in nuclear reactions involving {sup 9}Be projectiles onto various heavy targets at sub-barrier energies. In the present work we extend this kind of systematic analysis to the case of {sup 6}Li and {sup 7}Li projectiles with the purpose of investigating general features of projectile-like breakup probabilities for reactions induced by stable weakly bound nuclei. For that purpose we have obtained the probabilities of projectile and ejectile breakup for a large number of systems, starting from a compilation of the corresponding reported non-capture breakup cross sections. We parametrize the results in accordance with the previous studies for the case of beryllium projectiles, and we discuss their systematic behavior as a function of the projectile, the target mass and the reaction Q-value.

  13. A study of the proton spectra following the capture of $K^-$ in $^6$Li and $^{12}$C with FINUDA

    CERN Document Server

    Agnello, M; Benussi, L; Bertani, M; Bhang, H C; Bianco, S; Bonomi, G; Botta, E; Bregant, M; Bressani, Tullio; Bufalino, S; Busso, L; Calvo, D; Camerini, P; Cerello, P; Dalena, B; Mori, F D; D'Erasmo, G; Santo, D D; Elia, D; Fabbri, F L; Faso, D; Feliciello, A; Filippi, A; Filippini, V; Fini, R A; Fiore, E M; Fujioka, H; Gianotti, P; Grion, N; Hartmann, O; Krasnoperov, A V; Lenti, V; Lucherini, V; Manzari, V; Marcello, S; Maruta, T; Mirfakhraee, N; Morra, O; Nagae, T; Olin, A; Outa, H; Pace, E; Pallotta, M; Palomba, M; Pantaleo, A; Panzarasa, A; Paticchio, V; Piano, S; Pompili, F; Rui, R; Simonetti, G; Tereshchenko, V V; Tomassini, S; Toyoda, A; Wheadon, R; Zenoni, A

    2006-01-01

    Momenta spectra of protons emitted following the capture of $K^-$ in $^6$Li and $^{12}$C have been measured with 1% resolution. The $^{12}$C spectrum is smooth whereas for $^6$Li a well defined peak appears at about 500 MeV/$c$. The first observation of a structure in this region was identified as a strange tribaryon or, possibly, a $\\bar K$-nuclear state. The peak is correlated with a $\\pi^-$ coming from $\\Sigma^-$ decay in flight, selected by setting momenta larger than 275 MeV/$c$. The $\\Sigma^-$ could be produced, together with a 500 MeV/$c$ proton, by the capture of a $K^-$ in a deuteron-cluster substructure of the $^6$Li nucleus. The capture rate for such a reaction is $(1.62\\pm 0.23_{stat} ^{+0.71}_{-0.44}(sys))%/K^-_{stop}$, in agreement with the existing observations on $^4$He targets and with the hypothesis that the $^6$Li nucleus can be interpreted as a $(d+\\alpha)$ cluster.

  14. Towards {sup 6}Li-{sup 40}K ground state molecules

    Energy Technology Data Exchange (ETDEWEB)

    Brachmann, Johannes Felix Simon

    2013-02-08

    The production of a quantum gas with strong long - range dipolar interactions is a major scientific goal in the research field of ultracold gases. In their ro - vibrational ground state Li-K dimers possess a large permanent dipole moment, which could possibly be exploited for the realization of such a quantum gas. A production of these molecules can be achieved by the association of Li and K at a Feshbach resonance, followed by a coherent state transfer. In this thesis, detailed theoretical an experimental preparations to achieve state transfer by means of Stimulated Raman Adiabatic Passage (STIRAP) are described. The theoretical preparations focus on the selection of an electronically excited molecular state that is suitable for STIRAP transfer. In this context, molecular transition dipole moments for both transitions involved in STIRAP transfer are predicted for the first time. This is achieved by the calculation of Franck-Condon factors and a determination of the state in which the {sup 6}Li-{sup 40}K Feshbach molecules are produced. The calculations show that state transfer by use of a single STIRAP sequence is experimentally very well feasible. Further, the optical wavelengths that are needed to address the selected states are calculated. The high accuracy of the data will allow to carry out the molecular spectroscopy in a fast and efficient manner. Further, only a comparatively narrow wavelength tuneability of the spectroscopy lasers is needed. The most suitable Feshbach resonance for the production of {sup 6}Li-{sup 40}K molecules at experimentally manageable magnetic field strengths is occurring at 155 G. Experimentally, this resonance is investigated by means of cross-dimensional relaxation. The application of the technique at various magnetic field strengths in the vicinity of the 155 G Feshbach resonance allows a determination of the resonance position and width with so far unreached precision. This reveals the production of molecules on the atomic side

  15. Compounds of 6Li and natural Li for EPR dosimetry in photon/neutron mixed radiation fields.

    Science.gov (United States)

    Lund, E; Gustafsson, H; Danilczuk, M; Sastry, M D; Lund, A

    2004-05-01

    Formates and dithionates of 6Li, enriched and 7Li in natural composition of Li offer a possibility to measure the absorbed dose from photons and thermal neutrons in a mixed radiation field for instance at a boron neutron capture therapy (BNCT) facility. Tests with formates and dithionates of enriched 6Li and lithium compounds with natural composition have been performed at the BNCT facility at Studsvik, Sweden. Irradiations have been performed at 3 cm depth in a Perspex phantom in a fluence rate of thermal neutrons 1.8 x 10(9) n cm(-2) s(-1). The compounds were also irradiated in a pure X-ray field from a 4MV linear accelerator at 5 cm depth in a phantom with accurately determined absorbed doses. The signal intensity and shape was investigated within 3 h after the irradiation. A single line spectrum attributed to the CO2- radical was observed after irradiation of lithium formate. An increase in line width occurring after neutron irradiation in comparison with photon irradiation of the 6Li sample was attributed to dipolar broadening between CO2- radicals trapped in the tracks of the alpha particles. A spectrum due to the SO3- radical anion was observed after irradiation of lithium dithionate. The signal amplitude increased using the 6Li in place of the Li with natural composition of isotopes, in studies with low energy X-ray irradiation. Due to the decreased line width, caused by the difference in g(N) and I between the isotopes, the sensitivity with 6Li dithionate may be enhanced by an order of magnitude compared to alanine dosimetry. After comprehensive examination of the different combinations of compounds with different amounts of 6Li and 7Li regarding dosimetry, radiation chemistry and EPR properties these dosimeter material might be used for dose determinations at BNCT treatments and for biomedical experiments. Interesting properties of the radical formation might be visible due to the large difference in ionization density of neutrons compared to photons.

  16. The Trojan-Horse Method applied to the {sup 6}Li(p,{alpha}){sup 3}He reaction down to astrophysical energies

    Energy Technology Data Exchange (ETDEWEB)

    Tumino, A.; Spitaleri, C.; Pappalardo, L.; Cherubini, S.; Del Zoppo, A.; La Cognata, M.; Musumarra, A.; Pellegriti, M.G.; Pizzone, R.G.; Rinollo, A.; Romano, S.; Typel, S

    2004-04-05

    The Trojan-Horse Method has been applied to the three-body d({sup 6}Li,{alpha}{sup 3}He)n break-up reaction in order to extract the bare nucleus S(E) factor for the {sup 6}Li(p,{alpha}){sup 3}He down to astrophysical energies.

  17. Direct Observation of Lattice Aluminum Environments in Li Ion Cathodes LiNi 1–yz Co y Al z O 2 and Al-Doped LiNi x Mn y Co z O 2 via 27 Al MAS NMR Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Dogan, Fulya; Vaughey, John T.; Iddir, Hakim; Key, Baris

    2016-07-06

    Direct observations of local lattice aluminum environments have been a major challenge for aluminum -bearing Li ion battery materials, such as LiNi1-y-zCoyAlzO2 Al(NCA) and aluminum-doped LiNixMnyCozO2 (NMC). Al-27 magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy is the only structural probe currently available that can qualitatively and quantitatively characterize lattice and nonlattice (i.e., surface, coatings, segregation, secondary phase etc.) aluminum coordination and provide information that helps discern its effect in the lattice. In the present study, we use NMR to gain new insights into transition metal (TM)-O-Al coordination and evolution of lattice aluminum sites upon cycling. With the aid of first-principles DFT calculations, we show direct evidence of lattice Al sites, nonpreferential Ni/Co-O-Al ordering in NCA, and the lack of bulk lattice aluminum in aluminum -"doped" NMC. Aluminum coordination of the paramagnetic (lattice) and diamagnetic (nonlattice) nature is investigated for Al-doped NMC and NCA. For the latter, the evolution of the lattice site(s) upon cycling is also studied. A clear reordering of lattice aluminum environments due to nickel migration is observed in NCA upon extended cycling.

  18. Theory of laser enhancement and suppression of cold reactions: the fermion-boson 6Li+7Li2(variant Planck's over 2pi omega0) 6Li7Li+7Li radiative collision.

    Science.gov (United States)

    Li, Xuan; Parker, Gregory A; Brumer, Paul; Thanopulos, Ioannis; Shapiro, Moshe

    2008-03-28

    We present a nonperturbative time-dependent quantum mechanical theory of the laser catalysis and control of a bifurcating A+BC(variant Planck's over 2pi omega(0))ABC*(v)(variant Planck's over 2pi omega(0) )AB+C reaction, with ABC*(v) denoting an intermediate, electronically excited, complex of ABC in the vth vibrational state. We apply this theory to the low collision energy fermion-boson light-induced exchange reaction, (6)Li((2)S)+(7)Li(2)((3)Sigma(u)(+))(variant Planck's over 2pi omega(0))((6)Li(7)Li(7)Li)*(variant Planck's over 2pi omega(0))(6)Li(7)Li((3)Sigma(+))+(7)Li((2)S). We show that at very low collision energies and energetically narrow (approximately 0.01 cm(-1)) initial reactant wave packets, it is possible to tune the yield of the exchange reaction from 0 to near-unity (yield >or=99%) values. Controllability is somewhat reduced at collisions involving energetically wider (approximately 1 cm(-1)) initial reactant wave packets. At these energetic bandwidths, the radiative reactive control, although still impressive, is limited to the 0%-76% reactive-probabilities range.

  19. Multinuclear NMR Study of the Solid Electrolyte Interface Formed in Lithium Metal Batteries

    Energy Technology Data Exchange (ETDEWEB)

    Wan, Chuan; Xu, Suochang; Hu, Mary Y.; Cao, Ruiguo; Qian, Jiangfeng; Qin, Zhaohai; Liu, Jun; Mueller, Karl T.; Zhang, Ji-Guang; Hu, Jian Zhi

    2017-04-18

    The composition of the solid electrolyte interphase (SEI) layers associated with a high performance Cu|Li cell using lithium bis(fluorosulfonyi)imide (LiFSI) in 1,2-dimethoxyethane (DME) as electrolyte is determined by a multinuclear (6Li, 19F, 13C and 1H) solid-state MAS NMR study at high magnetic field (850 MHz). This cell can be cycled at high rates (4 mA•cm-2) for more than 1000 cycles with no increase in the cell impedance at high Columbic efficiency (average of 98.4%) in a highly concentrated LiFSI-DME electrolyte (4 M). LiFSI, LiF, Li2O2 (and/or CH3OLi), LiOH, Li2S and Li2O are observed in the SEI and validated by comparing with the spectra acquired on standard compounds and literature reports. To gain further insight into the role of the solute and its concentration dependence on the formation of SEIs while keeping the solvent of DME unchanged, the SEIs from different concentrations of LiFSI-DME and lithium bis(trifluoromethanesulfonyl)imide (LiTFSI)-DME electrolyte are also investigated. It is found that LiF, a lithiated compound with superior mechanical strength and good Li+ ionic conductivity, is observed in the concentrated 4.0 M LiFSI-DME and the 3.0 M LiTFSI-DME systems but not in the diluted 1.0 M LiFSI-DME system. Li2O exists in both low and high concentration of LiFSI-DME while no Li2O is observed in the LiTFSI system. Furthermore, the dead metallic Li is reduced in the 4 M LiFSI-DME system compared with that in the 1 M LiFSI-DME system. Quantitative 6Li MAS results indicate that the SEI associated with the 4 M LiFSI-DEME is denser or thicker than that of the 1 M LiFSI-DME and the 3 M LiTFSI-DME systems. These findings are likely the reasons for explaining the high electrochemical performance associated with the high concentration LiFSI-DME system.

  20. High Tech M&As

    DEFF Research Database (Denmark)

    Toppenberg, Gustav

    2013-01-01

    of findings are not applicable to the high-tech industry; in fact this industry has many additional challenges. In this study, we aim to explore the process of M&A in the high-tech industry by drawing on extant literature and empirical field work. The paper outlines a research project in progress which...... intends to provide theoretical, empirical and practical contributions in answering the research question: what role does Operations and IT play in creating value in high-tech M&As? The research adds a needed perspective on M&A literature by unveiling unique challenges and opportunities faced by the M...

  1. Projectile breakup dynamics for {sup 6}Li+{sup 59}Co: Kinematical analysis of {alpha}-d coincidences

    Energy Technology Data Exchange (ETDEWEB)

    Souza, F.A.; Carlin, N.; Liguori Neto, R.; Siqueira-Mello, C.; Moura, M.M. de; Munhoz, M.G.; Oliveira, R.A.N.; Santo, M.G. del; Suaide, A.A.P.; Szanto, E.M.; Szanto de Toledo, A. [Instituto de Fisica - Universidade de Sao Paulo, Departamento de Fisica Nuclear, Sao Paulo, SP (Brazil); Beck, C. [CNRS-IN2P3 and Universite Louis Pasteur, Institut Pluridisciplinaire Hubert Curien, UMR 7178, Strasbourg (France); Keeley, N. [The Andrzej Soltan Institute for Nuclear Studies, Department of Nuclear Reactions, Warsaw (Poland); Diaz-Torres, A. [University of Surrey, Department of Physics, Faculty of Engineering and Physical Sciences, Guildford (United Kingdom)

    2010-05-15

    A study of the kinematics of the {alpha} -d coincidences in the {sup 6}Li+{sup 59}Co system at a bombarding energy of E{sub lab}=29.6 MeV is presented. With exclusive measurements performed over different angular intervals it is possible to identify the respective contributions of the sequential and direct projectile breakup components. The angular distributions of both breakup components are fairly well described by the Continuum-Discretized Coupled-Channels framework (CDCC). Furthermore, a careful analysis of these processes using a semiclassical approach provides information on both their lifetime and their distance of occurrence with respect to the target. Breakup to the low-lying (near-threshold) continuum is delayed, and happens at large internuclear distances. This suggests that the influence of the projectile breakup on the complete fusion process can be related essentially to the direct breakup to the {sup 6}Li high-lying continuum spectrum. (orig.)

  2. Comparison of Thermal Neutron Detection Efficiency of $^{6}$Li Scintillation Glass and $^{3}$He Gas Proportional Tube

    CERN Document Server

    Xu, Ming; Chen, Guo-Ming; Tao, Jun-Quan

    2013-01-01

    We report on a comparison study of the $^{3}$He gas proportional tube and the $^{6}$Li incorporated scintillation glasses on thermal neutron detection efficiency. Both $^{3}$He and $^{6}$Li are used commonly for thermal neutron detection because of their high neutron capture absorption coefficient. By using a neutron source $^{252}$Cf and a paraffin moderator in an alignment system, we can get a small beam of thermal neutrons. A flash ADC is used to measure the thermal neutron spectrum of each detector, and the detected number of events is determined from the spectrum, then we can calculate the detection efficiency of different detectors. Meanwhile, the experiment have been modeled with GEANT4 to validate the results against the Monte Carlo simulation.

  3. Astrophysical S-factor for $^6$Li$(p,\\gamma)$$^7$Be in the coupled-channel Gamow shell model

    CERN Document Server

    Dong, G X; Michel, N; Płoszajczak, M

    2015-01-01

    We have applied the Gamow shell model (GSM) in the coupled-channel representation to study the astrophysical $S$-factor for the proton radiative capture reaction of $^6$Li. Reaction channels are built by coupling the proton wave function expanded in different partial waves with the GSM wave functions of the ground state ($1^+$) and the excited states ($3^+_1$, $0^+_1$ and $2^+_1$) of $^6$Li. All relevant $E1$, $M1$, and $E2$ transitions from the initial continuum states in $^7$Be to the final bound states (${3/2}^-_1$ and ${1/2}^-_1$) states are included. It is found that the calculated total astrophysical $S$ factor for this reaction agrees well with the experimental data.

  4. Integration of a $^6$LiInSe$_2$ Thermal Neutron Detector into a CubeSat Instrument

    CERN Document Server

    Egner, Joanna C; Burger, Arnold; Stassun, Keivan G; Buliga, Vladimir; Matei, Liviu; Bodnarik, Julia G; Stowe, Ashley C; Prettyman, Thomas H

    2016-01-01

    We present a preliminary design for a novel neutron detection system that is compact, lightweight, and low power consuming, utilizing the CubeSat platform making it suitable for space-based applications. This is made possible using the scintillating crystal lithium indium diselenide ($^6$LiInSe$_2$), the first crystal to include $^6$Li in the crystalline structure, and a silicon avalanche photodiode (Si-APD). The schematics of this instrument are presented as well as the response of the instrument to initial testing under alpha radiation. A principal aim of this work is to demonstrate the feasibility of such a neutron detection system within a CubeSat platform. The entire end-to-end system presented here is 10 cm x 10 cm x 15 cm, weighs 670 grams and requires 5 Volts direct current at 3 Watts.

  5. Study of the {sup 9}Be(p,{alpha}){sup 6}Li reaction via the Trojan Horse Method

    Energy Technology Data Exchange (ETDEWEB)

    Romano, S.; Lamia, L.; Spitaleri, C.; Cherubini, S.; Gulino, M.; La Cognata, M.; Tumino, A. [INFN, Laboratori Nazionali del Sud, Catania (Italy); Universita di Catania, Dipartimento di Metodologie Fisiche e Chimiche per l' Ingegneria, Catania (Italy); Li, C.; Pizzone, R.G. [INFN, Laboratori Nazionali del Sud, Catania (Italy)

    2006-03-15

    The Trojan Horse Method has been applied to the {sup 2}H({sup 9}Be,{sup 6}Li{alpha})n three-body reaction in order to investigate the {sup 9}Be(p,{alpha}){sup 6}Li two-body reaction, which is involved in the study of light element abundances (lithium, beryllium and boron). A coincidence measurement was performed in order to identify the presence of the quasi-free mechanism in the three-body reaction, needed for the application of the method. The astrophysical S(E)-factor was extracted and compared to direct data. No information about electron screening effects can be extracted due to the poor resolution of the indirect data. (orig.)

  6. Formation of η{sup '} (958) meson bound states by the {sup 6}Li(γ,d) reaction

    Energy Technology Data Exchange (ETDEWEB)

    Miyatani, M.; Nagahiro, H.; Hirenzaki, S. [Nara Women' s University, Department of Physics, Nara (Japan); Ikeno, N. [Tottori University, Department of Regional Environment, Tottori (Japan)

    2016-07-15

    We have investigated the {sup 6}Li(γ,d) reaction theoretically for the formation of the η{sup '}(958) mesic nucleus close to the recoilless kinematics. We have developed the theoretical formula and reported the quantitative results of the formation spectra for various cases in this article. We have found that the formation cross sections are reduced by the effects of the fragile deuteron form factor. (orig.)

  7. Theoretical study of the α +d →6Li +γ astrophysical capture process in a three-body model

    Science.gov (United States)

    Tursunov, E. M.; Kadyrov, A. S.; Turakulov, S. A.; Bray, I.

    2016-07-01

    The astrophysical capture process α +d →6Li is studied in a three-body model. The initial state is factorized into the deuteron bound state and the (α +d )-scattering state. The final nucleus 6Li (1+) is described as a three-body bound state α +n +p in the hyperspherical Lagrange-mesh method. The contribution of the E 1 -transition operator from the initial isosinglet states to the isotriplet components of the final state is estimated to be negligible. An estimation of the forbidden E 1 transition to the isosinglet components of the final state is comparable with the corresponding results of the two-body model. However, the contribution of the E 2 -transition operator is found to be much smaller than the corresponding estimations of the two-body model. The three-body model perfectly matches the new experimental data of the LUNA Collaboration with the spectroscopic factor of 2.586 estimated from the bound-state wave functions of 6Li and a deuteron.

  8. Unified description of $^6$Li structure and deuterium-$^4$He dynamics with chiral two- and three-nucleon forces

    CERN Document Server

    Hupin, Guillaume; Navrátil, Petr

    2014-01-01

    Prototype for the study of weakly bound projectiles colliding on stable targets, the scattering of deuterium ($d$) on $^4$He ($\\alpha$) is an important milestone in the search for a fundamental understanding of low-energy reactions. At the same time, it is also important for its role in the Big-bang nucleosynthesis of $^6$Li and applications in the characterization of deuterium impurities in materials. We present the first unified {\\em ab initio} study of the $^6$Li ground state and $d$-$^4$He elastic scattering using two- and three-nucleon forces derived within the framework of chiral effective field theory. The six-nucleon bound-state and scattering observables are calculated by means of the no-core shell model with continuum. %and are compared to available experimental data. We analyze the influence of the dynamic polarization of the deuterium and of the chiral three-nucleon force, and examine the role of the continuum degrees of freedom in shaping the low-lying spectrum of $^6$Li. We find that the adopted...

  9. First direct measurement of the 2H(α,γ)6Li cross section at big bang energies and the primordial lithium problem.

    Science.gov (United States)

    Anders, M; Trezzi, D; Menegazzo, R; Aliotta, M; Bellini, A; Bemmerer, D; Broggini, C; Caciolli, A; Corvisiero, P; Costantini, H; Davinson, T; Elekes, Z; Erhard, M; Formicola, A; Fülöp, Zs; Gervino, G; Guglielmetti, A; Gustavino, C; Gyürky, Gy; Junker, M; Lemut, A; Marta, M; Mazzocchi, C; Prati, P; Rossi Alvarez, C; Scott, D A; Somorjai, E; Straniero, O; Szücs, T

    2014-07-25

    Recent observations of (6)Li in metal poor stars suggest a large production of this isotope during big bang nucleosynthesis (BBN). In standard BBN calculations, the (2)H(α,γ)(6)Li reaction dominates (6)Li production. This reaction has never been measured inside the BBN energy region because its cross section drops exponentially at low energy and because the electric dipole transition is strongly suppressed for the isoscalar particles (2)H and α at energies below the Coulomb barrier. Indirect measurements using the Coulomb dissociation of (6)Li only give upper limits owing to the dominance of nuclear breakup processes. Here, we report on the results of the first measurement of the (2)H(α,γ)(6)Li cross section at big bang energies. The experiment was performed deep underground at the LUNA 400 kV accelerator in Gran Sasso, Italy. The primordial (6)Li/(7)Li isotopic abundance ratio has been determined to be (1.5 ± 0.3) × 10(-5), from our experimental data and standard BBN theory. The much higher (6)Li/(7)Li values reported for halo stars will likely require a nonstandard physics explanation, as discussed in the literature.

  10. Moderate MAS enhances local (1)H spin exchange and spin diffusion.

    Science.gov (United States)

    Roos, Matthias; Micke, Peter; Saalwächter, Kay; Hempel, Günter

    2015-11-01

    Proton NMR spin-diffusion experiments are often combined with magic-angle spinning (MAS) to achieve higher spectral resolution of solid samples. Here we show that local proton spin diffusion can indeed become faster at low (MAS (Clauss et al., 1993). The enhancement of spin diffusion by slow MAS relies on the modulation of the orientation-dependent dipolar couplings during sample rotation and goes along with transient level crossings in combination with dipolar truncation. The experimental finding and its explanation is supported by density matrix simulations, and also emphasizes the sensitivity of spin diffusion to the local coupling topology. The amplification of spin diffusion by slow MAS cannot be explained by any model based on independent spin pairs; at least three spins have to be considered. Copyright © 2015 Elsevier Inc. All rights reserved.

  11. Sol-gel chemistry synthesis and DTA-TGA, XRPD, SIC and {sup 7}Li, {sup 31}P, {sup 29}Si MAS-NMR studies on the Li-NASICON Li{sub 3}Zr{sub 2-y}Si{sub 2-4y}P{sub 1+4y}O{sub 12} (0 Less-Than-Or-Slanted-Equal-To y Less-Than-Or-Slanted-Equal-To 0.5) system

    Energy Technology Data Exchange (ETDEWEB)

    Belam, W., E-mail: WahidBelam@yahoo.fr [Chemistry Department, Bizerta Science Faculty, 7021 Jarzouna, Bizerta (Tunisia)

    2013-02-25

    Highlights: Black-Right-Pointing-Pointer The samples of Li-NASICON were elaborated by sol-gel chemistry. Black-Right-Pointing-Pointer The calcined temperatures of the studied samples were deduced from their thermograms. Black-Right-Pointing-Pointer The recorded X-ray powder diffractograms were indexed in the rhombohedral system. Black-Right-Pointing-Pointer The synthesized Li-NASICON materials are excellent lithium fast cation conductors. - Abstract: Five selected compounds of Li-NASICON, Li{sub 3}Zr{sub 2-y}Si{sub 2-4y}P{sub 1+4y}O{sub 12} (0 Less-Than-Or-Slanted-Equal-To y Less-Than-Or-Slanted-Equal-To 0.5), were synthesized by sol-gel chemistry in order to obtain pure polycrystalline powder and then analyzed by different physicochemical characterizations such as coupled DTA (differential thermal analysis)-TGA (thermogravimetric analysis), XRPD (X-ray powder diffraction), CIS (complex impedance spectroscopy) and MAS (magic angle spinning)-NMR (nuclear magnetic resonance). So the calcined temperature of each sample has been deduced from its corresponding DTA-TGA thermogram. However, the recorded X-ray powder diffractograms were indexed in the rhombohedral system with R3{sup Macron }c space group which corresponds to the ideal structure of NASICON. Whereas, the complex impedance spectroscopy study showed that these Li-NASICON materials are excellent lithium fast cation conductors with total electric conductivity maximal value 1.97 Multiplication-Sign 10{sup -3} S cm{sup -1} at 293 K in the case of Li{sub 3}Zr{sub 1.5}P{sub 3}O{sub 12}. Furthermore, {sup 7}Li, {sup 31}P and {sup 29}Si MAS-NMR spectroscopy study and DFT/B3LYP theoretical calculations of chemical shifts were performed to discuss the ambiguousness that exists between the resonance peak number in the experimental spectrum and the crystallographic site number relative to Li{sub 3}Zr{sub 2}Si{sub 2}PO{sub 12}.

  12. Measuring the ratio of aqueous diffusion coefficients between 6Li +Cl - and 7Li +Cr - by osmometry

    Science.gov (United States)

    Fritz, Steven J.

    1992-10-01

    Osmotic equilibrium is a singular occurrence in the evolution of an osmotic cell because at this event the net solution flux is zero such that -J w · V¯w = J s · V¯s. At this juncture, the diffusion coefficient of the solute through the membrane (ω) equals the solute flux ( Js) divided by the osmotic pressure (ΔΠ). Because the solute permeability coefficient (ω) is related to the Fickian diffusion coefficient ( D) through the gas constant, temperature, and the membrane's thickness and tortuosity, the ratio of ω values for individual isotopic species equals the ratio of D values for the same isotopic components. A 0.9450 molal LiCl solution was placed within sealed dialysis tubing and osmoted against a kilogram of deionized water at 22°C. Osmotic equilibrium occurred at 164 ± 10 min. The ratio of ω6Li +Cl -/ω7Li +Cl - was measured to be 1.011 ± 0.003 - a value close to the square root of the mass ratio between 7LiCl and 6LiCl (= 1.012) as calculated by Graham's Law. The measured diffusion coefficient ratio was used to predict the degree of hyperfiltration-induced fractionation of Li isotopes as a function of membrane ideality. When a membrane's σ exceeds 0.95 (as is likely for low-porosity shales) the 6Li /7Li ratio on the high-pressure side of the membrane can theoretically vary by more than 0.0017.

  13. Probing the role of Skyrme interactions on the fission dynamics of the 6Li + 238U reaction

    Science.gov (United States)

    Sharma, Ishita; Kumar, Raj; Sharma, Manoj K.

    2017-06-01

    The performance of selected five Skyrme forces (out of a set of 240), tested by Dutra et al., is analyzed in view of fusion-fission dynamics. These forces are assumed to perform better for neutron-rich systems, so the choice of the reaction is accordingly made by opting for a neutron-rich target in 6Li + 238U reaction. This reaction is diagnosed further in reference to fusion hindrance within the dynamical approach of the cluster-decay model (DCM). In order to reduce the computational time, three Skyrme forces are figured out with the criteria that these forces cover the barrier characteristics of the remaining two forces as well. The fission cross-sections are successfully addressed at low energies for the 6Li + 238U reaction. However, at relatively higher energies, the excitation functions show theoretical suppression with respect to experimental data, which may be associated with the possible existence of incomplete fusion (ICF). For ICF, we have considered that the 6Li broke into 4He + 2H, as mentioned in the experimental work. The calculations of ICF are carried out for the 4He + 238U reaction with the selected Skyrme forces at E_{c.m.} = 26.20 and 27.51 MeV. These forces address the data nicely for the compound nucleus (CN) as well as ICF processes. Here, the NRAPR force seems to require lesser barrier modification as compared to the other forces, therefore it can be used as an alternate choice for calculating the interaction potential. Additionally, the prediction of cross-sections at lower energies has been done with DCM using the NRAPR force. The ℓ-dependent % barrier modification of the Skyrme forces undertaken is also worked out in reference to fusion hindrance at below barrier energies.

  14. Role of neutron transfer processes on the 6Li+120Sn and 7Li+119Sn fusion reactions

    Directory of Open Access Journals (Sweden)

    Fisichella M.

    2015-01-01

    Full Text Available The results concerning the study of 6Li+120Sn and 7Li+119Sn systems are presented. These two sistems are characterised by very similar structures of the interacting nuclei and by different Q-value for one-and two- neutron transfer. Our aim is to disentangle the possible effects due to the different n-transfer Q-values, at sub-barriers energies, by comparing the two fusion excitation function. In these experiments the fusion cross section has been measured by using a stack activation technique. No particular differences in the two fusion excitation functions have been observed.

  15. Study of Two-Step Mechanisms in Pion Absorption on $^{6}Li$, $^{12}C$ via Deuteron Emission

    CERN Document Server

    Huber, G M; Papandreou, Z; Hovdebo, J; Naqvi, S I H; Ottewell, D F; Walden, P L; Jones, G; Aslanoglou, X

    2000-01-01

    The (pi+,pd), and (pi+,dd) reactions were investigated with pions of 100 and 165 MeV kinetic energy on 6Li and 12C targets. In comparison with previously published (pi+,pp) data on the same targets and at the same beam energies, kinematic regions were identified in which the neutron pickup process n+p->d dominated the observed deuteron yield. The importance of this mechanism increases with energy, contributing half of the observed cross section at 165 MeV. The contribution of direct quasi-triton absorption is significant only at 100 MeV.

  16. {sup 16}O resonances near 4α threshold through {sup 12}C({sup 6}Li,d) reaction

    Energy Technology Data Exchange (ETDEWEB)

    Rodrigues, M. R. D.; Borello-Lewin, T.; Miyake, H.; Horodynski-Matsushigue, L. B.; Duarte, J. L. M.; Rodrigues, C. L.; Faria, P. Neto de [Instituto de Física, Universidade de São Paulo, Caixa Postal 66318, CEP 05314-970, São Paulo, SP (Brazil); Cunsolo, A.; Cappuzzello, F.; Foti, A.; Agodi, C.; Cavallaro, M. [INFN - Laboratori Nazionali del Sud, Via S. Sofia 62, 95125 Catania (Italy); Napoli, M. di; Ukita, G. M. [Faculdade de Psicologia, Universidade de Santo Amaro, R. Prof. Eneas da Siqueira Neto, 340, CEP 04829-300, São Paulo, SP (Brazil)

    2014-11-11

    Several narrow alpha resonant {sup 16}O states were detected through the {sup 12}C({sup 6}Li,d) reaction, in the range of 13.5 to 17.5 MeV of excitation energy. The reaction was measured at a bombarding energy of 25.5 MeV employing the São Paulo Pelletron-Enge-Spectrograph facility and the nuclear emulsion technique. Experimental angular distributions associated with natural parity quasi-bound states around the 4α threshold are presented and compared to DWBA predictions. The upper limit for the resonance widths obtained is near the energy resolution (15 keV)

  17. (p,px) reaction on /sup 6/Li and /sup 7/Li nuclei at incident proton energy of 70 MeV

    Energy Technology Data Exchange (ETDEWEB)

    Gorpinich, O.K.; Kadkin, E.P.; Kondrat' ev, S.N.; Lobach, Yu.M.; Pasechnik, M.V.; Saltykov, L.S.; Tokarevskij, V.V. (AN Ukrainskoj SSR, Kiev. Inst. Yadernykh Issledovanij)

    1983-01-01

    Measurements of two-dimensional coincidence spectra of charged particles from the /sup 6/Li(p, 2p)/sup 5/He, /sup 6/Li(p, p..cap alpha..)/sup 2/H, /sup 7/Li(p, pt)/sup 4/He, /sup 7/Li(p, p..cap alpha..)/sup 3/H reactions has been carried out using the equipment for simultaneous investigation of correlation of charged particles of different types. The /sup 6/Li(p, pd) reaction probability reaches the maximum value when the residual nucleus momentum is close to zero. This fact may confirm an existance of strong /sup 6/Li ..cap alpha..d-clusterization. The /sup 7/Li(p, pt) reaction occurs with the minimum probability in a quasi-free region that confirms /sup 7/Li ..cap alpha..t-structure. A direct comparison of particle two-dimensional spectra projections of (p, px) type reactions reveals that a probability of quasi-free scattering of proton on deuteron (triton) /sup 6/Li(/sup 7/Li) cluster is higher than quasi-free scattering on intranuclear protons. This fact is also confirmed by an assumption on ..cap alpha..d(..cap alpha..t)-cluster /sup 6/Li(/sup 7/Li) nucleus structure.

  18. Analysis of the normal optical, Michel and molecular potentials on the $^{40}$Ca($^6$Li, d)$^{44}$ Ti reaction

    Indian Academy of Sciences (India)

    MAZUMDER UTTAM K; SOMADDER ANOCK; HOQUE ENAMUL; HAQUE YASMEEN; DAS SUSANTA K; SEN GUPTA H M

    2016-06-01

    Full finite-range (FFR) distorted-wave Born approximation (DWBA) method has been applied to analyse the angular distributions of cross-sections of the $^{40}$Ca($^{6}$Li, d)$^{44}$Ti reaction at 28 MeV incident energy for the 22 transitions involving both the bound and unbound states of $^{44}$Ti byusing the normal optical, Michel and molecular potentials. The extracted spectroscopic factors for the three optical potentials are compared with those of some previous studies of zero-range (ZR) calculations of the$^{40}$Ca($^{6}$Li, d)$^{44}$Ti reaction using the normal optical potential. The $\\chi^{2}$ values of all the levels are obtained for the three optical potentials to estimate the quality of the fits. Molecular and Michel potentials have been used for the first time to analyse the four-nucleon transfer reaction and it seems that the molecular potential fits the experimental data more satisfactorily for some of the states than the normal optical and Michel potentials.

  19. Low energy R-matrix fits for the 6Li(d,a)4He S factor

    CERN Document Server

    Grineviciute, J; Lamia, L; Spitaleri, C; La Cognata, M

    2014-01-01

    Background: The information about the 6Li(d,a)4He reaction rates of the astrophysical interest can be obtained by extrapolating direct data to the lower energies, or by indirect methods. The indirect Trojan Horse method, as well as various R-matrix and polynomial fits to direct data, estimate the electron screening energies much larger than the adiabatic limit. Calculations that include the subthreshold resonance estimate smaller screening energies. Purpose: Obtain the 6Li(d,a)4He reaction R-matrix parameters and the astrophysical S factor for the energies relevant to the stellar plasmas by fitting the R-matrix formulas for the subthreshold resonances to the S factor data above 60 keV. Methods: The bare S factor is calculated using the single and the two-level R-matrix formulas for the closest to the threshold 0+ and 2+ subthreshold states at 22.2, 20.2 and 20.1 MeV. The electron screening potential Ue is then obtained by fitting it as a single parameter to the low energy data. Results: The low energy S facto...

  20. Theoretical study of the $\\alpha+d$ $\\rightarrow$ $^6$Li + $\\gamma $ astrophysical capture process in a three-body model

    CERN Document Server

    Tursunov, E M; Turakulov, S A; Bray, I

    2016-01-01

    The astrophysical capture process $\\alpha+d$ $\\rightarrow$ $^6$Li + $\\gamma$ is studied in a three-body model. The initial state is factorized into the deuteron bound state and the $\\alpha+d$ scattering state. The final nucleus $^6$Li(1+) is described as a three-body bound state $\\alpha+n+p$ in the hyperspherical Lagrange-mesh method. The contribution of the E1 transition operator from the initial isosinglet states to the isotriplet components of the final state is estimated to be negligible. An estimation of the forbidden E1 transition to the isosinglet components of the final state is comparable with the corresponding results of the two-body model. However, the contribution of the E2 transition operator is found to be much smaller than the corresponding estimations of the two-body model. The three-body model perfectly matches the new experimental data of the LUNA collaboration with the help of the spectroscopic factor 2.586, very consistent with the three-body structure of the final state.

  1. Resonance and non-resonance effect of continuum states of 6Li on elastic scattering angular distributions

    Science.gov (United States)

    Gómez Camacho, A.

    2016-07-01

    CDCC calculations of elastic scattering angular distributions for reactions of the weakly bound projectile 6Li with targets 28Si and 58Ni at energies around the Coulomb barrier are presented. Special emphasis is given to account for the effect of couplings from 6Li resonance states l = 2, J π = 3+, 2+, 1+. Similarly, the effect produced by non-resonant state couplings is studied. The convergent calculations are carried out with global α-target and d-target interactions. The calculated elastic scattering angular distributions are in general in good agreement with the measurements for the systems considered in this work. It is found that the calculations with only resonance states are very similar to that with all couplings (resonance+non-resonance). So, the absence of these states have a strong effect on elastic scattering (non-resonance states calculation). It is shown that the effects increase as the collision energy increases. An interpretation of the strength of the different effects is given in terms of the polarization potentials that emerge from the different couplings.

  2. Prospective conceptual qualification of hybrid centrifugation/distillatory for {sup 6}LI nuclear fusion technology scaled supply demands; Calificacion conceptual prospectiva de centrifugador/destilador hibrido para produccion de {sup 6}Li a demanda de la tecnologia Nuclear Fusion

    Energy Technology Data Exchange (ETDEWEB)

    Sedano, L.; Herranz, J. L.; Casado, J. L.; Castro, P.; Xiberta, J.

    2013-07-01

    The change in the demand for exploitation of lithium as a resource appears during the last decade, related to the development of the ion-Li batteries market and with the requirements of Nuclear Fusion fuels (deuterium and lithium) as coming energy option. A prospective analysis of synergistic demands of both markets, in its technical and in its economic aspects appears of prospective interest. The civil market {sup 6}Li/{sup 7}Li enrichment demand is analyzed. Specific technological developments permitting on-line production according to demand is discussed. A [centrifugation /thermal diffusion / combined distillation] technique is selected and qualified as technologically viable option for scaled production of litiated-forms. A conceptual design of a production plant is finally proposed according to the new technical capability.

  3. Fluid flow dynamics in MAS systems.

    Science.gov (United States)

    Wilhelm, Dirk; Purea, Armin; Engelke, Frank

    2015-08-01

    The turbine system and the radial bearing of a high performance magic angle spinning (MAS) probe with 1.3mm-rotor diameter has been analyzed for spinning rates up to 67kHz. We focused mainly on the fluid flow properties of the MAS system. Therefore, computational fluid dynamics (CFD) simulations and fluid measurements of the turbine and the radial bearings have been performed. CFD simulation and measurement results of the 1.3mm-MAS rotor system show relatively low efficiency (about 25%) compared to standard turbo machines outside the realm of MAS. However, in particular, MAS turbines are mainly optimized for speed and stability instead of efficiency. We have compared MAS systems for rotor diameter of 1.3-7mm converted to dimensionless values with classical turbomachinery systems showing that the operation parameters (rotor diameter, inlet mass flow, spinning rate) are in the favorable range. This dimensionless analysis also supports radial turbines for low speed MAS probes and diagonal turbines for high speed MAS probes. Consequently, a change from Pelton type MAS turbines to diagonal turbines might be worth considering for high speed applications. CFD simulations of the radial bearings have been compared with basic theoretical values proposing considerably smaller frictional loss values. The discrepancies might be due to the simple linear flow profile employed for the theoretical model. Frictional losses generated inside the radial bearings result in undesired heat-up of the rotor. The rotor surface temperature distribution computed by CFD simulations show a large temperature gradient over the rotor.

  4. 同位素7Li和6Li的性质殊异%The diverse of isotopes 7 Li and 6 Li

    Institute of Scientific and Technical Information of China (English)

    朱正和; 宋江锋; 罗德礼

    2014-01-01

    本文研究了同位素7 Li和6 Li在几个方面的性质差异.用相对论量子力学计算指出,6 Li的电子能级比7 Li的能级低,同时,对电偶极E (1)和磁偶极M (1)的能级跃迁波长,6 Li的跃迁波长都要比7 Li的长.由于7 Li和6 Li的核自旋的大小不同,可以看出在磁场2万高斯和温度100-20 K之间,7 Li的磁极化比6 Li的约大13倍.7 Li和6 Li的磁极化这种差异,也是一种可能的同位素7 Li/6 Li的分离方法.%The diverse of isotopes 7 Li and 6 Li was examined on the several respects.The calculations of relativistic quantum mechanics shows that the energy levels of 6 Li are lower than that of 7 Li, and therefore the transitional wave length of E(1) and M(1) for 6 Li are longer than that of 7 Li.The variation of couple constant due to the different nu-clear spin of 7 Li and 6 Li could be as a basis for the isotope separation between 7 Li and 6 Li.Ratio of the molar intensi-ty of magnetization of 7 Li to 6 Li is about 13 under 100-20 K and 20, 000 gauss, which is favorable to separate out 6 Li.

  5. Nuclear structure with accurate chiral perturbation theory nucleon-nucleon potential: Application to 6Li and 10B

    Energy Technology Data Exchange (ETDEWEB)

    Navratil, P; Caurier, E

    2003-10-14

    The authors calculate properties of A = 6 system using the accurate charge-dependent nucleon-nucleon (NN) potential at fourth order of chiral perturbation theory. By application of the ab initio no-core shell model (NCSM) and a variational calculation in the harmonic oscillator basis with basis size up to 16 {h_bar}{Omega} they obtain the {sup 6}Li binding energy of 28.5(5) MeV and a converged excitation spectrum. Also, they calculate properties of {sup 10}B using the same NN potential in a basis space of up to 8 {h_bar}{Omega}. The results are consistent with results obtained by standard accurate NN potentials and demonstrate a deficiency of Hamiltonians consisting of only two-body terms. At this order of chiral perturbation theory three-body terms appear. It is expected that inclusion of such terms in the Hamiltonian will improve agreement with experiment.

  6. Effect of compound nuclear reaction mechanism in 12C(6Li,d) reaction at sub-Coulomb energy

    Science.gov (United States)

    Mondal, Ashok; Adhikari, S.; Basu, C.

    2017-09-01

    The angular distribution of the 12C(6Li,d) reaction populating the 6.92 and 7.12 MeV states of 16O at sub-Coulomb energy (Ecm=3 MeV) are analysed in the framework of the Distorted Wave Born Approximation (DWBA). Recent results on excitation function measurements and backward angle angular distributions derive ANC for both the states on the basis of an alpha transfer mechanism. In the present work, we show that considering both forward and backward angle data in the analysis, the 7.12 MeV state at sub-Coulomb energy is populated from Compound nuclear process rather than transfer process. The 6.92 MeV state is however produced from direct reaction mechanism.

  7. Characterization of charge-exchange collisions between ultracold $\\rm{^6Li}$ atoms and $\\rm{^{40}Ca^+}$ ions

    CERN Document Server

    Saito, R; Sasakawa, M; Nakai, R; Raoult, M; Silva, H Da; Dulieu, O; Mukaiyama, T

    2016-01-01

    We investigate the energy dependence and the internal-state dependence of the charge-exchange collision cross sections in a mixture of $^6$Li atoms and $^{40}$Ca$^+$ ions in the collision energy range from 0.2 mK to 1 K. Deliberately excited ion micromotion is used to control the collision energy of atoms and ions. The energy dependence of the charge-exchange collision cross section obeys the Langevin model in the temperature range of the current experiment, and the measured magnitude of the cross section is correlated to the internal state of the $^{40}$Ca$^+$ ions. Revealing the relationship between the charge-exchange collision cross sections and the interaction potentials is an important step toward the realization of the full quantum control of the chemical reactions at an ultralow temperature regime.

  8. Hypernuclear spectroscopy of products from 6Li projectiles on a carbon target at 2 AGeV

    CERN Document Server

    Rappold, C; Nakajima, D; Saito, T R; Bertini, O; Bianchin, S; Bozkurt, V; Kavatsyuk, M; Ma, Y; Maas, F; Minami, S; Özel-Tashenov, B; Yoshida, K; Achenbach, P; Ajimura, S; Aumann, T; Gayoso, C Ayerbe; Bhang, H C; Caesar, C; Erturk, S; Fukuda, T; Göküzüm, B; Guliev, E; Hiraiwa, T; Hoffmann, J; Ickert, G; Ketenci, Z S; Khaneft, D; Kim, M; Kim, S; Koch, K; Kurz, N; Fèvre, A Le; Mizoi, Y; Moritsu, M; Nagae, T; Nungesser, L; Okamura, A; Ott, W; Pochodzalla, J; Sakaguchi, A; Sako, M; Schmidt, C J; Sekimoto, M; Simon, H; Sugimura, H; Takahashi, T; Tambave, G J; Tamura, H; Trautmann, W; Voltz, S; Yokota, N; Yoon, C J

    2013-01-01

    A novel experiment, aiming at demonstrating the feasibility of hypernuclear spectroscopy with heavy-ion beams, was conducted. Using the invariant mass method, the spectroscopy of hypernuclear products of 6Li projectiles on a carbon target at 2 AGeV was performed. Signals of the \\Lambda-hyperon and 3\\Lambda H and 4\\Lambda H hypernuclei were observed for final states of p+\\pi^-, 3He+\\pi^- and 4He+\\pi^-, respectively, with significance values of 6.7, 4.7 and 4.9\\sigma. By analyzing the proper decay time from secondary vertex distribution with the unbinned maximum likelihood fitting method, their lifetime values were deduced to be $262 ^{+56}_{-43} \\pm 45$ ps for \\Lambda, $183 ^{+42}_{-32} \\pm 37$ ps for 3\\Lambda H, and $140 ^{+48}_{-33}\\pm 35 $ ps for 4\\Lambda H.

  9. Magnetic control of ultra-cold $^6$Li and $^{174}$Yb($^3P_2$) atom mixtures with Feshbach resonances

    CERN Document Server

    Petrov, Alexander; Kotochigova, Svetlana

    2015-01-01

    We theoretically evaluate the feasibility to form magnetically-tunable Feshbach molecules in collisions between fermionic $^6$Li atoms and bosonic metastable $^{174}$Yb($^3$P$_2$) atoms. In contrast to the well-studied alkali-metal atom collisions, collisions with meta-stable atoms are highly anisotropic. Our first-principle coupled-channel calculation of these collisions reveals the existence of broad Feshbach resonances due to the combined effect of anisotropic-molecular and atomic-hyperfine interactions. In order to fit our predictions to the specific positions of experimentally-observed broad resonance structures \\cite{Deep2015} we optimized the shape of the short-range potentials by direct least-square fitting. This allowed us to identify the dominant resonance by its leading angular momentum quantum numbers and describe the role of collisional anisotropy in the creation and broadening of this and other resonances.

  10. AN UPDATED {sup 6}Li(p, {alpha}){sup 3}He REACTION RATE AT ASTROPHYSICAL ENERGIES WITH THE TROJAN HORSE METHOD

    Energy Technology Data Exchange (ETDEWEB)

    Lamia, L.; Spitaleri, C.; Sergi, M. L. [Dipartimento di Fisica e Astronomia, Universita di Catania, I-95123 Catania (Italy); Pizzone, R. G.; Tumino, A.; La Cognata, M. [INFN-Laboratori Nazionali del Sud, I-95125 Catania (Italy); Tognelli, E.; Degl' Innocenti, S.; Prada Moroni, P. G. [Dipartimento di Fisica, Universita di Pisa, I-56127 Pisa (Italy); Pappalardo, L. [Dipartimento di Fisica e Scienze della Terra, Universita di Ferrara, I-44100 Ferrara (Italy)

    2013-05-01

    The lithium problem influencing primordial and stellar nucleosynthesis is one of the most interesting unsolved issues in astrophysics. {sup 6}Li is the most fragile of lithium's stable isotopes and is largely destroyed in most stars during the pre-main-sequence (PMS) phase. For these stars, the convective envelope easily reaches, at least at its bottom, the relatively low {sup 6}Li ignition temperature. Thus, gaining an understanding of {sup 6}Li depletion also gives hints about the extent of convective regions. For this reason, charged-particle-induced reactions in lithium have been the subject of several studies. Low-energy extrapolations of these studies provide information about both the zero-energy astrophysical S(E) factor and the electron screening potential, U{sub e} . Thanks to recent direct measurements, new estimates of the {sup 6}Li(p, {alpha}){sup 3}He bare-nucleus S(E) factor and the corresponding U{sub e} value have been obtained by applying the Trojan Horse method to the {sup 2}H({sup 6}Li, {alpha} {sup 3}He)n reaction in quasi-free kinematics. The calculated reaction rate covers the temperature window 0.01 to 2T{sub 9} and its impact on the surface lithium depletion in PMS models with different masses and metallicities has been evaluated in detail by adopting an updated version of the FRANEC evolutionary code.

  11. Development of antireflection coatings with a sup 6 LiF/ sup 6 sup 2 Ni multilayer converter for ultracold neutron detectors

    CERN Document Server

    Maier-Komor, P; Bergmaier, A; Dollinger, G; Paul, S; Schott, W

    2002-01-01

    High efficiency detectors for ultracold neutrons (UCN) are needed at the new high flux neutron source, Forschungsreaktor Muenchen II. In the development described, silicon PIN diodes were chosen to detect the alpha-particles or the tritons created in the reaction sup 6 Li(n,alpha)t. The high reflectance of UCN on sup 6 Li with its positive optical potential must be compensated by a material with negative optical potential. The isotope sup 6 sup 2 Ni was chosen for this. To avoid problems due to chemical reactions of Li with humidity, the compound sup 6 LiF was chosen. One hundred and fifty double layers of sup 6 LiF/ sup 6 sup 2 Ni had to be deposited by physical vapor deposition on silicon PIN diodes which had already been coated with 88 nm approx 77 mu g/cm sup 2 of sup 5 sup 8 Ni for reflection of the UCN. The theoretical optimal thickness of the sup 6 sup 2 Ni layers is 3 nm, and that of sup 6 LiF is 6 nm. Since expensive isotopes were involved, a small source-to-substrate distance had to be used, but wit...

  12. Breakup Coupling Effects on Near-Barrier {sup 6}Li, {sup 7}Be and {sup 8}B + {sup 58}Ni Elastic Scattering Compared

    Energy Technology Data Exchange (ETDEWEB)

    Keeley, N. [Department of Nuclear Reactions, Andrzej Soltan Institute for Nuclear Studies, ul. Hoza 69, 00-681 Warsaw (Poland); Mackintosh, R.S. [Department of Physics and Astronomy, Open University, Milton Keynes, MK7 6AA (United Kingdom); Beck, C. [Institut Pluridisciplinaire Hubert Curien et Universite Louis Pasteur, Boite Postale 28, F-67037 Strasbourg Cedex 2 (France)

    2010-03-01

    New data for near-barrier {sup 6}Li, {sup 7}Be and {sup 8}B + {sup 58}Ni elastic scattering enable a comparison of breakup coupling effects for these loosely-bound projectiles. Coupled Discretised Continuum Channels (CDCC) calculations suggest that the large total reaction cross sections for {sup 8}B + {sup 58}Ni are dominated by breakup at near-barrier energies, unlike {sup 6}Li and {sup 7}Be where breakup makes a small contribution. In spite of this, the CDCC calculations show a small coupling influence due to breakup for {sup 8}B, in contrast to the situation for {sup 6}Li and {sup 7}Be. An examination of the S matrices gives a clue to this counter-intuitive behaviour.

  13. Instrumentation for solid-state dynamic nuclear polarization with magic angle spinning NMR

    Science.gov (United States)

    Rosay, Melanie; Blank, Monica; Engelke, Frank

    2016-03-01

    Advances in dynamic nuclear polarization (DNP) instrumentation and methodology have been key factors in the recent growth of solid-state DNP NMR applications. We review the current state of the art of solid-state DNP NMR instrumentation primarily based on available commercial platforms. We start with a general system overview, including options for microwave sources and DNP NMR probes, and then focus on specific developments for DNP at 100 K with magic angle spinning (MAS). Gyrotron microwave sources, passive components to transmit microwaves, the DNP MAS probe, a cooling device for low-temperature MAS, and sample preparation procedures including radicals for DNP are considered.

  14. A method for investigation of the D(4He, γ)6Li reaction in the Ultralow energy region under a high background

    Science.gov (United States)

    Bystritsky, V. M.; Dudkin, G. N.; Krylov, A. R.; Gazi, S.; Huran, J.; Nechaev, B. A.; Padalko, V. N.; Sadovsky, A. B.; Tuleushev, Yu. Zh.; Filipowicz, M.; Philippov, A. V.

    2016-07-01

    The cosmological lithium problem, that is, a noticeable discrepancy between the predicted and observed abundances of lithium, is in conflict with the Standard Big Bang Nucleosynthesis model. For example, the abundance of 7Li is 2-4 times smaller than predicted by the Standard Big Bang Nucleosynthesis. As to the abundance of 6Li, recent more accurate optical investigations have yielded only the upper limit on the 6Li/7Li ratio, which makes the problem of 6Li abundance and accordingly of disagreement with the Standard Big Bang Nucleosynthesis predictions less acute. However, experimental study of the D(4He, γ)6Li reaction cross section is still of current importance because there is a theoretical approach predicting its anomalously large value in the region of energies below the Standard Big Bang Nucleosynthesis energy. The work is dedicated to the measurement of the cross section for the D(4He, γ)6Li reaction proceeding in zirconium deuteride at the incident 4He+ion energy of 36 keV. The experiment is performed at a pulsed Hall plasma accelerator with an energy spread of 20% FWHM. A method for direct measurement of the background from the reaction chain D(4He, 4He)D→D(D, n)3He→(n, γ) and/or (n, n‧γ) ending with activation of the surrounding material by neutrons is proposed and implemented in the work. An upper limit on the D(4He, γ)6Li reaction cross section σ≤7·10-36 cm2 at the 90% confidence level is obtained.

  15. A method for investigation of the D({sup 4}He, γ){sup 6}Li reaction in the Ultralow energy region under a high background

    Energy Technology Data Exchange (ETDEWEB)

    Bystritsky, V.M. [Joint Institute for Nuclear Research, Dubna (Russian Federation); Dudkin, G.N. [National Research Tomsk Polytechnic University, Tomsk (Russian Federation); Krylov, A.R. [Joint Institute for Nuclear Research, Dubna (Russian Federation); Gazi, S.; Huran, J. [Institute of Electrical Engineering, Slovak Academy of Sciences, Bratislava (Slovakia); Nechaev, B.A.; Padalko, V.N. [National Research Tomsk Polytechnic University, Tomsk (Russian Federation); Sadovsky, A.B. [Joint Institute for Nuclear Research, Dubna (Russian Federation); Tuleushev, Yu.Zh. [Institute of Nuclear Physics, Ministry of Power Engineering, Almaty (Kazakhstan); Filipowicz, M. [Faculty of Energy and Fuels, University of Science and Technologies, Krakow (Poland); Philippov, A.V. [Joint Institute for Nuclear Research, Dubna (Russian Federation)

    2016-07-21

    The cosmological lithium problem, that is, a noticeable discrepancy between the predicted and observed abundances of lithium, is in conflict with the Standard Big Bang Nucleosynthesis model. For example, the abundance of {sup 7}Li is 2–4 times smaller than predicted by the Standard Big Bang Nucleosynthesis. As to the abundance of {sup 6}Li, recent more accurate optical investigations have yielded only the upper limit on the {sup 6}Li/{sup 7}Li ratio, which makes the problem of {sup 6}Li abundance and accordingly of disagreement with the Standard Big Bang Nucleosynthesis predictions less acute. However, experimental study of the D({sup 4}He, γ){sup 6}Li reaction cross section is still of current importance because there is a theoretical approach predicting its anomalously large value in the region of energies below the Standard Big Bang Nucleosynthesis energy. The work is dedicated to the measurement of the cross section for the D({sup 4}He, γ){sup 6}Li reaction proceeding in zirconium deuteride at the incident {sup 4}He{sup +}ion energy of 36 keV. The experiment is performed at a pulsed Hall plasma accelerator with an energy spread of 20% FWHM. A method for direct measurement of the background from the reaction chain D({sup 4}He, {sup 4}He)D→D(D, n){sup 3}He→(n, γ) and/or (n, n′γ) ending with activation of the surrounding material by neutrons is proposed and implemented in the work. An upper limit on the D({sup 4}He, γ){sup 6}Li reaction cross section σ≤7·10{sup −36} cm{sup 2} at the 90% confidence level is obtained.

  16. UAV Robust Strategy Control Based on MAS

    Directory of Open Access Journals (Sweden)

    Jian Han

    2014-01-01

    Full Text Available A novel multiagent system (MAS has been proposed to integrate individual UAV (unmanned aerial vehicle to form a UAV team which can accomplish complex missions with better efficiency and effect. The MAS based UAV team control is more able to conquer dynamic situations and enhance the performance of any single UAV. In this paper, the MAS proposed and established combines the reacting and thinking abilities to be an initiative and autonomous hybrid system which can solve missions involving coordinated flight and cooperative operation. The MAS uses BDI model to support its logical perception and to classify the different missions; then the missions will be allocated by utilizing auction mechanism after analyzing dynamic parameters. Prim potential algorithm, particle swarm algorithm, and reallocation mechanism are proposed to realize the rational decomposing and optimal allocation in order to reach the maximum profit. After simulation, the MAS has been proved to be able to promote the success ratio and raise the robustness, while realizing feasibility of coordinated flight and optimality of cooperative mission.

  17. Quasi-bound alpha resonant states populated by the {sup 12}C({sup 6}Li, d) reaction

    Energy Technology Data Exchange (ETDEWEB)

    Rodrigues, M.R.D.; Borello-Lewin, T.; Miyake, H.; Horodynski-Matsushigue, L.B.; Duarte, J.L.M.; Rodrigues, C.L.; Souza, M.A. [Universidade de Sao Paulo (IF/USP), SP (Brazil). Inst. de Fisica; Cunsolo, A.; Cappuzzello, F.; Foti, A.; Agodi, C.; Cavallaro, M. [Istituto Nazionale di Fisica Nucleare (LNS/INFN), Catania (Italy). Lab. Nazionali del Sud; Ukita, G.M. [Universidade de Santo Amaro (UNISA), Sao Paulo, SP (Brazil). Faculdade de Psicologia

    2012-07-01

    Full text: The alpha cluster phenomenon in the light nuclei structure has been the subject of a long time investigation since the proposal of the Ikeda diagrams [1]. The main purpose of the research program in progress is the investigation of this phenomenon in (x{alpha}) and (x{alpha}+n) nuclei through the ({sup 6}Li, d) alpha transfer reaction [2-4]. Alpha resonant states around the (4{alpha}) threshold in the nucleus {sup 16}O are the focus of the present contribution. In fact, the importance of these resonances at the elements production in stars is recognized, as primarily pointed out by Hoyle in {sup 12}C [6]. The existence of a rotational band with the {alpha} +{sup 12} C (Hoyle) cluster state structure was recently demonstrated by Ohkubo and Hirabayashi [6]. In order to explore this region of interest, measurements of the {sup 12}C({sup 6}Li, d){sup 16}O reaction up to 17 MeV of excitation at an incident energy of 25.5 MeV, have been performed employing the Sao Paulo Pelletron-Enge Split-Pole facility and the nuclear emulsion detection technique (plates Fuji G6B, 50 {mu}m thick). Spectra associated with six scattering angles, from 5 deg to 29 deg in the laboratory frame, each one 50 cm along the focal surface, were measured. Several narrow resonances with a quasi-bound behavior embedded in the continuum were detected and the resolution of 25 keV allowed for the separation of doublets not resolved before [7,8]. The absolute cross sections and the respective deuteron angular distributions were determined and the analysis is in progress. [1] K. Ikeda et al., Prog. Theor. Phys. Suppl. E 68, 464 (1968); H. Horiuchi, K. Ikeda, and Y. Suzuki, ibid. 44, 225 (1978). [2] M.R.D.Rodrigues et al., in12th International Conference on Nuclear Reaction Mechanism, Varenna, Italy, edited by F. Cerutti and A. Ferrari , CERN Proceedings, 2010-2, pp. 331- 335. [3] T. Borello-Lewin et al., Proceedings of SOTANCP2, Brussels, Belgium 2010, edited by P. Descouvemount et al., Int. J

  18. Millimeter-Wave Atmospheric Sounder (MAS)

    Science.gov (United States)

    Hartmann, G. K.

    1988-01-01

    MAS is a remote sensing instrument for passive sounding (limb sounding) of the earth's atmosphere from the Space Shuttle. The main objective of the MAS is to study the composition and dynamic structure of the stratosphere, mesosphere, and lower thermosphere in the height range 20 to 100 km, the region known as the middle atmosphere. The MAS will be flown on the Atmospheric Laboratory for Applications and Science (ATLAS 1) NASA mission scheduled for late 1990. The Millimeter-Wave Atmospheric Sounder will provide, for the first time, information obtained simultaneously on the temperature and on ozone concentrations in the 20 to 90 km altitude region. The information will cover a large area of the globe, will have high accuracy and high vertical resolution, and will cover both day and night times. Additionally, data on the two important molecules, H2O and ClO, will also be provided.

  19. (/sup 6/Li,d) reactions on /sup 24/Mg and /sup 26/Mg at 73 MeV

    Energy Technology Data Exchange (ETDEWEB)

    Tanabe, T.; Haga, K.; Yasue, M.; Sato, K. (Tokyo Univ., Tanashi (Japan). Inst. for Nuclear Study); Ogino, K.; Kadota, Y.; Tochi, M.; Makino, K. (Kyoto Univ. (Japan). Faculty of Engineering); Kitahara, T. (Yamanashi Medical Coll. (Japan)); Shiba, T. (Kyoto Univ. (Japan). Lab. of Nuclear Reaction)

    1983-05-09

    The sup(24,26)Mg(/sup 6/Li, d)sup(28,30)Si reactions have been studied at 73 MeV bombarding energy. The angular distributions were analyzed with exact finite-range distorted wave Born approximation calculations assuming a direct ..cap alpha..-cluster transfer. Extracted spectroscopic strengths leading to low-lying levels of /sup 28/Si and relative spectroscopic strengths between transitions to /sup 28/Si and /sup 30/Si ground states are consistent with those previously obtained by several ..cap alpha..-transfer reactions. Many strongly populated levels have been observed at Esub(x)> or approx.10 MeV for /sup 28/Si. A marked similarity was found between the deuteron spectrum and the /sup 24/Mg(..cap alpha.., ..cap alpha..)/sup 24/Mg excitation function in this excitation energy region. A brief comparison of the present ..cap alpha..-transfer results with previous two-nucleon transfer data leading to sup(28,30)Si is also presented.

  20. Improved neutron-gamma discrimination for a 6Li-glass neutron detector using digital signal analysis methods

    Science.gov (United States)

    Wang, C. L.; Riedel, R. A.

    2016-01-01

    A 6Li-glass scintillator (GS20) based neutron Anger camera was developed for time-of-flight single-crystal diffraction instruments at Spallation Neutron Source. Traditional Pulse-Height Analysis (PHA) for Neutron-Gamma Discrimination (NGD) resulted in the neutron-gamma efficiency ratio (defined as NGD ratio) on the order of 104. The NGD ratios of Anger cameras need to be improved for broader applications including neutron reflectometers. For this purpose, six digital signal analysis methods of individual waveforms acquired from photomultiplier tubes were proposed using (i) charge integration, (ii) pulse-amplitude histograms, (iii) power spectrum analysis combined with the maximum pulse-amplitude, (iv) two event parameters (a1, b0) obtained from a Wiener filter, (v) an effective amplitude (m) obtained from an adaptive least-mean-square filter, and (vi) a cross-correlation coefficient between individual and reference waveforms. The NGD ratios are about 70 times those from the traditional PHA method. Our results indicate the NGD capabilities of neutron Anger cameras based on GS20 scintillators can be significantly improved with digital signal analysis methods.

  1. Development of neutron-monitor detector using liquid organic scintillator coupled with 6Li + ZnS(Ag) Sheet.

    Science.gov (United States)

    Sato, Tatsuhiko; Endo, Akira; Yamaguchi, Yasuhiro; Takahashi, Fumiaki

    2004-01-01

    A phoswitch-type detector has been developed for monitoring neutron doses in high-energy accelerator facilities. The detector is composed of a liquid organic scintillator (BC501A) coupled with ZnS(Ag) sheets doped with 6Li. The dose from neutrons with energies above 1 MeV is evaluated from the light output spectrum of the BC501A by applying the G-function, which relates the spectrum to the neutron dose directly. The dose from lower energy neutrons, on the other hand, is estimated from the number of scintillations emitted from the ZnS(Ag) sheets. Characteristics of the phoswitch-type detector were studied experimentally in some neutron fields. It was found from the experiments that the detector has an excellent property of pulse-shape discrimination between the scintillations of BC501A and the ZnS(Ag) sheets. The experimental results also indicate that the detector is capable of reproducing doses from thermal neutrons as well as neutrons with energies from one to several tens of megaelectronvolts (MeV).

  2. Hypernuclear production cross section in the reaction of 6Li + 12C at 2A GeV

    Directory of Open Access Journals (Sweden)

    C. Rappold

    2015-07-01

    Full Text Available Hypernuclear production cross sections have been deduced for the first time with induced reaction of heavy ion beam on fixed target and by means of the invariant mass method by the HypHI Collaboration exploiting the reaction of 6Li + 12C at 2A GeV or sNN=2.70 GeV. A production cross section of 3.9±1.4 μb for 3ΛH and of 3.1±1.0 μb for 4ΛH respectively in the projectile rapidity region was inferred as well as the total production cross section of the Λ hyperon was measured and found to be equal to 1.7±0.8 mb. A global fit based on a Bayesian approach was performed in order to include and propagate statistical and systematic uncertainties. Production ratios of 3ΛH/4ΛH, 3ΛH/Λ and 4ΛH/Λ were included in the inference procedure. The strangeness population factors S3 and S4 of 3ΛH and 4ΛH respectively were extracted. In addition, the multiplicities of the Λ hyperon, 3ΛH, and 4ΛH together with the rapidity and transversal momentum density distributions of the observed hypernuclei were extracted and reported.

  3. Hypernuclear spectroscopy of products from {sup 6}Li projectiles on a carbon target at 2A GeV

    Energy Technology Data Exchange (ETDEWEB)

    Rappold, C., E-mail: c.rappold@gsi.de [Justus-Liebig-Universität Giessen, Heinrich-Buff-Ring 16, 35392 Giessen (Germany); GSI Helmholtz Centre for Heavy Ion Research, Planckstrasse 1, 64291 Darmstadt (Germany); Kim, E. [GSI Helmholtz Centre for Heavy Ion Research, Planckstrasse 1, 64291 Darmstadt (Germany); Seoul National University, Gwanakro Sillim-dong, Gwanak-gu, Seoul 151-747 (Korea, Republic of); Nakajima, D. [GSI Helmholtz Centre for Heavy Ion Research, Planckstrasse 1, 64291 Darmstadt (Germany); The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033 (Japan); Saito, T.R., E-mail: t.saito@gsi.de [GSI Helmholtz Centre for Heavy Ion Research, Planckstrasse 1, 64291 Darmstadt (Germany); Johannes Gutenberg-Universität Mainz, J.J. Becherweg 40, 55099 Mainz (Germany); The Helmholtz Institute Mainz (HIM), J.J. Becherweg 40, 55099 Mainz (Germany); Bertini, O. [GSI Helmholtz Centre for Heavy Ion Research, Planckstrasse 1, 64291 Darmstadt (Germany); Johannes Gutenberg-Universität Mainz, J.J. Becherweg 40, 55099 Mainz (Germany); Bianchin, S. [GSI Helmholtz Centre for Heavy Ion Research, Planckstrasse 1, 64291 Darmstadt (Germany); Bozkurt, V. [GSI Helmholtz Centre for Heavy Ion Research, Planckstrasse 1, 64291 Darmstadt (Germany); Nigde University, 51100 Nigde (Turkey); Kavatsyuk, M. [KVI, University of Groningen, Zernikelaan 25, NL-9747 AA Groningen (Netherlands); Ma, Y. [GSI Helmholtz Centre for Heavy Ion Research, Planckstrasse 1, 64291 Darmstadt (Germany); Johannes Gutenberg-Universität Mainz, J.J. Becherweg 40, 55099 Mainz (Germany); Maas, F. [GSI Helmholtz Centre for Heavy Ion Research, Planckstrasse 1, 64291 Darmstadt (Germany); Johannes Gutenberg-Universität Mainz, J.J. Becherweg 40, 55099 Mainz (Germany); The Helmholtz Institute Mainz (HIM), J.J. Becherweg 40, 55099 Mainz (Germany); and others

    2013-09-02

    A novel experiment, aiming at demonstrating the feasibility of hypernuclear spectroscopy with heavy ion beams, was conducted. Using the invariant mass method, the spectroscopy of hypernuclear products of {sup 6}Li projectiles on a carbon target at 2A GeV was performed. Signals of the Λ-hyperon and {sup 3}{sub Λ}H and {sup 4}{sub Λ}H hypernuclei were observed for final states of p+π{sup −}, {sup 3}He+π{sup −} and {sup 4}He+π{sup −}, respectively, with significance values of 6.7, 4.7 and 4.9σ. By analyzing the proper decay time from secondary vertex distribution with the unbinned maximum likelihood fitting method, their lifetime values were deduced to be 262{sub −43}{sup +56}±45 ps for Λ, 183{sub −32}{sup +42}±37 ps for {sup 3}{sub Λ}H, and 140{sub −33}{sup +48}±35 ps for {sup 4}{sub Λ}H.

  4. Improved neutron-gamma discrimination for a {sup 6}Li-glass neutron detector using digital signal analysis methods

    Energy Technology Data Exchange (ETDEWEB)

    Wang, C. L., E-mail: wangc@ornl.gov; Riedel, R. A. [Instrument and Source Division, Neutron Sciences Directorate, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States)

    2016-01-15

    A {sup 6}Li-glass scintillator (GS20) based neutron Anger camera was developed for time-of-flight single-crystal diffraction instruments at Spallation Neutron Source. Traditional Pulse-Height Analysis (PHA) for Neutron-Gamma Discrimination (NGD) resulted in the neutron-gamma efficiency ratio (defined as NGD ratio) on the order of 10{sup 4}. The NGD ratios of Anger cameras need to be improved for broader applications including neutron reflectometers. For this purpose, six digital signal analysis methods of individual waveforms acquired from photomultiplier tubes were proposed using (i) charge integration, (ii) pulse-amplitude histograms, (iii) power spectrum analysis combined with the maximum pulse-amplitude, (iv) two event parameters (a{sub 1}, b{sub 0}) obtained from a Wiener filter, (v) an effective amplitude (m) obtained from an adaptive least-mean-square filter, and (vi) a cross-correlation coefficient between individual and reference waveforms. The NGD ratios are about 70 times those from the traditional PHA method. Our results indicate the NGD capabilities of neutron Anger cameras based on GS20 scintillators can be significantly improved with digital signal analysis methods.

  5. Multi-elemental characterization of organic liquid samples by use of a 13 MeV {sup 6}Li{sup 3+} beam

    Energy Technology Data Exchange (ETDEWEB)

    Liendo, J.A., E-mail: jliendo@usb.v [Department of Physics, Simon Bolivar University, PO Box 89000, Caracas 1080-A (Venezuela, Bolivarian Republic of); Bernal, M.A., E-mail: mbernal@usb.v [Department of Physics, Simon Bolivar University, PO Box 89000, Caracas 1080-A (Venezuela, Bolivarian Republic of); Gonzalez, A.C. [Centro de Fisica, Instituto Venezolano de Investigaciones Cientificas, Caracas (Venezuela, Bolivarian Republic of); Caussyn, D.D.; Fletcher, N.R.; Momotyuk, O.A. [Department of Physics, Florida State University, Tallahassee (United States); Muruganathan, R.M. [Department of Chemistry, Florida State University, Tallahassee (United States); Roeder, B.T.; Wiedenhoever, I. [Department of Physics, Florida State University, Tallahassee (United States); Fischer, T. [Department of Chemistry, Florida State University, Tallahassee (United States); Kemper, K.W.; Barber, P. [Department of Physics, Florida State University, Tallahassee (United States); Sajo-Bohus, L. [Department of Physics, Simon Bolivar University, PO Box 89000, Caracas 1080-A (Venezuela, Bolivarian Republic of)

    2009-10-15

    Evaporated amniotic fluid (AF) targets have been bombarded with a 13 MeV {sup 6}Li{sup 3+} beam. Forward angle data have served to identify the {sup 1}H({sup 6}Li,{sup 1}H){sup 6}Li reaction as an alternative for hydrogen characterization of such organic samples. Detected {sup 6}Li ions elastically scattered from C, N, O, Na and Cl can also be used to determine the concentrations of these elements in AF. The analyzed AF samples have been diluted with distilled water. The effect of sample dilution on the improvement of spectrum energy resolution has been observed, confirming previous reports. The hydrogen concentration determined in the studied AF targets is shown to vary linearly with sample dilution. Two detector arrangements have been used to find out which detection scheme is the most convenient. The combination of a counter telescope and a single detector, set up at the same polar angle on the opposite side of the beam, seems to be the best choice to have a reliable particle identification and an adequate energy resolution simultaneously.

  6. Spectroscopic strengths for /sup 6/Li-induced alpha-particle transfers on /sup 18/O at 72 MeV

    Energy Technology Data Exchange (ETDEWEB)

    Tanabe, T.; Ogino, K.; Kadota, Y.; Haga, K.; Kitahara, T.; Shiba, T.

    1982-08-01

    The /sup 18/O(/sup 6/Li,d)/sup 22/Ne reaction has been studied at 72-MeV bombarding energy. The angular distributions for transitions to low-lying states in /sup 22/Ne are fitted by exact finite-range distorted-wave Born approximation calculations and yield relative spectroscopic factors in good agreement with theoretical predictions.

  7. Effects of t- and α-transfer on the spectroscopic information from the {sup 6}Li({sup 3}He,d){sup 7}Be reaction

    Energy Technology Data Exchange (ETDEWEB)

    Burtebayev, N., E-mail: nburtebayev@yandex.ru [Institute of Nuclear Physics of National Nuclear Center, 480082, Almaty, Ibragimova str. 1 (Kazakhstan); Burtebayeva, J.T.; Glushchenko, N.V.; Kerimkulov, Zh.K. [Institute of Nuclear Physics of National Nuclear Center, 480082, Almaty, Ibragimova str. 1 (Kazakhstan); Amar, A. [Al-Farabi Kazakh National University, 480078, Almaty, al-Farabi ave. 71 (Kazakhstan); Tanta University, Faculty of Science, Physics Department, Tanta (Egypt); Nassurlla, M. [Al-Farabi Kazakh National University, 480078, Almaty, al-Farabi ave. 71 (Kazakhstan); Sakuta, S.B. [National Research Center “Kurchatov Institute”, Kurchatov Sq. 1, 123182 Moscow (Russian Federation); Artemov, S.V.; Igamov, S.B.; Karakhodzhaev, A.A. [Institute of Nuclear Physics, Tashkent, Avliyo Ota str. 61 (Uzbekistan); Rusek, K. [Heavy Ion Laboratory of Warsaw University, ul. L. Pasteura 5A, PL-02-093 Warsaw (Poland); Kliczewski, S. [H. Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, ul. Radzikowskiego 152, PL-31-342 Cracow (Poland)

    2013-07-01

    Angular distributions of differential cross sections have been measured for elastic, inelastic scattering and the ({sup 3}He,d) reaction on {sup 6}Li nuclei at the E{sub lab}({sup 3}He)=34 MeV energy. The new and early obtained elastic scattering data at 34, 50, 60 and 72 MeV have been analyzed with Coupled Reaction Channels Method (CRC) taking into account triton transfer mechanism. The spectroscopic factors for t+{sup 3}He configuration of {sup 6}Li were extracted. Parameters for real part of potential have been also calculated microscopically with double folding model. The differential cross sections for proton stripping to the {sup 7}Be ground and first excited states have been analyzed by modified DWBA and CRC methods at 34 MeV. The effect of triton and α exchange on proton transfer reaction {sup 6}Li({sup 3}He,d){sup 7}Be for both ground and excited state is discussed. Spectroscopic factors and asymptotical normalization coefficients for p+{sup 6}Li configuration of {sup 7}Be have been obtained from the experimental data.

  8. 48 CFR 538.271 - MAS contract awards.

    Science.gov (United States)

    2010-10-01

    ... 48 Federal Acquisition Regulations System 4 2010-10-01 2010-10-01 false MAS contract awards. 538... Schedules 538.271 MAS contract awards. (a) MAS awards will be for commercial items as defined in FAR 2.101. Negotiate contracts as a discount from established catalog prices. (b) Before awarding any MAS contract...

  9. Novel 4{pi} Detection System for the Measurement of the {sup 6}Li(n,{alpha}){sup 3}H Reaction Cross Section

    Energy Technology Data Exchange (ETDEWEB)

    Giorginis, Georgios; Bencardino, Raffaele [European Commission, Joint Research Centre, Institute for Reference Materials and Measurements (IRMM), Retieseweg 111, B-2440 Geel (Belgium)

    2011-12-13

    A dedicated one-dimensional Time Projection Chamber (1D-TPC) was designed and produced at IRMM to determine the {sup 6}Li(n,{alpha}){sup 3}H cross section in the 0.4-2.8 MeV energy range, aiming at 5% accuracy. The basic TPC components were a twin gridded ionisation chamber (GIC) with interwired electrodes and fast digitisation of the anode and cathode signals. The energy of both reaction products emitted from a thin {sup 6}LiF sample at the common TPC cathode was measured. A Kr(97%)CO{sub 2}(3%) mixture was used as the detector gas at a pressure up to 3.5 bar. A {sup 238}U sample mounted on the cathode of an ionisation chamber without grid was used as the neutron flux monitor. Special care was taken to reduce the experimental sources of uncertainty. The beam-monitor {sup 238}U sample was characterised at IRMM by low-geometry {alpha}-counting with an accuracy of 0.1%. A {sup 6}Li sample was produced at IRMM by vacuum evaporation of {sup 6}LiF onto transparent aluminium backing. The number of {sup 6}Li atoms will be measured via Thermal Neutron Depth Profiling with an expected accuracy of 2% with respect to an IRMM Standard Reference Material. First test measurements were performed using a monoenergetic neutron beam produced by the T(p,n){sup 3}He reaction at the IRMM 7 MV Van de Graaff accelerator. The experimental method and preliminary results are presented.

  10. Functions of MgH2 in hydrogen storage reactions of the 6LiBH4-CaH2 reactive hydride composite.

    Science.gov (United States)

    Zhou, Yifan; Liu, Yongfeng; Zhang, Yu; Gao, Mingxia; Pan, Hongge

    2012-08-28

    A significant improvement of hydrogen storage properties was achieved by introducing MgH(2) into the 6LiBH(4)-CaH(2) system. It was found that ~8.0 wt% of hydrogen could be reversibly stored in a 6LiBH(4)-CaH(2)-3MgH(2) composite below 400 °C and 100 bar of hydrogen pressure with a stepwise reaction, which is superior to the pristine 6LiBH(4)-CaH(2) and LiBH(4) samples. Upon dehydriding, MgH(2) first decomposed to convert to Mg and liberate hydrogen with an on-set temperature of ~290 °C. Subsequently, LiBH(4) reacted with CaH(2) to form CaB(6) and LiH in addition to further hydrogen release. Hydrogen desorption from the 6LiBH(4)-CaH(2)-3MgH(2) composite finished at ~430 °C in non-isothermal model, a 160 °C reduction relative to the 6LiBH(4)-CaH(2) sample. JMA analyses revealed that hydrogen desorption was a diffusion-controlled reaction rather than an interface reaction-controlled process. The newly produced Mg of the first-step dehydrogenation possibly acts as the heterogeneous nucleation center of the resultant products of the second-step dehydrogenation, which diminishes the energy barrier and facilitates nucleation and growth, consequently reducing the operating temperature and improving the kinetics of hydrogen storage.

  11. Fundamental Science Tools for Geologic Carbon Sequestration and Mineral Carbonation Chemistry: In Situ Magic Angle Spinning (MAS) Nuclear Magnetic Resonance

    Science.gov (United States)

    Hoyt, D. W.; Turcu, R. V.; Sears, J. A.; Rosso, K. M.; Burton, S. D.; Kwak, J.; Felmy, A. R.; Hu, J.

    2010-12-01

    GCS is one of the most promising ways of mitigating atmospheric greenhouse gases. Mineral carbonation reactions are potentially important to the long-term sealing effectiveness of caprock but remain poorly predictable, particularly reactions occurring in low-water supercritical CO2(scCO2)-dominated environments where the chemistry has not been adequately explored. In situ probes that provide molecular-level information is desirable for investigating mechanisms and rates of GCS mineral carbonation reactions. MAS-NMR is a powerful tool for obtaining detailed molecular structure and dynamics information of a system regardless whether the system is in a solid, a liquid, a gaseous, or a supercritical state, or a mixture thereof. However, MAS NMR under scCO2 conditions has never been realized due to the tremendous technical difficulties of achieving and maintaining high pressure within a fast spinning MAS rotor. In this work, we report development of a unique high pressure MAS NMR capability, and its application to mineral carbonation chemistry in scCO2 under geologically relevant temperatures and pressures. Our high pressure MAS rotor has successfully maintained scCO2 conditions with minimal leakage over a period of 72 hours. Mineral carbonation reactions of a model magnesium silicate (forsterite) reacted with 96 bars scCO2 containing varying amounts of H2O (both below and above saturation of the scCO2) were investigated at 50○C. Figure 1 shows typical in situ 13C MAS NMR spectra demonstrating that the peaks corresponding to the reactants, intermediates, and the magnesium carbonation products are all observed in a single spectrum. For example, the scCO2 peak is located at 126.1 ppm. Reaction intermediates include the aqueous species HCO3-(160 ppm), partially hydrated/hydroxylated magnesium carbonates(166-168 ppm), and can easily be distinguished from final product magnesite(170 ppm). The new capability and this model mineral carbonation process will be overviewed in

  12. Ultra fast magic angle spinning solid - state NMR spectroscopy of intact bone.

    Science.gov (United States)

    Singh, Chandan; Rai, Ratan Kumar; Kayastha, Arvind M; Sinha, Neeraj

    2016-02-01

    Ultra fast magic angle spinning (MAS) has been a potent method to significantly average out homogeneous/inhomogeneous line broadening in solid-state nuclear magnetic resonance (ssNMR) spectroscopy. It has given a new direction to ssNMR spectroscopy with its different applications. We present here the first and foremost application of ultra fast MAS (~60 kHz) for ssNMR spectroscopy of intact bone. This methodology helps to comprehend and elucidate the organic content in the intact bone matrix with resolution and sensitivity enhancement. At this MAS speed, amino protons from organic part of intact bone start to appear in (1) H NMR spectra. The experimental protocol of ultra-high speed MAS for intact bone has been entailed with an additional insight achieved at 60 kHz.

  13. On the use of ultracentrifugal devices for routine sample preparation in biomolecular magic-angle-spinning NMR.

    Science.gov (United States)

    Mandal, Abhishek; Boatz, Jennifer C; Wheeler, Travis B; van der Wel, Patrick C A

    2017-02-22

    A number of recent advances in the field of magic-angle-spinning (MAS) solid-state NMR have enabled its application to a range of biological systems of ever increasing complexity. To retain biological relevance, these samples are increasingly studied in a hydrated state. At the same time, experimental feasibility requires the sample preparation process to attain a high sample concentration within the final MAS rotor. We discuss these considerations, and how they have led to a number of different approaches to MAS NMR sample preparation. We describe our experience of how custom-made (or commercially available) ultracentrifugal devices can facilitate a simple, fast and reliable sample preparation process. A number of groups have since adopted such tools, in some cases to prepare samples for sedimentation-style MAS NMR experiments. Here we argue for a more widespread adoption of their use for routine MAS NMR sample preparation.

  14. Characterization of {sup 6}LiF:Mg,Cu,P (TLD-600 H) estimate of E, b and s parameters

    Energy Technology Data Exchange (ETDEWEB)

    Andres, P. A., E-mail: andresp@cab.cnea.gov.ar [Centro Atomico Bariloche, Division Proteccion Radiologica / CNEA, Av. E. Bustillo Km 9.5, R8402AGP San Carlos de Bariloche (Argentina)

    2015-10-15

    LiF:Mg,Cu,P dosemeters are useful for low-dose measurements because of its high sensitivity compared to the LiF:Mg,Ti dosemeters. {sup 7}LiF:Mg,Cu,P have been used for environmental dosimetry in Bariloche Atomic Centre for almost a decade. Since {sup 6}LiF:Mg,Cu,P dosemeters were intended to be used for X ray diagnosis dosimetry in neonatology, they had to be characterized first. The main goal of measuring and analyzing Tl glow curves is the extraction of some parameters that can be used to describe the Tl process in the material. This job focused on the estimation of the activation energy E for the Tl traps, the frequency factor s and the order of kinetics b of the Tl process. Furthermore, the most appropriate time-temperature profile (Ttp) was determined as well as the annealing temperature and time, which resulted being 240 degrees C for 10 minutes. The Ttp used was 140 degrees C for 10 seconds, a heating rate of 20/s until 240 degrees C, remaining at this temperature for 20 seconds, and then an exponential cooling until 50 degrees C. After applying the whole glow-peak method for different orders of kinetic, and the Kitis equation assuming a first order kinetics, the values obtained were: E = (1.066 ± 0.025) eV, as a weighted average of both methods, and a frequency factor s = (3.57 ± 1.56) E-10 s{sup -1} again as a weighted average of both methods. In both cases a first order kinetics (b = 1) was assumed. The dosemeters were irradiated with a calibrated {sup 137}Cs source and read with a Harshaw TLD{sup TM} Model 3500 reader resulting in a minimum detectable dose of about 20 μGy. (Author)

  15. Compact NMR

    Energy Technology Data Exchange (ETDEWEB)

    Bluemich, Bernhard; Haber-Pohlmeier, Sabina; Zia, Wasif [RWTH Aachen Univ. (Germany). Inst. fuer Technische und Makromolekulare Chemie (ITMC)

    2014-06-01

    Nuclear Magnetic Resonance (NMR) spectroscopy is the most popular method for chemists to analyze molecular structures, while Magnetic Resonance Imaging (MRI) is a non-invasive diagnostic tool for medical doctors that provides high-contrast images of biological tissue. In both applications, the sample (or patient) is positioned inside a large, superconducting magnet to magnetize the atomic nuclei. Interrogating radio-frequency pulses result in frequency spectra that provide the chemist with molecular information, the medical doctor with anatomic images, and materials scientist with NMR relaxation parameters. Recent advances in magnet technology have led to a variety of small permanent magnets to allow compact and low-cost instruments. The goal of this book is to provide an introduction to the practical use of compact NMR at a level nearly as basic as the operation of a smart phone.

  16. A social-democracia do MAS boliviano

    Directory of Open Access Journals (Sweden)

    Guilherme Simões Reis

    2013-12-01

    Full Text Available O partido MAS, que governa a Bolívia e é liderado pelo presidente Evo Morales, geralmente é classificado como populista ou como revolucionário. Este artigo contesta ambos os diagnósticos, e sustenta que o MAS é um partido social-democrata. Tanto em sua gênese, como em seu comportamento na oposição, como em suas políticas no governo, o MAS apresenta todas as características necessárias para ser classificado como um representante da social-democracia. Para contestar os diagnósticos predominantes na literatura, o argumento desenvolve-se aplicando três distintas abordagens sobre a social-democracia. Uma comparação histórico-ideológica com os partidos tradicionalmente apontados como social-democratas mostra que o MAS assemelha-se a eles tanto em sua origem fortemente sindical como no tipo de mudança que introduziu na política do país. Uma análise institucional mostra que não procedem as acusações de que é antissistema e contrário à democracia, características associadas tanto aos "populistas", de acordo com "teóricos das duas esquerdas latino-americanas", como aos partidos adeptos da "revolução violenta". Por fim, uma análise das políticas adotadas pelo MAS no governo indica que estão alinhadas com aquelas consideradas como social-democráticas no contexto de integração dos mercados globais. Argumenta-se no texto que o MAS não é em geral classificado como social-democrata, em parte devido a uma visão equivocada sobre suas práticas, e em parte por uma tendência dos estudiosos a chamarem a atenção para o que lhe é específico, e não para o que ele tem em comum com outros partidos de esquerda, como é feito com quaisquer partidos ao catalogá-los em famílias.

  17. In situ NMR analysis of fluids contained in sedimentary rock

    Science.gov (United States)

    de Swiet TM; Tomaselli; Hurlimann; Pines

    1998-08-01

    Limitations of resolution and absorption in standard chemical spectroscopic techniques have made it difficult to study fluids in sedimentary rocks. In this paper, we show that a chemical characterization of pore fluids may be obtained in situ by magic angle spinning (MAS) nuclear magnetic resonance (NMR), which is normally used for solid samples. 1H MAS-NMR spectra of water and crude oil in Berea sandstone show sufficient chemical shift resolution for a straightforward determination of the oil/water ratio. Copyright 1998 Academic Press.

  18. 一个多Agent系统规范--MAS/KIB%MAS/KIB--a Multiagent System Specification

    Institute of Scientific and Technical Information of China (English)

    胡舜耕; 钟义信

    2000-01-01

    采用K(知道),B(相信),I(意愿)等几个基本的心智状态,建立了一个多Agent系统逻辑规范-MAS/KIB,讨论了其语法、模型和语义,给出了公理和推理规则,研究了MAS/KIB的一些基本性质.

  19. Magic angle spinning NMR of paramagnetic proteins.

    Science.gov (United States)

    Knight, Michael J; Felli, Isabella C; Pierattelli, Roberta; Emsley, Lyndon; Pintacuda, Guido

    2013-09-17

    Metal ions are ubiquitous in biochemical and cellular processes. Since many metal ions are paramagnetic due to the presence of unpaired electrons, paramagnetic molecules are an important class of targets for research in structural biology and related fields. Today, NMR spectroscopy plays a central role in the investigation of the structure and chemical properties of paramagnetic metalloproteins, linking the observed paramagnetic phenomena directly to electronic and molecular structure. A major step forward in the study of proteins by solid-state NMR came with the advent of ultrafast magic angle spinning (MAS) and the ability to use (1)H detection. Combined, these techniques have allowed investigators to observe nuclei that previously were invisible in highly paramagnetic metalloproteins. In addition, these techniques have enabled quantitative site-specific measurement of a variety of long-range paramagnetic effects. Instead of limiting solid-state NMR studies of biological systems, paramagnetism provides an information-rich phenomenon that can be exploited in these studies. This Account emphasizes state-of-the-art methods and applications of solid-state NMR in paramagnetic systems in biological chemistry. In particular, we discuss the use of ultrafast MAS and (1)H-detection in perdeuterated paramagnetic metalloproteins. Current methodology allows us to determine the structure and dynamics of metalloenzymes, and, as an example, we describe solid-state NMR studies of microcrystalline superoxide dismutase, a 32 kDa dimer. Data were acquired with remarkably short times, and these experiments required only a few milligrams of sample.

  20. Study of 29Si MAS NMR Spectroscopy and Electro-Optic Property Based on Polyimide/SiO2%聚酰亚胺/SiO2杂化材料的硅核磁共振波谱和电光性质的研究

    Institute of Scientific and Technical Information of China (English)

    邱凤仙; 周钰明; 刘举正; 张旭苹

    2006-01-01

    以含氟的二胺5,5′-(六氟异丙基)-二-(2-氨基苯酚)(6FHP)及二酐4,4′-(六氟异丙基)-苯二酸酐(6FDA)或均苯四甲酸酐 (PMDA)为单体,以分散红1 (DR1) 为活性生色分子合成具有非线性光学特性的含氟聚酰亚胺,并采用溶胶-凝胶(Sol-Gel) 法合成相应的聚酰亚胺/SiO2杂化材料.采用固态29Si MAS NMR谱研究了含氟聚酰亚胺/SiO2杂化材料的交联结构,结果表明杂化材料中是以T3、Q3、Q4结构为主,说明在杂化材料中形成了交联网状结构.采用衰减全反射(ATR)测定了聚酰亚胺和杂化材料在832 nm处的电光系数,其值分别为32、28、34和29 pm/V,结果表明具有较高的电光系数.

  1. Performance of RINEPT is amplified by dipolar couplings under ultrafast MAS conditions.

    Science.gov (United States)

    Zhang, Rongchun; Ramamoorthy, Ayyalusamy

    2014-06-01

    The refocused insensitive nuclei enhanced by polarization transfer (RINEPT) technique is commonly used for heteronuclear polarization transfer in solution and solid-state NMR spectroscopy. Suppression of dipolar couplings, either by fast molecular motions in solution or by a combination of MAS and multiple pulse sequences in solids, enables the polarization transfer via scalar couplings. However, the presence of unsuppressed dipolar couplings could alter the functioning of RINEPT, particularly under fast/ultrafast MAS conditions. In this study, we demonstrate, through experiments on rigid solids complemented by numerical simulations, that the polarization transfer efficiency of RINEPT is dependent on the MAS frequency. In addition, we show that heteronuclear dipolar coupling is the dominant factor in the polarization transfer, which is strengthened by the presence of (1)H-(1)H dipolar couplings. In fact, the simultaneous presence of homonuclear and heteronuclear dipolar couplings is the premise for the polarization transfer by RINEPT, whereas the scalar coupling plays an insignificant role under ultrafast MAS conditions on rigid solids. Our results additionally reveal that the polarization transfer efficiency decreases with the increasing duration of RF pulses used in the RINEPT sequence.

  2. Upgrade of the POLDI diffractometer with a ZnS(Ag)/6LiF scintillation detector read out with WLS fibers coupled to SiPMs

    OpenAIRE

    Mosset, J. -B.; Stoykov, A.; Davydov, V.; Hildebrandt, M.; Van Swygenhoven, H.; W. Wagner

    2013-01-01

    A thermal neutron detector based on ZnS(Ag)/6LiF scintillator, wavelength-shifting fibers (WLS) and silicon photomultipliers (SiPM) is under development at the Paul Scherrer Institute (PSI) for upgrading the POLDI instrument, a pulse-overlap diffractometer. The design of the detector is outlined, and the measurements performed on a single channel prototype are presented. An innovative signal processing system based on a photon counting approach is under development. Its principle of operation...

  3. Characteristics of a thermal neutrons scintillation detector with the [ZnS(Ag)+$^6$LiF] at different conditions of measurements

    OpenAIRE

    Alekseenko, V. V.; Barabanov, I. R.; Etezov, R. A.; Gavrilyuk, Yu. M.; Gangapshev, A. M.; Gezhaev, A. M.; Kazalov, V. V.; Khokonov, A. Kh.; V.V. Kuzminov; Panasenko, S. I.; Ratkevich, S. S.

    2015-01-01

    A construction of a thermal neutron testing detector with a thin [ZnS(Ag)+$^6$LiF] scintillator is described. Results of an investigation of sources of the detector pulse origin and the pulse features in a ground and underground conditions are presented. Measurements of the scintillator own background, registration efficiency and a neutron flux at different objects of the BNO INR RAS were performed. The results are compared with the ones measured by the $^3$He proportional counter.

  4. Ultracold neutron detection with {sup 6}Li-doped glass scintillators. NANOSC: A fast ultracold neutron detector for the nEDM experiment at the Paul Scherrer Institute

    Energy Technology Data Exchange (ETDEWEB)

    Ban, G.; Lefort, T.; Lemiere, Y.; Naviliat-Cuncic, O.; Pierre, E.; Quemener, G.; Rogel, G. [Normandie Univ, ENSICAEN, UNICAEN, CNRS/IN2P3, LPC Caen, Caen (France); Bison, G.; Chowdhuri, Z.; Henneck, R.; Lauss, B.; Mtchedlishvili, A.; Schmidt-Wellenburg, P.; Zsigmond, G. [Paul Scherrer Institute, Villigen-PSI (Switzerland); Bodek, K.; Zejma, J. [Jagiellonian University, Marian Smoluchowski Institute of Physics, Cracow (Poland); Geltenbort, P. [Institut Laue-Langevin, Grenoble (France); Griffith, W.C.; Musgrave, M. [University of Sussex, Falmer, Department of Physics and Astronomy, Brighton (United Kingdom); Helaine, V. [Normandie Univ, ENSICAEN, UNICAEN, CNRS/IN2P3, LPC Caen, Caen (France); Paul Scherrer Institute, Villigen-PSI (Switzerland); Kasprzak, M.; Koss, P.A.; Severijns, N.; Wursten, E. [Katholieke Universiteit Leuven, Instituut voor Kernen Stralingsfysica, Leuven (Belgium); Kermaidic, Y.; Pignol, G.; Rebreyend, D. [LPSC, Universite Grenoble Alpes, CNRS/IN2P3, Grenoble (France); Kirch, K.; Komposch, S.; Krempel, J.; Ries, D. [Paul Scherrer Institute, Villigen-PSI (Switzerland); Institute for Particle Physics, ETH Zuerich, Zuerich (Switzerland); Kozela, A. [Henryk Niedwodniczanski Institute for Nuclear Physics, Cracow (Poland); Piegsa, F.M.; Rawlik, M. [Institute for Particle Physics, ETH Zuerich, Zuerich (Switzerland); Roccia, S. [CSNSM, Universite Paris Sud, CNRS/IN2P3, Orsay (France)

    2016-10-15

    This paper summarizes the results from measurements aiming to characterize ultracold neutron detection with {sup 6}Li-doped glass scintillators. Single GS10 or GS20 scintillators, with a thickness of 100-200μm, fulfill the ultracold neutron detection requirements with an acceptable neutron-gamma discrimination. This discrimination is clearly improved with a stack of two scintillators: a {sup 6}Li-depleted glass bonded to a {sup 6}Li-enriched glass. The technique of optical contact bonding is used between the two glasses in order to eliminate the need for optical glue or grease between them. Relative to a {sup 3}He Strelkov gas detector, the scintillator's detection efficiency is lower for UCN energies close to the scintillator's Fermi potential (85-100 neV), but becomes larger at higher UCN energies. Coupled to a digital data acquisition system, counting rates up to a few 10{sup 5} counts/s can be handled. A detector based on such a scintillator stack arrangement was built and has been used in the neutron electric dipole moment experiment at the Paul Scherrer Institute since 2010. Its response for routine runs of the neutron electric dipole moment experiment is presented. (orig.)

  5. Ultracold neutron detection with 6Li-doped glass scintillators, NANOSC: a fast ultracold neutron detector for the nEDM experiment at the Paul Scherrer Institute

    CERN Document Server

    Ban, G; Bodek, K; Chowdhuri, Z; Geltenbort, P; Griffith, W C; Hélaine, V; Henneck, R; Kasprzak, M; Kermaidic, Y; Kirch, K; Komposch, S; Koss, P A; Kozela, A; Krempel, J; Lauss, B; Lefort, T; Lemière, Y; Mtchedlishvili, A; Musgrave, M; Naviliat-Cuncic, O; Piegsa, F M; Pierre, E; Pignol, G; Quéméner, G; Rawlik, M; Ries, D; Rebreyend, D; Roccia, S; Rogel, G; Schmidt-Wellenburg, P; Severijns, N; Wursten, E; Zejma, J; Zsigmond, G

    2016-01-01

    This paper summarizes the results from measurements aiming to characterize ultracold neutron detection with 6Li-doped glass scintillators. Single GS10 or GS20 scintillators, with a thickness of 100-200 micrometer, fulfill the ultracold neutron detection requirements with an acceptable neutron-gamma discrimination. This discrimination is clearly improved with a stack of two scintillators: a 6Li-depleted glass bonded to a 6Li-enriched glass. The optical contact bonding is used between the scintillators in order to obtain a perfect optical contact. The scintillator's detection efficiency is similar to that of a 3He Strelkov gas detector. Coupled to a digital data acquisition system, counting rates up to a few 10^5 counts/s can be handled. A detector based on such a scintillator stack arrangement was built and has been used in the neutron electric dipole moment experiment at the Paul Scherrer Institute since 2010. Its response for the regular runs of the neutron electric dipole moment experiment is presented.

  6. Ultracold neutron detection with 6Li-doped glass scintillators. NANOSC: A fast ultracold neutron detector for the nEDM experiment at the Paul Scherrer Institute

    Science.gov (United States)

    Ban, G.; Bison, G.; Bodek, K.; Chowdhuri, Z.; Geltenbort, P.; Griffith, W. C.; Hélaine, V.; Henneck, R.; Kasprzak, M.; Kermaidic, Y.; Kirch, K.; Komposch, S.; Koss, P. A.; Kozela, A.; Krempel, J.; Lauss, B.; Lefort, T.; Lemière, Y.; Mtchedlishvili, A.; Musgrave, M.; Naviliat-Cuncic, O.; Piegsa, F. M.; Pierre, E.; Pignol, G.; Quéméner, G.; Rawlik, M.; Ries, D.; Rebreyend, D.; Roccia, S.; Rogel, G.; Schmidt-Wellenburg, P.; Severijns, N.; Wursten, E.; Zejma, J.; Zsigmond, G.

    2016-10-01

    This paper summarizes the results from measurements aiming to characterize ultracold neutron detection with 6Li-doped glass scintillators. Single GS10 or GS20 scintillators, with a thickness of 100-200μm, fulfill the ultracold neutron detection requirements with an acceptable neutron-gamma discrimination. This discrimination is clearly improved with a stack of two scintillators: a 6Li-depleted glass bonded to a 6Li-enriched glass. The technique of optical contact bonding is used between the two glasses in order to eliminate the need for optical glue or grease between them. Relative to a 3He Strelkov gas detector, the scintillator's detection efficiency is lower for UCN energies close to the scintillator's Fermi potential (85-100 neV), but becomes larger at higher UCN energies. Coupled to a digital data acquisition system, counting rates up to a few 105 counts/s can be handled. A detector based on such a scintillator stack arrangement was built and has been used in the neutron electric dipole moment experiment at the Paul Scherrer Institute since 2010. Its response for routine runs of the neutron electric dipole moment experiment is presented.

  7. NMR GHZ

    CERN Document Server

    Laflamme, R; Zurek, W H; Catasti, P; Mariappan, S V S

    1998-01-01

    We describe the creation of a Greenberger-Horne-Zeilinger (GHZ) state of the form |000>+|111> (three maximally entangled quantum bits) using Nuclear Magnetic Resonance (NMR). We have successfully carried out the experiment using the proton and carbon spins of trichloroethylene, and confirmed the result using state tomography. We have thus extended the space of entangled quantum states explored systematically to three quantum bits, an essential step for quantum computation.

  8. 1020MHz single-channel proton fast magic angle spinning solid-state NMR spectroscopy.

    Science.gov (United States)

    Pandey, Manoj Kumar; Zhang, Rongchun; Hashi, Kenjiro; Ohki, Shinobu; Nishijima, Gen; Matsumoto, Shinji; Noguchi, Takashi; Deguchi, Kenzo; Goto, Atsushi; Shimizu, Tadashi; Maeda, Hideaki; Takahashi, Masato; Yanagisawa, Yoshinori; Yamazaki, Toshio; Iguchi, Seiya; Tanaka, Ryoji; Nemoto, Takahiro; Miyamoto, Tetsuo; Suematsu, Hiroto; Saito, Kazuyoshi; Miki, Takashi; Ramamoorthy, Ayyalusamy; Nishiyama, Yusuke

    2015-12-01

    This study reports a first successful demonstration of a single channel proton 3D and 2D high-throughput ultrafast magic angle spinning (MAS) solid-state NMR techniques in an ultra-high magnetic field (1020MHz) NMR spectrometer comprised of HTS/LTS magnet. High spectral resolution is well demonstrated.

  9. Solid State NMR Characterization of Complex Metal Hydrides systems for Hydrogen Storage Applications

    Directory of Open Access Journals (Sweden)

    Son-Jong Hwang

    2011-12-01

    Full Text Available Solid state NMR is widely applied in studies of solid state chemistries for hydrogen storage reactions. Use of 11B MAS NMR in studies of metal borohydrides (BH4 is mainly focused, revisiting the issue of dodecaborane formation and observation of 11B{1H} Nuclear Overhauser Effect.

  10. Bare astrophysical S(E)-factor for the {sup 6}Li(d, {alpha}){sup 4}He and {sup 7}Li(p, {alpha}){sup 4}He reactions at astrophysical energies

    Energy Technology Data Exchange (ETDEWEB)

    Pizzone, R.G.; Spitaleri, C.; Lattuada, M.; Musumarra, A.; Pellegriti, M.G.; Romano, S.; Tumino, A.; Cherubini, S.; Figuera, P.; Miljanic, D.; Rolfs, C.; Typel, S.; Wolter, H.H.; Castellani, V.; Degl' Innocenti, S.; Imperio, A

    2003-05-05

    The Trojan Horse Method has been applied to study the {sup 7}Li(p, {alpha}){sup 4}He and {sup 6}(Li(d, {alpha}){sup 4}He reactions through the {sup 7}Li(d, {alpha}{alpha})n and {sup 6}Li({sup 6}Li, {alpha}{alpha}){sup 4}He three body processes, respectively. The electron screening potential deduced from these experiments is much larger than the adiabatic approximation prediction for both cases; the systematic discrepancy between data and theoretical predictions is thus confirmed. Astrophysical implications of these measurements are also discussed.

  11. Dynamic nuclear polarization NMR spectroscopy allows high-throughput characterization of microporous organic polymers.

    Science.gov (United States)

    Blanc, Frédéric; Chong, Samantha Y; McDonald, Tom O; Adams, Dave J; Pawsey, Shane; Caporini, Marc A; Cooper, Andrew I

    2013-10-16

    Dynamic nuclear polarization (DNP) solid-state NMR was used to obtain natural abundance (13)C and (15)N CP MAS NMR spectra of microporous organic polymers with excellent signal-to-noise ratio, allowing for unprecedented details in the molecular structure to be determined for these complex polymer networks. Sensitivity enhancements larger than 10 were obtained with bis-nitroxide radical at 14.1 T and low temperature (∼105 K). This DNP MAS NMR approach allows efficient, high-throughput characterization of libraries of porous polymers prepared by combinatorial chemistry methods.

  12. Forensic examination of electrical tapes using high resolution magic angle spinning ¹H NMR spectroscopy.

    Science.gov (United States)

    Schoenberger, Torsten; Simmross, Ulrich; Poppe, Christian

    2016-01-01

    The application of high resolution magic angle spinning (HR-MAS) (1)H NMR spectroscopy is ideally suited for the differentiation of plastics. In addition to the actual material composition, the different types of polymer architectures and tacticity provide characteristic signals in the fingerprint of the (1)H NMR spectra. The method facilitates forensic comparison, as even small amounts of insoluble but swellable plastic particles are utilized. The performance of HR-MAS NMR can be verified against other methods that were recently addressed in various articles about forensic tape comparison. In this study samples of the 90 electrical tapes already referenced by the FBI laboratory were used. The discrimination power of HR-MAS is demonstrated by the fact that more tape groups can be distinguished by NMR spectroscopy than by using the combined evaluation of several commonly used analytical techniques. An additional advantage of this robust and quick method is the very simple sample preparation.

  13. $\\Sigma^- p$ emission rates in $K^-$ absorptions at rest on $^6$Li, $^7$Li, $^{9}$Be, $^{13}$C and $^{16}$O

    CERN Document Server

    Agnello, M; Bertani, M; Bonomi, G; Botta, E; Bregant, M; Bressani, T; Bufalino, S; Busso, L; Calvo, D; Camerini, P; Dalena, B; De Mori, F; D'Erasmo, G; Feliciello, A; Filippi, A; Fiore, E M; Fontana, A; Fujioka, H; Genova, P; Gianotti, P; Grion, N; Lucherini, V; Marcello, S; Morra, O; Nagae, T; Outa, H; Pantaleo, A; Paticchio, V; Piano, S; Rui, R; Simonetti, G; Wheadon, R; Zenoni, A

    2015-01-01

    An experimental study of the $K^-_{stop}A\\rightarrow \\Sigma^- p A'$ reaction on $A=^6$Li, $^7$Li, $^9$Be, $^{13}$C and $^{16}$O $p$-shell nuclei is presented. The data were collected by the FINUDA spectrometer operating at the DA$\\Phi$NE $\\phi$-factory (LNF-INFN, Italy). Emission rates for the reaction in the mentioned nuclei are measured and compared with the few existing data. The spectra of several observables are discussed; indications of Quasi-Free absorptions by a $(np)$ pair embedded in the $A$ nucleus can be obtained from the study of the missing mass distributions.

  14. All-optical production of dual Bose-Einstein condensates of paired fermions and bosons with 6Li and 7Li

    Science.gov (United States)

    Ikemachi, Takuya; Ito, Aki; Aratake, Yukihito; Chen, Yiping; Koashi, Masato; Kuwata-Gonokami, Makoto; Horikoshi, Munekazu

    2017-01-01

    We report the first all-optical production of dual Bose-Einstein condensates (BECs) of paired 6Li (fermion) and one spin state of 7Li (boson) at the magnetic field where the s-wave interactions between fermions are resonant. Fermions are cooled efficiently by evaporative cooling and they serve as coolant for bosons. As a result, the dual condensates can be achieved by using a simple experimental apparatus and procedures, as in the case of the all-optical production of a single BEC. We show that the all-optical method enables us to realize variety of ultracold Bose-Fermi mixtures.

  15. Breakup coupling effects on near-barrier inelastic scattering of the weakly bound {sup 6}Li projectile on a {sup 144}Sm target

    Energy Technology Data Exchange (ETDEWEB)

    Woodard, A.E., E-mail: awoodard@nd.edu [Laboratorio Tandar, Comision Nacional de Energia Atomica, B1650KNA San Martin, Buenos Aires (Argentina); Figueira, J.M. [Laboratorio Tandar, Comision Nacional de Energia Atomica, B1650KNA San Martin, Buenos Aires (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas, C1033AAJ Ciudad de Buenos Aires (Argentina); Otomar, D.R. [Instituto de Fisica, Universidade Federal Fluminense, Gragoata, Niteroi, R. J., 24210-340 (Brazil); Fernandez Niello, J.O. [Laboratorio Tandar, Comision Nacional de Energia Atomica, B1650KNA San Martin, Buenos Aires (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas, C1033AAJ Ciudad de Buenos Aires (Argentina); Escuela de Ciencia y Tecnologia, Universidad de San Martin, B1650BWA San Martin, Buenos Aires (Argentina); Lubian, J. [Instituto de Fisica, Universidade Federal Fluminense, Gragoata, Niteroi, R. J., 24210-340 (Brazil)

    2012-01-01

    Angular distributions for the inelastic scattering of the weakly bound {sup 6}Li nucleus from a {sup 144}Sm target (associated with the contributions of both the 2{sub 1}{sup +} and 3{sub 1}{sup -144}Sm excited states together) were measured at bombarding energies close to the Coulomb barrier. The experimental data were compared with expected results based on continuum discretized coupled-channel (CDCC) calculations. The results confirm that it is essential to include continuum-continuum couplings to reproduce the experimental data. The analysis demonstrates that inelastic scattering data can be a critical tool in testing full CDCC calculations involving weakly bound nuclei.

  16. Cross-section measurements for {sup 239}Pu(n,f) and {sup 6}Li(n,{alpha}) with a lead slowing-down spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Rochman, D. [National Nuclear Data Center, Brookhaven National Laboratory, Upton, NY 11973-5000 (United States)]. E-mail: drochman@bnl.gov; Haight, R.C. [Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)]. E-mail: haight@lanl.gov; O' Donnell, J.M. [Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)]. E-mail: odonnell@lanl.gov; Wender, S.A. [Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)]. E-mail: wender@lanl.gov; Vieira, D.J. [Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)]. E-mail: vieira@lanl.gov; Bond, E.M. [Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)]. E-mail: bond@lanl.gov; Bredeweg, T.A. [Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)]. E-mail: toddb@lanl.gov; Wilhelmy, J.B. [Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)]. E-mail: j_wilhelmy@lanl.gov; Granier, T. [Commissariat a l' Energie Atomique, 91680 Bruyeres-le-Chatel (France)]. E-mail: granier@cea.fr; Ethvignot, T. [Commissariat a l' Energie Atomique, 91680 Bruyeres-le-Chatel (France)]. E-mail: ethvignot@cea.fr; Petit, M. [Commissariat a l' Energie Atomique, 91680 Bruyeres-le-Chatel (France)]. E-mail: petit@cea.fr; Danon, Y. [Rensselaer Polytechnic Institute, Troy, NY 12180 (United States)]. E-mail: danony@rpi.edu; Romano, C. [Rensselaer Polytechnic Institute, Troy, NY 12180 (United States)]. E-mail: romanc2@rpi.edu

    2006-08-01

    We present fission cross-section measurements with {approx}10ng of {sup 239}Pu performed using the LANSCE Lead Slowing-Down Spectrometer. Results of Li6(n,{alpha}) measurements with a sample size of 760ng of {sup 6}Li are also reported. This technical achievement demonstrates the feasibility of measuring neutron-induced fission cross-section on samples with 10ng of fissile actinides that are available on ultra-small quantities. Furthermore, results on neutron-induced alpha emission show that measurements for astrophysics purposes are feasible with the LSDS.

  17. Cross-section measurements for 239Pu(n,f) and 6Li(n, α) with a lead slowing-down spectrometer

    Science.gov (United States)

    Rochman, D.; Haight, R. C.; O'Donnell, J. M.; Wender, S. A.; Vieira, D. J.; Bond, E. M.; Bredeweg, T. A.; Wilhelmy, J. B.; Granier, T.; Ethvignot, T.; Petit, M.; Danon, Y.; Romano, C.

    2006-08-01

    We present fission cross-section measurements with ˜10 ng of 239Pu performed using the LANSCE Lead Slowing-Down Spectrometer. Results of Li6(n,α) measurements with a sample size of 760 ng of 6Li are also reported. This technical achievement demonstrates the feasibility of measuring neutron-induced fission cross-section on samples with 10 ng of fissile actinides that are available on ultra-small quantities. Furthermore, results on neutron-induced alpha emission show that measurements for astrophysics purposes are feasible with the LSDS.

  18. Search for $^6_\\Lambda$H hypernucleus by the $^6$Li$(\\pi^-,K^+)$ reaction at $p_{\\pi^-}$ = 1.2 GeV/$c$

    CERN Document Server

    Sugimura, H; Ahn, J K; Ajimura, S; Akazawa, Y; Amano, N; Aoki, K; Bhang, H C; Chiga, N; Endo, M; Evtoukhovitch, P; Feliciello, A; Fujioka, H; Fukuda, T; Hasegawa, S; Hayakawa, S; Honda, R; Hosomi, K; Hwang, S H; Ichikawa, Y; Igarashi, Y; Imai, K; Ishibashi, N; Iwasaki, R; Joo, C W; Kiuchi, R; Lee, J K; Lee, J Y; Matsuda, K; Matsumoto, Y; Matsuoka, K; Miwa, K; Mizoi, Y; Moritsu, M; Nagae, T; Nagamiya, S; Nakagawa, M; Naruki, M; Noumi, H; Ota, R; Roy, B J; Saha, P K; Sakaguchi, A; Sako, H; Samanta, C; Samoilov, V; Sasaki, Y; Sato, S; Sekimoto, M; Shimizu, Y; Shiozaki, T; Shirotori, K; Soyama, T; Takahashi, T; Takahashi, T N; Tamura, H; Tanabe, K; Tanaka, T; Tanida, K; Tokiyasu, A O; Tsamalaidze, Z; Ukai, M; Yamamoto, T O; Yamamoto, Y; Yang, S B; Yoshida, K

    2014-01-01

    We have carried out an experiment to search for a neutron-rich hypernucleus, $^6_{\\Lambda}$H, by the $^6$Li($\\pi^-,K^+$) reaction at $p_{\\pi^-}$ =1.2 GeV/$c$. The obtained missing mass spectrum with an estimated energy resolution of 3.2 MeV (FWHM) showed no peak structure corresponding to the $^6_{\\Lambda}$H hypernucleus neither below nor above the $^4_{\\Lambda}$H$+2n$ particle decay threshold. An upper limit of the production cross section for the bound $^6_{\\Lambda}$H hypernucleus was estimated to be 1.2 nb/sr at 90% confidence level.

  19. Measurements of double-differential neutron emission cross sections of {sup 6}Li and {sup 7}Li for 18 MeV neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Ibaraki, Masanobu; Baba, Mamoru; Matsuyama, Shigeo; Sanami, Toshiya; Win, T.; Miura, Takako; Hirakawa, Naohiro [Tohoku Univ., Sendai (Japan). Faculty of Engineering

    1997-03-01

    Double-differential neutron emission cross sections of {sup 6}Li and {sup 7}Li were measured for 18 MeV neutrons at Tohoku University 4.5 MV Dynamitron facility. Neutron emission spectra were obtained down to 1 MeV at 13 angles with energy resolution good enough to separate discrete levels. A care was taken to eliminate the sample-dependent background due to parasitic neutrons. Experimental results were in fair agreement with the JENDL-3.2 data and a simple model considering a three-body breakup process and discrete level excitations. (author)

  20. Digital signal processing for a thermal neutron detector using ZnS(Ag):6LiF scintillating layers read out with WLS fibers and SiPMs

    OpenAIRE

    Mosset, J. -B.; Stoykov, A.; Greuter, U.; Hildebrandt, M.; Schlumpf, N.

    2015-01-01

    We present a digital signal processing system based on a photon counting approach which we developed for a thermal neutron detector consisting of ZnS(Ag):6LiF scintillating layers read out with WLS fibers and SiPMs. Three digital filters have been evaluated: a moving sum, a moving sum after differentiation and a digital CR-RC^4 filter. The performances of the detector with these filters are presented. A full analog signal processing using a CR-RC^4 filter has been emulated digitally. The dete...

  1. Digital signal processing for a thermal neutron detector using ZnS(Ag):6LiF scintillating layers read out with WLS fibers and SiPMs

    Science.gov (United States)

    Mosset, J.-B.; Stoykov, A.; Greuter, U.; Hildebrandt, M.; Schlumpf, N.

    2016-07-01

    We present a digital signal processing system based on a photon counting approach which we developed for a thermal neutron detector consisting of ZnS(Ag):6LiF scintillating layers read out with WLS fibers and SiPMs. Three digital filters have been evaluated: a moving sum, a moving sum after differentiation and a digital CR-RC4 filter. The performances of the detector with these filters are presented. A full analog signal processing using a CR-RC4 filter has been emulated digitally. The detector performance obtained with this analog approach is compared with the one obtained with the best performing digital approach.

  2. Digital signal processing for a thermal neutron detector using ZnS(Ag):6LiF scintillating layers read out with WLS fibers and SiPMs

    CERN Document Server

    Mosset, J -B; Greuter, U; Hildebrandt, M; Schlumpf, N

    2015-01-01

    We present a digital signal processing system based on a photon counting approach which we developed for a thermal neutron detector consisting of ZnS(Ag):6LiF scintillating layers read out with WLS fibers and SiPMs. Three digital filters have been evaluated: a moving sum, a moving sum after differentiation and a digital CR-RC^4 filter. The performances of the detector with these filters are presented. A full analog signal processing using a CR-RC^4 filter has been emulated digitally. The detector performance obtained with this analog approach is compared with the one obtained with the best performing digital approach.

  3. Study of Conformation and Dynamics of Molecules Adsorbed in Zeolites by 1H NMR

    Science.gov (United States)

    Michel, Dieter; Bohlmann, Winfried; Roland, Jorg; Mulla-Osman, Samir

    The chapter Study of Conformation and Dynamics of Molecules Adsorbed in Zeolites by 1H NMR is concerned with the application of high-resolution (HR) solid-state NMR techniques to study the behavior of molecules adsorbed on surfaces of nanoporous solids, such as zeolitic molecular sieves. This includes a combined or alternative application of conventional high-resolution NMR methods and of high-resolution solid-state NMR techniques, including magic-angle sample spinning (MAS), cross-polarization (CP), high-power decoupling and appropriate multiple-pulse sequences for two- or higher dimensional NMR and multiple-quantum spectroscopy. The interaction of adsorbed molecules with adsorption centers in the internal surfaces of porous solids does not only lead to changes in the reorientational and translational mobility of the molecular species but influences also the molecular conformation. Examples will be given for simple olefins in interaction with inner zeolite surfaces. Conclusions about the correlation times of the internal reorientational and translational dynamics are derived in complete agreement with the conclusion obtained from diffusion coefficients by means of PFG NMR (second chapter). Since the methodical approach of HR MAS NMR in heterogeneous systems presented here is also valuable for the investigation of lyotropic crystalline phases using HR MAS NMR (in Chap. 12) And for the NMR studies of cartilage (in Chap. 13) it was also the aim of this chapter to elucidate also the methodical background of these measurements in some more detail.

  4. In situ solid-state NMR for heterogeneous catalysis: a joint experimental and theoretical approach.

    Science.gov (United States)

    Zhang, Weiping; Xu, Shutao; Han, Xiuwen; Bao, Xinhe

    2012-01-07

    In situ solid-state NMR is a well-established tool for investigations of the structures of the adsorbed reactants, intermediates and products on the surface of solid catalysts. The techniques allow identifications of both the active sites such as acidic sites and reaction processes after introduction of adsorbates and reactants inside an NMR rotor under magic angle spinning (MAS). The in situ solid-state NMR studies of the reactions can be achieved in two ways, i.e. under batch-like or continuous-flow conditions. The former technique is low cost and accessible to the commercial instrument while the latter one is close to the real catalytic reactions on the solids. This critical review describes the research progress on the in situ solid-state NMR techniques and the applications in heterogeneous catalysis under batch-like and continuous-flow conditions in recent years. Some typical probe molecules are summarized here to detect the Brønsted and Lewis acidic sites by MAS NMR. The catalytic reactions discussed in this review include methane aromatization, olefin selective oxidation and olefin metathesis on the metal oxide-containing zeolites. With combining the in situ MAS NMR spectroscopy and the density functional theoretical (DFT) calculations, the intermediates on the catalyst can be identified, and the reaction mechanism is revealed. Reaction kinetic analysis in the nanospace instead of in the bulk state can also be performed by employing laser-enhanced MAS NMR techniques in the in situ flow mode (163 references).

  5. Studies of minute quantities of natural abundance molecules using 2D heteronuclear correlation spectroscopy under 100 kHz MAS.

    Science.gov (United States)

    Nishiyama, Y; Kobayashi, T; Malon, M; Singappuli-Arachchige, D; Slowing, I I; Pruski, M

    2015-01-01

    Two-dimensional (1)H{(13)C} heteronuclear correlation solid-state NMR spectra of naturally abundant solid materials are presented, acquired using the 0.75-mm magic angle spinning (MAS) probe at spinning rates up to 100 kHz. In spite of the miniscule sample volume (290 nL), high-quality HSQC-type spectra of bulk samples as well as surface-bound molecules can be obtained within hours of experimental time. The experiments are compared with those carried out at 40 kHz MAS using a 1.6-mm probe, which offered higher overall sensitivity due to a larger rotor volume. The benefits of ultrafast MAS in such experiments include superior resolution in (1)H dimension without resorting to (1)H-(1)H homonuclear RF decoupling, easy optimization, and applicability to mass-limited samples. The HMQC spectra of surface-bound species can be also acquired under 100 kHz MAS, although the dephasing of transverse magnetization has significant effect on the efficiency transfer under MAS alone. Published by Elsevier Inc.

  6. Measurement of differential cross sections and cross sections of the 6Li(n, t)4He reaction in the 1-2MeV energy range%1-2 MeV能区6Li(n,t)4He反应微分截面与截面的实验测量

    Institute of Scientific and Technical Information of China (English)

    张国辉; 陈金象; 唐国有; Gledenov Yu M; Sedysheva M; Khuukhenkhuu G

    2006-01-01

    利用屏栅电离室对1.05、1.54及2.25 MeV中子6Li(n,t)4He反应的微分截面与截面进行了实验测量.采用氚固体靶的T(p,n)3He反应产生准单能中子,用相对效率已知的BF3长中子管和238U裂变片相结合来测定绝对中子通量.将测量结果与已有数据进行了比较,1-2 MeV能区6Li(n,t)4He反应截面的分歧在一定程度上得到了澄清.

  7. Simultaneous sub-Doppler laser cooling of fermionic $^6$Li and $^{40}$K on the D$_1$ line: Theory and Experiment

    CERN Document Server

    Sievers, Franz; Kretzschmar, Norman; Fernandes, Diogo Rio; Suchet, Daniel; Rabinovic, Michael; Parker, Colin V; Khaykovich, Lev; Salomon, Christophe; Chevy, Frédéric

    2014-01-01

    We report on simultaneous sub-Doppler laser cooling of fermionic $^6$Li and $^{40}$K using the D$_1$ optical transitions. We compare experimental results to a numerical simulation of the cooling process applying a semi-classical Monte Carlo wavefunction method. The simulation takes into account the three dimensional optical molasses setup and the dipole interaction between atoms and the bichromatic light field driving the D$_1$ transitions. We discuss the physical mechanisms at play, we identify the important role of coherences between the ground state hyperfine levels and compare D$_1$ and D$_2$ sub-Doppler cooling. In 5 ms, the D$_1$ molasses phase largely reduces the temperature for both $^6$Li and $^{40}$K at the same time, with a final temperature of 44 $\\mu$K and 11 $\\mu$K, respectively. For both species this leads to a phase-space density close to $10^{-4}$. These conditions are well suited to directly load an optical or magnetic trap for efficient evaporative cooling to quantum degeneracy.

  8. Parsec-scale Variations in the 7Li i/6Li i Isotope Ratio Toward IC 348 and the Perseus OB 2 Association

    Science.gov (United States)

    Knauth, D. C.; Taylor, C. J.; Ritchey, A. M.; Federman, S. R.; Lambert, D. L.

    2017-01-01

    Measurements of the lithium isotopic ratio in the diffuse interstellar medium from high-resolution spectra of the Li i λ6708 resonance doublet have now been reported for a number of lines of sight. The majority of the results for the 7Li/6Li ratio are similar to the solar system ratio of 12.2, but the line of sight toward o Per, a star near the star-forming region IC 348, gave a ratio of about two, the expected value for gas exposed to spallation and fusion reactions driven by cosmic rays. To examine the association of IC 348 with cosmic rays more closely, we measured the lithium isotopic ratio for lines of sight to three stars within a few parsecs of o Per. One star, HD 281159, has 7Li/6Li ≃ 2 confirming production by cosmic rays. The lithium isotopic ratio toward o Per and HD 281159 together with published analyses of the chemistry of interstellar diatomic molecules suggest that the superbubble surrounding IC 348 is the source of the cosmic rays. Based on observations obtained with the Hobby-Eberly Telescope, which is a joint project of the University of Texas at Austin, the Pennsylvania State University, Ludwig-Maximilians-Universität München, and Georg-August-Universität Göttingen.

  9. An ultracold neutron (UCN) detector with Ti/ sup 6 LiF multi-layer converter and sup 5 sup 8 Ni reflector

    CERN Document Server

    Maier-Komor, P; Bergmaier, A; Dollinger, G; Paul, S; Petzoldt, G; Schott, W

    2002-01-01

    High efficient detectors for ultracold neutrons (UCN) must be developed for the new high flux neutron source Forschungsreaktor Muenchen II (FRM II). On silicon PIN diodes 76 mu g/cm sup 2 sup 5 sup 8 Ni was deposited as a UCN reflector. On this 100 double layers of sup n sup a sup t Ti (4.7 mu g/cm sup 2) and sup 6 LiF (1.8 mu g/cm sup 2) were deposited to function as a UCN converter. On top of this, 33 double layers of sup n sup a sup t Ti (3.4 mu g/cm sup 2) and sup 6 LiF (0.92 mu g/cm sup 2) were condensed in addition to provide sensitivity to very low-energy UCN. Finally, 6.0 mu g/cm sup 2 sup n sup a sup t V was deposited to protect the multi-layers. Vanadium has nearly zero optical potential for UCN and thus should not hinder their transmission. Since no expensive isotopes were involved, a source to substrate distance of 24 cm could be chosen, leading to excellent uniformity. The setup designed for deposition under ultrahigh vacuum conditions and the evaporation procedures are described.

  10. Simultaneous measurement of angular distribution of elastic scattering for {sup 6}Li, {sup 7}Be, and {sup 8}B in {sup 58}Ni; Medida simultanea de Distribuciones Angulares de Dispersion Elastica para {sup 6}Li, {sup 7}Be, y {sup 8}B en {sup 58}Ni

    Energy Technology Data Exchange (ETDEWEB)

    Ruiz S, A. [Facultad de Ciencias, UAEM, Toluca, Estado de Mexico (Mexico); Martinez Q, E.; Aguilera R, E.F.; Murillo O, G.; Lizcano C, D.; Gomez C, A. [Departamento de Aceleradores, ININ, 52750 La Marquesa, Estado de Mexico (Mexico)

    2007-07-01

    The experimental angular distributions of elastic scattering for the projectiles {sup 6}Li, {sup 7}Be, {sup 8}B in {sup 58}Ni were obtained. Using the Optical model with a Woods-Saxon potential form, as much for the real part as for the imaginary one, an adjustment to the experimental data varying only the depth of the imaginary part of the potential is made. A comparison of the results obtained for each projectile is made. (Author)

  11. Structural Investigations of Portland Cement Components, Hydration, and Effects of Admixtures by Solid-State NMR Spectroscopy

    DEFF Research Database (Denmark)

    Skibsted, Jørgen Bengaard; Andersen, Morten D.; Jakobsen, Hans Jørgen

    2006-01-01

    Solid-state, magic-angle spinning (MAS) NMR spectroscopy represents a valuable tool for structural investigations on the nanoscale of the most important phases in anhydrous and hydrated Portland cements and of various admixtures. This is primarily due to the fact that the method reflects the first...... in the cement phases. The role of flouride ions is of special interest for mineralized Portland cements and it demonstrated that the location of these anions in anhydrous and hydrated Portland cements can be clarified using 19F MAS or 29Si{19F} CP/MAS NMR despite these cements contain only about 0.2 wt...

  12. NMR Studies of Cartilage Dynamics, Diffusion, Degradation

    Science.gov (United States)

    Huster, Daniel; Schiller, Jurgen; Naji, Lama; Kaufmann Jorn; Arnold, Klaus

    An increasing number of people is suffering from rheumatic diseases, and, therefore, methods of early diagnosis of joint degeneration are urgently required. For their establishment, however, an improved knowledge about the molecular organisation of cartilage would be helpful. Cartilage consists of three main components: Water, collagen and chondroitin sulfate (CS) that is (together with further polysaccharides and proteins) a major constituent of the proteoglycans of cartilage. 1H and 13C MAS (magic-angle spinning) NMR (nuclear magnetic resonance) opened new perspectives for the study of the macromolecular components in cartilage. We have primarily studied the mobilities of CS and collagen in bovine nasal and pig articular cartilage (that differ significantly in their collagen/polysaccharide content) by measuring 13C NMR relaxation times as well as the corresponding 13C CP (cross polarisation) MAS NMR spectra. These data clearly indicate that the mobility of cartilage macromolecules is broadly distributed from almost completely rigid (collagen) to highly mobile (polysaccharides), which lends cartilage its mechanical strength and shock-absorbing properties.

  13. Rapid proton-detected NMR assignment for proteins with fast magic angle spinning.

    Science.gov (United States)

    Barbet-Massin, Emeline; Pell, Andrew J; Retel, Joren S; Andreas, Loren B; Jaudzems, Kristaps; Franks, W Trent; Nieuwkoop, Andrew J; Hiller, Matthias; Higman, Victoria; Guerry, Paul; Bertarello, Andrea; Knight, Michael J; Felletti, Michele; Le Marchand, Tanguy; Kotelovica, Svetlana; Akopjana, Inara; Tars, Kaspars; Stoppini, Monica; Bellotti, Vittorio; Bolognesi, Martino; Ricagno, Stefano; Chou, James J; Griffin, Robert G; Oschkinat, Hartmut; Lesage, Anne; Emsley, Lyndon; Herrmann, Torsten; Pintacuda, Guido

    2014-09-03

    Using a set of six (1)H-detected triple-resonance NMR experiments, we establish a method for sequence-specific backbone resonance assignment of magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectra of 5-30 kDa proteins. The approach relies on perdeuteration, amide (2)H/(1)H exchange, high magnetic fields, and high-spinning frequencies (ωr/2π ≥ 60 kHz) and yields high-quality NMR data, enabling the use of automated analysis. The method is validated with five examples of proteins in different condensed states, including two microcrystalline proteins, a sedimented virus capsid, and two membrane-embedded systems. In comparison to contemporary (13)C/(15)N-based methods, this approach facilitates and accelerates the MAS NMR assignment process, shortening the spectral acquisition times and enabling the use of unsupervised state-of-the-art computational data analysis protocols originally developed for solution NMR.

  14. Analysis of organic matter at the soil-water interface by NMR spectroscopy: Implications for contaminant sorption processes

    Science.gov (United States)

    Simpson, M.; Simpson, A.

    2009-05-01

    Contaminant sorption to soil organic matter (OM) is the main fate of nonionic, hydrophobic organic contaminants in terrestrial environments and a number of studies have suggested that both soil OM structure and physical conformation (as regulated by the clay mineral phase) govern contaminant sorption processes. To investigate this further, a number of soil samples were characterized by both solid-state 13 C Cross Polarization Magic Angle Spinning (CPMAS) NMR and 1H High Resolution Magic Angle Spinning (HR- MAS) NMR. HR-MAS NMR is an innovative NMR method that allows one to examine samples that are semi- solid using liquid state NMR methods (ie: observe 1H which is more sensitive than 13C). With HR-MAS NMR, only those structures that are in contact with the solvent are NMR visible thus one can probe different components within a mixture using different solvents. The 1H HR-MAS NMR spectrum of a grassland soil swollen in water (D2O) is dominated by signals from alkyl and O-alkyl structures but signals from aromatic protons are negligible (the peak at ~8.2ppm is attributed to formic acid). When the soil is swollen in DMSO-d6, a solvent which is more penetrating and capable of breaking hydrogen bonds, aromatic signals are visible suggesting that the aromatic structures are buried within the soil matrix and do not exist at the soil-water interface. The 13C solid-state NMR data confirms that aromatic carbon is present in substantial amounts (estimated at ~40% of the total 13C signal) therefore, the lack of 1H aromatic signals in the HR-MAS NMR spectrum indicates that aromatic structures are buried and that the soil-water interface is dominated by aliphatic chains, carbohydrates, and peptides. The NMR data indicates that the mineral component of soils governs the physical conformation of OM at the soil-water interface.

  15. 48 CFR 538.272 - MAS price reductions.

    Science.gov (United States)

    2010-10-01

    ... 48 Federal Acquisition Regulations System 4 2010-10-01 2010-10-01 false MAS price reductions. 538.272 Section 538.272 Federal Acquisition Regulations System GENERAL SERVICES ADMINISTRATION SPECIAL... Schedules 538.272 MAS price reductions. (a) Section 552.238-75, Price Reductions, requires the contractor to...

  16. 1H MAS NMR characterization of hydrogen over silica-supported rhodium catalyst

    Institute of Scientific and Technical Information of China (English)

    CHAO; Zisheng

    2001-01-01

    [1]Xu Songling, Measurement of Economic Loss of Environment Damage in China--Example and Theory, Beijing: Envi-ronment Science Press of China, 1998, 7-9.[2]Douglas, J. M., Process synthesis for waste minimization, Ind. Eng. Chem. Res., 1992, 31(1): 238.[3]Flower, J. R., Bikos, S, C., Johnson, S. W., The graphical mass balance in the early design of clean processes, Tran. of IChE, Part B, 1993, 194.[4]EI-Hakwagi, M. M., Manousiouthakis, V., Synthesis of mass exchange networks, AIChE Jl., 1989,35(8): 1233.[5]Wang, Y. P., Smith, R., Wastewater minimization, Chem. Eng. Sci., 1994, 49(7): 881.[6]Pistikopoulos, E. N., Stefanis, S. K., Livingston, A. G., A methodology for minimum environmental impact analysis, AL-CHE Symposium Series, Volume on Pollution Prevention through Process and Product Modifications, 1994, 90(303): 139.[7]Stefanis, S. K., Livingston, A. G., Pistikopoulos, E. N., Minimizing the environmental impact of process plants: A process systems methodology, Computers and Chemical Engineering, 1996, 20: S1419.[8]Rivero, R., The Exergoecologic improvement potential of industrial processes, in Proc.of TAIES'97, Beijing: World Pub-lishing Corporation, 1997, 299-304.[9]Stefanis, S. K., Buxton, A., Livingston, A. G. et al., A methodology for environmental impact minimization: Solvent des-ign and reaction path synthesis issues, Computers and Chemical Engineering, 1997, 21: S1419.[10]Rosen, M. A., Dincer, I., On exergy and environmental impact, International Journal of Energy Research, 1997, 21: 643.[11]Wang Yanfeng, Feng Xiao, Exergy analysis involving resource utilization and environmental influence, Computers and Chemical Engineering, 2000, 24: 1243.[12]Wang Jing,He Deke,Wang Yaoqu, The Handbook of Assessment Environment Data--Toxic Substance Identification Data, Beijing: Chemical Industry Press, 1988, 424-426.[13]Xiang Xinyao, Exergy Analysis Method in Engineering (in Chinese), Beijing: Petroleum Industry Press,1990, 313-314.[14]The Laws Assembly of Pollute Penalty (1982-1996), Xi'an: Environment Supervision and Control Office in Xi'an City, 1997, 199-208.[15]Sahaku, Y., Closed System of Chemical Production (in Chinese), (translated by Yu Puyi, An Jiaju, Liu Renkan), Beijing: Chemical Industry Press, 1987, 43-58

  17. Quantitative analysis of backbone motion in proteins using MAS solid-state NMR spectroscopy.

    Science.gov (United States)

    Chevelkov, Veniamin; Fink, Uwe; Reif, Bernd

    2009-09-01

    We present a comprehensive analysis of protein dynamics for a micro-crystallin protein in the solid-state. Experimental data include (15)N T (1) relaxation times measured at two different magnetic fields as well as (1)H-(15)N dipole, (15)N CSA cross correlated relaxation rates which are sensitive to the spectral density function J(0) and are thus a measure of T (2) in the solid-state. In addition, global order parameters are included from a (1)H,(15)N dipolar recoupling experiment. The data are analyzed within the framework of the extended model-free Clore-Lipari-Szabo theory. We find slow motional correlation times in the range of 5 and 150 ns. Assuming a wobbling in a cone motion, the amplitude of motion of the respective amide moiety is on the order of 10 degrees for the half-opening angle of the cone in most of the cases. The experiments are demonstrated using a perdeuterated sample of the chicken alpha-spectrin SH3 domain.

  18. Ammonia Vapor Removal by Cu3(BTC)2 and Its Characterization by MAS NMR

    Science.gov (United States)

    2009-01-01

    hysteresis . A majority of the nitrogen is adsorbed at relative pressures less than 10-3. Molecular simulations of Ar adsorption isotherm data on similar Cu...created by the unsaturated copper atoms. The hysteresis loop at relative pressures above 0.4 corre- sponds to previous argon adsorption studies by...Vishnayakov and co-workers and is indicative of mesoporous defects formed during crystallization.15 The exhausted samples exposed to ammonia under dry and 80

  19. Angular Distribution and Cross Section Measurement of the 6Li(3He,n8B Reaction at 5.8 MeV

    Directory of Open Access Journals (Sweden)

    Cinausero M.

    2014-03-01

    Full Text Available The reaction 6Li(3He,n8B was studied at Laboratori Nazionali di Legnaro in the framework of the EUROnu Design Study for a Beta Beam facility at CERN. The 8B production cross section was determined through neutron angular distribution by using the time-of-flight technique. Thanks to the high statistics achieved, the neutron angular distribution for the population of the 8B first excited state has been measured for the first time. Discrepancies with other available data sets for 8B ground state population are discussed and interpreted in the framework of DWBA calculations. Further measurements at beam energies above 10 MeV are needed to clarify the behaviour of the angular distribution

  20. Two-stage magneto-optical trapping and narrow-line cooling of $^6$Li atoms to high phase-space density

    CERN Document Server

    Sebastian, Jimmy; Li, Ke; Gan, Huat Chai Jaren; Li, Wenhui; Dieckmann, Kai

    2014-01-01

    We report an experimental study of peak and phase-space density of a two-stage magneto-optical trap (MOT) of 6-Li atoms, which exploits the narrower $2S_{1/2}\\rightarrow 3P_{3/2}$ ultra-violet (UV) transition at 323 nm following trapping and cooling on the more common D2 transition at 671 nm. The UV MOT is loaded from a red MOT and is compressed to give a high phase-space density up to $3\\times 10^{-4}$. Temperatures as low as 33 $\\mu$K are achieved on the UV transition. We study the density limiting factors and in particular find a value for the light-assisted collisional loss coefficient of $1.3 \\pm0.4\\times10^{-10}\\,\\textrm{cm}^3/\\textrm{s}$ for low repumping intensity.

  1. Microscopic Model Analysis of the $^{6}He,^{6}Li$ + $^{28}Si$ Total Reaction Cross Sections at the Energy Range 5-50 a Mev

    CERN Document Server

    Lukyanov, K V; Lukyanov, V K; Penionzhkevich, Yu E; Sobolev, Y G; Zemlyanaya, E V; Penionzhkevich, Yu.E.; Sobolev, Yu.G.

    2007-01-01

    The existing and some preliminary experimental data on the total cross sections of the $^{4,6}$He, $^{6,7}$Li +$^{28}$Si reactions at energies E=5-50 A MeV are demonstrated. The data on $^{6}$Li,$^{6}$He+$^{28}$Si are analyzed in the framework of the microscopic optical potential with real and imaginary parts obtained with a help of the double-folding procedure and by using the current models of densities of the projectile nuclei. Besides, the microscopic double-folding Coulomb potential is calculated and its effect on cross sections is compared with that when one applies the traditional Coulomb potential of the uniform charge distribution. The semi-microscopic potentials are constructed from both the renormalized microscopic potentials and their derivatives to take into account collective motion effect and to improve an agreement with experimental data.

  2. Detector for the FSD Fourier-Diffractometer Based on ZnS(Ag)/^{6}LiF Scintillation Screen and Wavelength Shifting Fibers Readout

    CERN Document Server

    Kuzmin, E S; Bokuchava, G D; Zhuk, V V; Kudryashov, V A; Buklin, A P; Trounov, V A

    2001-01-01

    At the IBR-2 pulsed reactor (FLNP, JINR, Dubna), a specialized time-of-flight instrument Fourier-Stress-Diffractometer (FSD) intended for the measurement of internal steresses in bulk samples by using high-resolution neutron diffraction is under construction. One of the main components of the diffractometer is a new-type detector with combined electronic - geometrical focusing uniting a large solid angle and a small geometry contribution to the instrumental resolution. The first two modules of the detector, based on scintillation screen ZnS(Ag)/^{6}LiF with wavelength shifting fibers readout have been developed and tested. The design of the detector and associated electronics are described. The method of time focusing surface approximation, using the screen flexibility is proposed. Characteristics of tested modules in comparison with a detector of previous generation are presented and advantages of new detector design for high-resolution diffractometry are discussed.

  3. Complete protocol for slow-spinning high-resolution magic-angle spinning NMR analysis of fragile tissues.

    Science.gov (United States)

    André, Marion; Dumez, Jean-Nicolas; Rezig, Lamya; Shintu, Laetitia; Piotto, Martial; Caldarelli, Stefano

    2014-11-04

    High-resolution magic-angle spinning (HR-MAS) nuclear magnetic resonance (NMR) is an essential tool to characterize a variety of semisolid systems, including biological tissues, with virtually no sample preparation. The "non-destructive" nature of NMR is typically compromised, however, by the extreme centrifugal forces experienced under conventional HR-MAS frequencies of several kilohertz. These features limit the usefulness of current HR-MAS approaches for fragile samples. Here, we introduce a full protocol for acquiring high-quality HR-MAS NMR spectra of biological tissues at low spinning rates (down to a few hundred hertz). The protocol first consists of a carefully designed sample preparation, which yields spectra without significant spinning sidebands at low spinning frequency for several types of sample holders, including the standard disposable inserts classically used in HR-MAS NMR-based metabolomics. Suppression of broad spectral features is then achieved using a modified version of the recently introduced PROJECT experiment with added water suppression and rotor synchronization, which deposits limited power in the sample and which can be suitably rotor-synchronized at low spinning rates. The performance of the slow HR-MAS NMR procedure is demonstrated on conventional (liver tissue) and very delicate (fish eggs) samples, for which the slow-spinning conditions are shown to preserve the structural integrity and to minimize intercompartmental leaks of metabolites. Taken together, these results expand the applicability and reliability of HR-MAS NMR spectroscopy. These results have been obtained at 400 and 600 MHz and suggest that high-quality slow HR-MAS spectra can be expected at higher magnetic fields using the described protocol.

  4. Combined zero-quantum and spin-diffusion mixing for efficient homonuclear correlation spectroscopy under fast MAS: broadband recoupling and detection of long-range correlations.

    Science.gov (United States)

    Lu, Xingyu; Guo, Changmiao; Hou, Guangjin; Polenova, Tatyana

    2015-01-01

    Fast magic angle spinning (MAS) NMR spectroscopy is emerging as an essential analytical and structural biology technique. Large resolution and sensitivity enhancements observed under fast MAS conditions enable structural and dynamics analysis of challenging systems, such as large macromolecular assemblies and isotopically dilute samples, using only a fraction of material required for conventional experiments. Homonuclear dipolar-based correlation spectroscopy constitutes a centerpiece in the MAS NMR methodological toolbox, and is used essentially in every biological and organic system for deriving resonance assignments and distance restraints information necessary for structural analysis. Under fast MAS conditions (rotation frequencies above 35-40 kHz), dipolar-based techniques that yield multi-bond correlations and non-trivial distance information are ineffective and suffer from low polarization transfer efficiency. To overcome this limitation, we have developed a family of experiments, CORD-RFDR. These experiments exploit the advantages of both zero-quantum RFDR and spin-diffusion based CORD methods, and exhibit highly efficient and broadband dipolar recoupling across the entire spectrum, for both short-range and long-range correlations. We have verified the performance of the CORD-RFDR sequences experimentally on a U-(13)C,(15)N-MLF tripeptide and by numerical simulations. We demonstrate applications of 2D CORD-RFDR correlation spectroscopy in dynein light chain LC8 and HIV-1 CA tubular assemblies. In the CORD-RFDR spectra of LC8 acquired at the MAS frequency of 40 kHz, many new intra- and inter-residue correlations are detected, which were not observed with conventional dipolar recoupling sequences. At a moderate MAS frequency of 14 kHz, the CORD-RFDR experiment exhibits excellent performance as well, as demonstrated in the HIV-1 CA tubular assemblies. Taken together, the results indicate that CORD-RFDR experiment is beneficial in a broad range of conditions

  5. Optimization of dental CBCT exposures through mAs reduction.

    Science.gov (United States)

    Pauwels, R; Seynaeve, L; Henriques, J C G; de Oliveira-Santos, C; Souza, P C; Westphalen, F H; Rubira-Bullen, I R F; Ribeiro-Rotta, R F; Rockenbach, M I B; Haiter-Neto, F; Pittayapat, P; Bosmans, H; Bogaerts, R; Jacobs, R

    2015-01-01

    To investigate the effect of tube current-exposure time (mAs) reduction on clinical and technical image quality for different CBCT scanners, and to determine preliminary minimally acceptable values for the mAs and contrast-to-noise ratio (CNR) in CBCT. A polymethyl methacrylate (PMMA) phantom and an anthropomorphic skull phantom, containing a human skeleton embedded in polyurethane, were scanned using four CBCT devices, including seven exposure protocols. For all protocols, the mAs was varied within the selectable range. Using the PMMA phantom, the CNRAIR was measured and corrected for voxel size. Eight axial slices and one coronal slice showing various anatomical landmarks were selected for each CBCT scan of the skull phantom. The slices were presented to six dentomaxillofacial radiologists, providing scores for various anatomical and diagnostic parameters. A hyperbolic relationship was seen between CNRAIR and mAs. Similarly, a gradual reduction in clinical image quality was seen at lower mAs values; however, for several protocols, image quality remained acceptable for a moderate or large mAs reduction compared with the standard exposure setting, depending on the clinical application. The relationship between mAs, CNRAIR and observer scores was different for each CBCT device. Minimally acceptable values for mAs were between 9 and 70, depending on the criterion and clinical application. Although noise increased at a lower mAs, clinical image quality often remained acceptable at exposure levels below the manufacturer's recommended setting, for certain patient groups. Currently, it is not possible to determine minimally acceptable values for image quality that are applicable to multiple CBCT models.

  6. Multinuclear solid-state high-resolution and C-13 -{Al-27} double-resonance magic-angle spinning NMR studies on aluminum alkoxides

    NARCIS (Netherlands)

    Abraham, A.; Prins, R.; Bokhoven, J.A. van; Eck, E.R.H. van; Kentgens, A.P.M.

    2006-01-01

    A combination of Al-27 magic-angle spinning (MAS)/multiple quantum (MQ)-MAS, C-13-H-1 CPMAS, and C-13-{Al-27} transfer of population in double-resonance (TRAPDOR) nuclear magnetic resonance (NMR) were used for the structural elucidation of the aluminum alkoxides aluminum ethoxide, aluminum

  7. Advanced solid-state NMR spectroscopy of natural organic matter.

    Science.gov (United States)

    Mao, Jingdong; Cao, Xiaoyan; Olk, Dan C; Chu, Wenying; Schmidt-Rohr, Klaus

    2017-05-01

    Solid-state NMR is essential for the characterization of natural organic matter (NOM) and is gaining importance in geosciences and environmental sciences. This review is intended to highlight advanced solid-state NMR techniques, especially a systematic approach to NOM characterization, and their applications to the study of NOM. We discuss some basics of how to acquire high-quality and quantitative solid-state (13)C NMR spectra, and address some common technical mistakes that lead to unreliable spectra of NOM. The identification of specific functional groups in NOM, primarily based on (13)C spectral-editing techniques, is described and the theoretical background of some recently-developed spectral-editing techniques is provided. Applications of solid-state NMR to investigating nitrogen (N) in NOM are described, focusing on limitations of the widely used (15)N CP/MAS experiment and the potential of improved advanced NMR techniques for characterizing N forms in NOM. Then techniques used for identifying proximities, heterogeneities and domains are reviewed, and some examples provided. In addition, NMR techniques for studying segmental dynamics in NOM are reviewed. We also briefly discuss applications of solid-state NMR to NOM from various sources, including soil organic matter, aquatic organic matter, organic matter in atmospheric particulate matter, carbonaceous meteoritic organic matter, and fossil fuels. Finally, examples of NMR-based structural models and an outlook are provided. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. A Construction Way of MAS Based on Organization Theory

    Institute of Scientific and Technical Information of China (English)

    GAO Bo; FEI Qi; CHEN Xue-guang

    2002-01-01

    With emphasizing that the integration of autonomy and coordination is the basis for constructing multi-agent systems (MAS), we analyze the organizational characters inherent with MAS and point out that it's a natural and essential way to construct MAS based on organization theory. We consider that the emphasis of the theory is the process of system analyzing. Then we present an analysis frame to expound the process, which includes the process of organization definition, the process of role definition, the process of organizational structure definition and the process of interaction protocol definition. Lastly, we discuss some issues associated with the processes of system design and implementation.

  9. Prediction of recrystallization behavior of troglitazone/polyvinylpyrrolidone solid dispersion by solid-state NMR.

    Science.gov (United States)

    Ito, Atsutoshi; Watanabe, Tomoyuki; Yada, Shuichi; Hamaura, Takeshi; Nakagami, Hiroaki; Higashi, Kenjirou; Moribe, Kunikazu; Yamamoto, Keiji

    2010-01-04

    The purpose of this study was to elaborate the relationship between the (13)C CP/MAS NMR spectra and the recrystallization behavior during the storage of troglitazone solid dispersions. The solid dispersions were prepared by either the solvent method or by co-grinding. The recrystallization behavior under storage conditions at 40 degrees C/94% RH was evaluated by the Kolmogorov-Johnson-Mehl-Avrami (KJMA) equation. Solid dispersions prepared by the solvent method or by prolonged grinding brought about inhibition of the nucleation and the nuclei growth at the same time. No differences in the PXRD profiles were found in the samples prepared by the co-grinding and solvent methods, however, (13)C CP/MAS NMR showed significant differences in the spectra. The correlation coefficients using partial least square regression analysis between the PXRD profiles and the apparent nuclei-growth constant or induction period to nucleation were 0.1305 or 0.6350, respectively. In contrast, those between the (13)C CP/MAS NMR spectra and the constant or the period were 0.9916 or 0.9838, respectively. The (13)C CP/MAS NMR spectra had good correlation with the recrystallization kinetic parameters evaluated by the KJMA equation. Consequently, solid-state NMR was judged to be a useful tool for the prediction of the recrystallization behavior of solid dispersions.

  10. Endothelin-1 downregulates Mas receptor expression in human cardiomyocytes.

    Science.gov (United States)

    Chen, Zhiheng; Tang, Yamei; Yang, Zuocheng; Liu, Shaojun; Liu, Yong; Li, Yan; He, Wei

    2013-09-01

    Endothelin-1 (ET-1) and the renin-angiotensin system (RAS) are involved in the pathogenesis of cardiac dysfunction. The Mas receptor is a functional binding site for angiotensin (Ang)‑(1-7), which is now considered a critical component of the RAS and exerts cardioprotective effects. To the best of our knowledge, the present study aimed to examine, for the first time, the effects of ET-1 on Mas expression in cultured human cardiomyocytes. Human cardiomyocytes were treated with ET-1 at different concentrations (1, 5, 10, 20 and 30 nM) for varied time periods (0.5, 1.5, 3, 4.5 or 6 h) with or without the transcription inhibitor actinomycin D, endothelin A (ETA) receptor blocker BQ123 and ETB receptor blocker BQ788, or different kinase inhibitors. ET-1 decreased the Mas mRNA level in a statistically significant dose- and time-dependent manner within 4.5 h, which was reflected in the dose-dependent downregulation of Mas promoter activity, Mas protein levels and Ang-(1-7) binding on the cell membrane. Actinomycin D (1 mg/ml), BQ123 (1 µM), p38 mitogen-activated protein kinase (MAPK) siRNA and inhibitor PD169316 (25 µM), completely eliminated the inhibitory effects of ET-1 on Mas expression in human cardiomyocytes. In conclusion, the present study demonstrated that ET-1 downregulates Mas expression at the transcription level in human cardiomyocytes via the ETA receptor by a p38 MAPK‑dependent mechanism. This study provides novel insights into the function of ET-1 and the Ang‑(1-7)/Mas axis in cardiac pathophysiology.

  11. NMR of lignins

    Science.gov (United States)

    John Ralph; Larry L. Landucci

    2010-01-01

    This chapter will consider the basic aspects and findings of several forms of NMR spectroscopy, including separate discussions of proton, carbon, heteronuclear, and multidimensional NMR. Enhanced focus will be on 13C NMR, because of its qualitative and quantitative importance, followed by NMR’s contributions to our understanding of lignin...

  12. Magnetic signature of charge ordering in Li[Mn sub 1 sub . sub 9 sub 6 Li sub 0 sub . sub 0 sub 4]O sub 4 and Li sub 0 sub . sub 2 [Mn sub 1 sub . sub 9 sub 6 Li sub 0 sub . sub 0 sub 4]O sub 4

    CERN Document Server

    Verhoeven, V W J; Mulder, F M

    2002-01-01

    The stoichiometric compound LiMn sub 2 O sub 4 is known to show charge ordering with well-defined Mn sup 3 sup + and Mn sup 4 sup + sites just below room temperature (RT). Above RT the electrons are hopping rapidly between sites. For lithium-ion batteries the material Li[Mn sub 1 sub . sub 9 sub 6 Li sub 0 sub . sub 0 sub 4]O sub 4 is technologically relevant. Due to the small amount of Li on the Mn site, the low-T regular ordering of the Mn charge appears to be destroyed completely, as is evidenced by neutron diffraction in the magnetically ordered state. However, the charges are still fixed in an irregular fashion, as can also be deduced from sup 7 Li nuclear magnetic resonance measurements. In the lithium-extracted compound Li sub 0 sub . sub 2 [Mn sub 1 sub . sub 9 sub 6 Li sub 0 sub . sub 0 sub 4]O sub 4 , predominantly Mn sup 4 sup + is present. Neutron diffraction in the magnetically ordered state shows a well-defined antiferromagnetic ordering, with doubling of the unit cell in three directions. Clear...

  13. Characterization of new materials in chromatography and fuel cell development by modern NMR techniques

    OpenAIRE

    Schauff, Siri

    2007-01-01

    Phosphonic acids for high temperature fuel cell membrane materials were investigated with respect to proton mobility and transport applying solid-state NMR spectroscopy. Water uptake and its effects on anhydride formation were studied on samples that were equilibrated with saturated salt solutions. For polyvinylphosphonic acid reversible anhydride formation was found. Variable temperature 1H MAS NMR spectroscopy of three different phosphonic acids revealed single proton sites, and 1H chemical...

  14. Elastic scattering and total reaction cross sections for {sup 8}B, {sup 7}Be and {sup 6}Li + {sup 12}C systems

    Energy Technology Data Exchange (ETDEWEB)

    Zamora, J.C.; Barioni, A.; Guimaraes, V. [Universidade de Sao Paulo (USP), SP (Brazil); Paes, B.; Lubian, J. [Universidade Federal Fluminense (UFF), Niteroi, RJ (Brazil); Aguilera, E.F. [Instituto Nacional de Investigaciones Nucleares (Mexico); Kolata, J.J.; Roberts, A.L. [University of Notre Dame, Indiana (United States); Becchetti, F.D.; Villano, A.; Ojaruega, M.; Jing, H. [University of Michigan (United States)

    2011-07-01

    In this work we have measured angular distributions for the elastic scattering of {sup 8}B, {sup 7}Be and {sup 6}Li on {sup 12}C target at laboratory energies of 25.8 MeV, 18.8 MeV and 12.3 MeV, respectively. The optical model has been used for the analysis of such data using Woods-Saxon and Sao Paulo potentials. We also probed the effect of breakup on the elastic scattering of {sup 8}B+{sup 12}C as this mechanism may become important due to the low binding energy of this nucleus. This investigation was performed by means of coupled channels calculations and cluster folding potentials. This study is very interesting because there are few data on {sup 8}B elastic scattering. There are some of its elastic scattering on carbon target, but at higher energies, where it was not possible to get information on its halo peculiarities. Also, we present here the total reaction cross section obtained from the elastic scattering analysis and compared with other weakly and tightly bound projectiles on carbon target. (author)

  15. Pulse shape discrimination characteristics of stilbene crystal, pure and 6Li loaded plastic scintillators for a high resolution coded-aperture neutron imager

    Science.gov (United States)

    Cieślak, M. J.; Gamage, K. A. A.; Glover, R.

    2017-07-01

    Pulse shape discrimination performances of single stilbene crystal, pure plastic and 6Li loaded plastic scintillators have been compared. Three pulse shape discrimination algorithms have been tested for each scintillator sample, assessing their quality of neutron/gamma separation. Additionally, the digital implementation feasibility of each algorithm in a real-time embedded system was evaluated. Considering the pixelated architecture of the coded-aperture imaging system, a reliable method of simultaneous multi-channel neutron/gamma discrimination was sought, accounting for the short data analysis window available for each individual channel. In this study, each scintillator sample was irradiated with a 252Cf neutron source and a bespoke digitiser system was used to collect the data allowing detailed offline examination of the sampled pulses. The figure-of-merit was utilised to compare the discrimination quality of the collected events with respect to various discrimination algorithms. Single stilbene crystal presents superior neutron/gamma separation performance when compared to the plastic scintillator samples.

  16. Increased vascular sympathetic modulation in mice with Mas receptor deficiency.

    Science.gov (United States)

    Rabello Casali, Karina; Ravizzoni Dartora, Daniela; Moura, Marina; Bertagnolli, Mariane; Bader, Michael; Haibara, Andrea; Alenina, Natalia; Irigoyen, Maria Claudia; Santos, Robson A

    2016-01-01

    The angiotensin-converting enzyme 2 (ACE2)/angiotensin (Ang)-(1-7)/Mas axis could modulate the heart rate (HR) and blood pressure variabilities (BPV) which are important predictors of cardiovascular risk and provide information about the autonomic modulation of the cardiovascular system. Therefore we investigated the effect of Mas deficiency on autonomic modulation in wild type and Mas-knockout (KO) mice. Blood pressure was recorded at high sample rate (4000 Hz). Stationary sequences of 200-250 beats were randomly chosen. Frequency domain analysis of HR and BPV was performed with an autoregressive algorithm on the pulse interval sequences and on respective systolic sequences. The KO group presented an increase of systolic arterial pressure (SAP; 127.26±11.20 vs 135.07±6.98 mmHg), BPV (3.54±1.54 vs 5.87±2.12 mmHg(2)), and low-frequency component of systolic BPV (0.12±0.11 vs 0.47±0.34 mmHg(2)). The deletion of Mas receptor is associated with an increase of SAP and with an increased BPV, indicating alterations in autonomic control. Increase of sympathetic vascular modulation in absence of Mas evidences the important role of Ang-(1-7)/Mas on cardiovascular regulation. Moreover, the absence of significant changes in HR and HRV can indicate an adaptation of autonomic cardiac balance. Our results suggest that the Ang-(1-7)/Mas axis seems more important in autonomic modulation of arterial pressure than HR. © The Author(s) 2016.

  17. Ca(AlH4)2, CaAlH5, and CaH2+6LiBH4: Calculated dehydrogenation enthalpy, including zero point energy, and the structure of the phonon spectra

    NARCIS (Netherlands)

    Marashdeh, A.; Frankcombe, T.J.

    2008-01-01

    The dehydrogenation enthalpies of Ca(AlH4)2, CaAlH5, and CaH2+6LiBH4 have been calculated using density functional theory calculations at the generalized gradient approximation level. Harmonic phonon zero point energy (ZPE) corrections have been included using Parlinski’s direct method. The dehydrog

  18. Solid-state NMR structures of integral membrane proteins.

    Science.gov (United States)

    Patching, Simon G

    2015-01-01

    Solid-state NMR is unique for its ability to obtain three-dimensional structures and to measure atomic-resolution structural and dynamic information for membrane proteins in native lipid bilayers. An increasing number and complexity of integral membrane protein structures have been determined by solid-state NMR using two main methods. Oriented sample solid-state NMR uses macroscopically aligned lipid bilayers to obtain orientational restraints that define secondary structure and global fold of embedded peptides and proteins and their orientation and topology in lipid bilayers. Magic angle spinning (MAS) solid-state NMR uses unoriented rapidly spinning samples to obtain distance and torsion angle restraints that define tertiary structure and helix packing arrangements. Details of all current protein structures are described, highlighting developments in experimental strategy and other technological advancements. Some structures originate from combining solid- and solution-state NMR information and some have used solid-state NMR to refine X-ray crystal structures. Solid-state NMR has also validated the structures of proteins determined in different membrane mimetics by solution-state NMR and X-ray crystallography and is therefore complementary to other structural biology techniques. By continuing efforts in identifying membrane protein targets and developing expression, isotope labelling and sample preparation strategies, probe technology, NMR experiments, calculation and modelling methods and combination with other techniques, it should be feasible to determine the structures of many more membrane proteins of biological and biomedical importance using solid-state NMR. This will provide three-dimensional structures and atomic-resolution structural information for characterising ligand and drug interactions, dynamics and molecular mechanisms of membrane proteins under physiological lipid bilayer conditions.

  19. NMR spectroscopy applied to the eye: Drugs and metabolic studies

    Energy Technology Data Exchange (ETDEWEB)

    Saether, Oddbjoern

    2005-07-01

    NMR spectroscopy has been extensively applied in biomedical research during the last decades. It has proved to be an analytical tool of great value. From being mainly used in chemistry, technological developments have expanded the application of NMR spectroscopy to a great wealth of disciplines. With this method, biochemical information can be obtained by analysing tissue extracts. Moreover, NMR spectroscopy is increasingly employed for pharmacokinetic studies and analysis of biofluids. Technological progress has provided increased sensitivity and resolution in the spectra, which enable even more of the complexity of biological samples to be elucidated. With the implementation of high-resolution magic angle spinning (HR-MAS) NMR spectroscopy in biomedicine, intact tissue samples or biopsies can be investigated. Thus, NMR spectroscopy has an ever-increasing impact in metabolic screening of human samples and in animal models, and methods are also increasingly realised in vivo. The present work, NMR spectroscopy applied to eye research, consists of two main parts. Firstly, the feasibility to monitor fluorinated ophthalmic drugs directly in the eye was assessed. Secondly, HR-MAS H1 NMR spectroscopy was applied for metabolic profiling of the anterior eye segment, specifically to analyse metabolic changes in intact corneal and lenticular samples after cataractogenic insults. This work included metabonomics with the application of pattern recognition methods to analyse HR-MAS spectra of eye tissues. Optimisation strategies were explored for F19 NMR detection of fluorinated drugs in a phantom eye. S/N gains in F19 NMR spectroscopy were achieved by implementing time-share H1 decoupling at 2.35 T. The method is advantageous for compounds displaying broad spectral coupling patterns, though detection of drugs at concentrations encountered in the anterior eye segment after topical application was not feasible. Higher magnetic fields and technological improvements could enable

  20. KINERJA USAHA TANAMAN HIAS POTONG PT PESONA DAUN MAS ASRI

    Directory of Open Access Journals (Sweden)

    Muhamad Arief Bangun Sanjaya

    2017-01-01

    Full Text Available Pesona Daun Mas Asri is a company in cut flowers  and leaves cultivation. The  achievement is shown by the performance of the company. The overall company’s performance contributes in developing the company’s vision. Balanced score card is a management tool used to observe and maintain the stability between financial indicators (financial perspective and non financial indicators (customer, business internal process, growth and learning.  The objective of the journal is to plan the performance of the company using balanced scorecard approach, analyze and calculate the vision, mission and strategy implemented by Pesona Daun Mas in it business activity..  The result for every strategic target shows that the performance of Pesona Daun Mas is excellent with the achieved score of 78,04%.  However the target for the selling growth level and marketing activities are classified as average which means that it still needs to be developed.   Keywords:  balanced scorecard, performance evaluation, KPI performance index, ornamental plants cutAbstrakPesona Daun Mas Asri merupakan perusahaan yang bergerak dalam bidang budi daya bunga potong dan daun potong. Pencapaian dalam menjalankan sebuah perusahaan dapat dilihat dari kinerja perusahaan tersebut.Kinerja perusahaan Pesona Daun Mas Asri secara keseluruhan dapat berkontribusi untuk mengembangkan perusahaan dalam mencapai visi. Balanced scorecard adalah salah satu alat manajemen yang dapat melihat dan menjaga keseimbangan antara indikator keuangan (perspektif keuangan dan indikator non-keuangan (pelanggan, proses bisnisinternal, pertumbuhan dan pembelajaran. Tujuan dari jurnal ini adalah untuk merancang pengukuran kinerja perusahaan dengan pendekatan Balanced scorecard. Penelitian ini juga bertujuan menganalisis dan mengukur pelaksanaan visi, misi dan strategi yang dijalankan oleh Pesona Daun Mas Asri dalam kegiatan bisnisnya. Selain itu, memberikan saran dan rekomendasi, serta merumuskan implikasi

  1. O sentido argumentativo do articulador mas no discurso oral

    OpenAIRE

    Nesello, Marcela Cristiane

    2008-01-01

    Esta pesquisa tem por objetivo estudar o sentido do articulador mas no discurso oral pela Teoria da Argumentação na Língua de Oswald Ducrot e colaboradores. Temos o propósito de identificar e analisar os sentidos que o articulador mas assume no discurso oral, bem como suas diferentes funções, por isso trata-se de uma pesquisa qualitativa. Também é objetivo desta pesquisa identificar os encadeamentos precedentes e subseqüentes ao articulador. Para esses fins, apresentamos estudos sobre o artic...

  2. NMR at 900 MHz

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    @@ An important factor in the development of solutionstate NMR has always been th e ability to produce stable and homogeneous magnetic fields. As higher and higher field strengths are reached the pressure is growing on manufacturers to produce NMR systems with greatly improved spectral resolution and signal to noise ratio. The introduction of the Varian 900 MHz INOVA system in August 2000 featuring Oxford Instruments 21.1 T magnet represents the latest pioneering development in NMR technology.

  3. Authenticity study of Phyllanthus species by NMR and FT-IR techniques coupled with chemometric methods

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Maiara S.; Pereira-Filho, Edenir R.; Ferreira, Antonio G. [Universidade Federal de Sao Carlos (UFSCAR), SP (Brazil). Dept. de Quimica; Boffo, Elisangela F. [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Inst. de Quimica; Figueira, Glyn M., E-mail: maiarassantos@yahoo.com.br [Universidade Estadual de Campinas (UNICAMP), Campinas, SP (Brazil). Centro Pluridisciplinar de Pesquisas Quimicas, Biologicas e Agricolas

    2012-07-01

    The importance of medicinal plants and their use in industrial applications is increasing worldwide, especially in Brazil. Phyllanthus species, popularly known as 'quebra-pedras' in Brazil, are used in folk medicine for treating urinary infections and renal calculus. This paper reports an authenticity study, based on herbal drugs from Phyllanthus species, involving commercial and authentic samples using spectroscopic techniques: FT-IR, {sup 1}H HR-MAS NMR and {sup 1}H NMR in solution, combined with chemometric analysis. The spectroscopic techniques evaluated, coupled with chemometric methods, have great potential in the investigation of complex matrices. Furthermore, several metabolites were identified by the NMR techniques. (author)

  4. Authenticity study of Phyllanthus species by NMR and FT-IR Techniques coupled with chemometric methods

    Directory of Open Access Journals (Sweden)

    Maiara S. Santos

    2012-01-01

    Full Text Available The importance of medicinal plants and their use in industrial applications is increasing worldwide, especially in Brazil. Phyllanthus species, popularly known as "quebra-pedras" in Brazil, are used in folk medicine for treating urinary infections and renal calculus. This paper reports an authenticity study, based on herbal drugs from Phyllanthus species, involving commercial and authentic samples using spectroscopic techniques: FT-IR, ¹H HR-MAS NMR and ¹H NMR in solution, combined with chemometric analysis. The spectroscopic techniques evaluated, coupled with chemometric methods, have great potential in the investigation of complex matrices. Furthermore, several metabolites were identified by the NMR techniques.

  5. The evolution of the MasAgro hubs

    NARCIS (Netherlands)

    Camacho-Villa, Tania Carolina; Almekinders, Conny; Hellin, Jon; Martinez-Cruz, Tania Eulalia; Rendon-Medel, Roberto; Guevara-Hernández, Francisco; Beuchelt, Tina D.; Govaerts, Bram

    2016-01-01

    Purpose: Little is known about effective ways to operationalize agricultural innovation processes. We use the MasAgro program in Mexico (which aims to increase maize and wheat productivity, profitability and sustainability), and the experiences of middle level ‘hub managers’, to understand how innov

  6. Angiotensin type 2 receptor (AT2R) and receptor Mas

    DEFF Research Database (Denmark)

    Villela, Daniel; Leonhardt, Julia; Patel, Neal

    2015-01-01

    The angiotensin type 2 receptor (AT2R) and the receptor Mas are components of the protective arms of the renin-angiotensin system (RAS), i.e. they both mediate tissue protective and regenerative actions. The spectrum of actions of these two receptors and their signalling mechanisms display striking...

  7. The evolution of the MasAgro hubs

    NARCIS (Netherlands)

    Camacho-Villa, Tania Carolina; Almekinders, Conny; Hellin, Jon; Martinez-Cruz, Tania Eulalia; Rendon-Medel, Roberto; Guevara-Hernández, Francisco; Beuchelt, Tina D.; Govaerts, Bram

    2016-01-01

    Purpose: Little is known about effective ways to operationalize agricultural innovation processes. We use the MasAgro program in Mexico (which aims to increase maize and wheat productivity, profitability and sustainability), and the experiences of middle level ‘hub managers’, to understand how

  8. A Vision in Jeopardy: Royal Navy Maritime Autonomous Systems (MAS)

    Science.gov (United States)

    2017-03-31

    article in The Economist, which observed that to break from the structures of Augustine’s 16th Law and unaffordable cost trends, defense needed a...52 Bibliography ...developed, not by the RN, but by the industrial and scientific research communities. Hoping to encourage the RN to invest in unmanned and MAS

  9. In Vivo Detection of the Cyclic Osmoregulated Periplasmic Glucan of Ralstonia solanacearum by High-Resolution Magic Angle Spinning NMR

    Science.gov (United States)

    Wieruszeski, J.-M.; Bohin, A.; Bohin, J.-P.; Lippens, G.

    2001-07-01

    We investigate the mobility of the osmoregulated periplasmic glucans of Ralstonia solanacearum in the bacterial periplasm through the use of high-resolution (HR) NMR spectroscopy under static and magic angle spinning (MAS) conditions. Because the nature of periplasm is far from an isotropic aqueous solution, the molecules could be freely diffusing or rather associated to a periplasmic protein, a membrane protein, a lipid, or the peptidoglycan. HR MAS NMR spectroscopy leads to more reproducible results and allows the in vivo detection and characterization of the complex molecule.

  10. Dynamics and interactions of ibuprofen in cyclodextrin nanosponges by solid-state NMR spectroscopy

    Science.gov (United States)

    Ferro, Monica; Pastori, Nadia; Punta, Carlo; Melone, Lucio; Panzeri, Walter; Rossi, Barbara; Trotta, Francesco

    2017-01-01

    Two different formulations of cyclodextrin nanosponges (CDNS), obtained by polycondensation of β-cyclodextrin with ethylenediaminetetraacetic acid dianhydride (EDTAn), were treated with aqueous solutions of ibuprofen sodium salt (IbuNa) affording hydrogels that, after lyophilisation, gave two solid CDNS-drug formulations. 1H fast MAS NMR and 13C CP-MAS NMR spectra showed that IbuNa was converted in situ into its acidic and dimeric form (IbuH) after freeze-drying. 13C CP-MAS NMR spectra also indicated that the structure of the nanosponge did not undergo changes upon drug loading compared to the unloaded system. However, the 13C NMR spectra collected under variable contact time cross-polarization (VCT-CP) conditions showed that the polymeric scaffold CDNS changed significantly its dynamic regime on passing from the empty CDNS to the drug-loaded CDNS, thus showing that the drug encapsulation can be seen as the formation of a real supramolecular aggregate rather than a conglomerate of two solid components. Finally, the structural features obtained from the different solid-state NMR approaches reported matched the information from powder X-ray diffraction profiles. PMID:28228859

  11. Bulk magnetization and 1H NMR spectra of magnetically heterogeneous model systems

    Energy Technology Data Exchange (ETDEWEB)

    Levin, E M; Bud& #x27; ko, S L

    2011-04-28

    Bulk magnetization and ¹H static and magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectra of two magnetically heterogeneous model systems based on laponite (LAP) layered silicate or polystyrene (PS) with low and high proton concentration, respectively, and ferrimagnetic Fe₂O₃ nano- or micro-particles have been studied. In LAP+Fe₂O₃, a major contribution to the NMR signal broadening is due to the dipolar coupling between the magnetic moments of protons and magnetic particles. In PS+Fe₂O₃, due to the higher proton concentration in polystyrene and stronger proton–proton dipolar coupling, an additional broadening is observed, i.e. ¹H MAS NMR spectra of magnetically heterogeneous systems are sensitive to both proton–magnetic particles and proton–proton dipolar couplings. An increase of the volume magnetization by ~1 emu/cm³ affects the ¹H NMR signal width in a way that is similar to an increase of the proton concentration by ~2×10²²/cm³. ¹H MAS NMR spectra, along with bulk magnetization measurements, allow the accurate determination of the hydrogen concentration in magnetically heterogeneous systems.

  12. Bulk magnetization and 1H NMR spectra of magnetically heterogeneous model systems

    Science.gov (United States)

    Levin, E. M.; Bud'ko, S. L.

    2011-10-01

    Bulk magnetization and 1H static and magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectra of two magnetically heterogeneous model systems based on laponite (LAP) layered silicate or polystyrene (PS) with low and high proton concentration, respectively, and ferrimagnetic Fe2O3 nano- or micro-particles have been studied. In LAP+Fe2O3, a major contribution to the NMR signal broadening is due to the dipolar coupling between the magnetic moments of protons and magnetic particles. In PS+Fe2O3, due to the higher proton concentration in polystyrene and stronger proton-proton dipolar coupling, an additional broadening is observed, i.e. 1H MAS NMR spectra of magnetically heterogeneous systems are sensitive to both proton-magnetic particles and proton-proton dipolar couplings. An increase of the volume magnetization by ∼1 emu/cm3 affects the 1H NMR signal width in a way that is similar to an increase of the proton concentration by ∼2×1022/cm3. 1H MAS NMR spectra, along with bulk magnetization measurements, allow the accurate determination of the hydrogen concentration in magnetically heterogeneous systems.

  13. [Hepatic manifestation of a macrophage activation syndrome (MAS)].

    Science.gov (United States)

    Nagel, Michael; Schwarting, Andreas; Straub, Beate K; Galle, Peter R; Zimmermann, Tim

    2017-05-01

    Background Elevated liver values are the most common pathological laboratory result in Germany. Frequent findings, especially in younger patients, are nutritive- or medicamentous- toxic reasons, viral or autoimmune hepatitis. A macrophage activation syndrome (MAS) may manifest like a viral infectious disease with fever, hepatosplenomegaly and pancytopenia and is associated with a high mortality. It is based on an enhanced activation of macrophages with increased cytokine release, leading to organ damage and multi-organ failure. In addition to genetic causes, MAS is commonly associated with infections and rheumatic diseases. We report the case of a 26-year-old female patient suffering from MAS as a rare cause of elevated liver enzymes. Methods Patient characteristics, laboratory values, liver histology, bone marrow and radiological imaging were documented and analyzed. Case Report After an ordinary upper airway infection with bronchitis, a rheumatic arthritis appeared and was treated with leflunomide und methotrexate. In the further course of the disease, the patient developed an acute hepatitis with fever, pancytopenia and massive hyperferritinemia. Immunohistochemistry of the liver biopsy revealed hemophagocytosis and activation of CD68-positive macrophages. In the radiological and histological diagnostics of the liver and bone marrow, an MAS was diagnosed as underlying disease of the acute hepatitis. Under therapy with prednisolone, the fever disappeared and transaminases and ferritin rapidly normalized. Conclusion Aside from the frequent causes of elevated liver values in younger patients, such as nutritive toxic, drug induced liver injury, viral or autoimmune hepatitis, especially in case of massive hyperferritinemia, a MAS should be considered as a rare cause of acute liver disease. © Georg Thieme Verlag KG Stuttgart · New York.

  14. Solid-state NMR studies of bacteriorhodopsin and the purple membrane

    CERN Document Server

    Mason, A J

    2001-01-01

    proteins. This technique may prove particularly useful when studying large proteins that are difficult to orient where the MAS lineshapes will remain relatively unaffected in comparison with current static NMR methods. Finally the MAOSS method was extended to the study of the lipid components of the purple membrane and the feasibility of determining structural constraints from phospholipid headgroups was assessed. The potential of using sup 3 sup 1 P NMR to observe qualitative protein-lipid interactions in both the purple membrane and reconstituted membranes containing bovine rhodopsin was also demonstrated. Following the demonstration of a new MAS NMR method for resolving orientational constraints in uni-axially oriented biological membranes (Glaubitz and Watts, 1998), experiments were performed to realise the potential of the new method on large, oriented membrane proteins. Using bacteriorhodopsin in the purple membrane as a paradigm for large membrane proteins, the protein was specifically labelled with de...

  15. NMR logging apparatus

    Energy Technology Data Exchange (ETDEWEB)

    Walsh, David O; Turner, Peter

    2014-05-27

    Technologies including NMR logging apparatus and methods are disclosed. Example NMR logging apparatus may include surface instrumentation and one or more downhole probes configured to fit within an earth borehole. The surface instrumentation may comprise a power amplifier, which may be coupled to the downhole probes via one or more transmission lines, and a controller configured to cause the power amplifier to generate a NMR activating pulse or sequence of pulses. Impedance matching means may be configured to match an output impedance of the power amplifier through a transmission line to a load impedance of a downhole probe. Methods may include deploying the various elements of disclosed NMR logging apparatus and using the apparatus to perform NMR measurements.

  16. NMR logging apparatus

    Science.gov (United States)

    Walsh, David O; Turner, Peter

    2014-05-27

    Technologies including NMR logging apparatus and methods are disclosed. Example NMR logging apparatus may include surface instrumentation and one or more downhole probes configured to fit within an earth borehole. The surface instrumentation may comprise a power amplifier, which may be coupled to the downhole probes via one or more transmission lines, and a controller configured to cause the power amplifier to generate a NMR activating pulse or sequence of pulses. Impedance matching means may be configured to match an output impedance of the power amplifier through a transmission line to a load impedance of a downhole probe. Methods may include deploying the various elements of disclosed NMR logging apparatus and using the apparatus to perform NMR measurements.

  17. NMR studies of metalloproteins.

    Science.gov (United States)

    Li, Hongyan; Sun, Hongzhe

    2012-01-01

    Metalloproteins represent a large share of the proteomes, with the intrinsic metal ions providing catalytic, regulatory, and structural roles critical to protein functions. Structural characterization of metalloproteins and identification of metal coordination features including numbers and types of ligands and metal-ligand geometry, and mapping the structural and dynamic changes upon metal binding are significant for understanding biological functions of metalloproteins. NMR spectroscopy has long been used as an invaluable tool for structure and dynamic studies of macromolecules. Here we focus on the application of NMR spectroscopy in characterization of metalloproteins, including structural studies and identification of metal coordination spheres by hetero-/homo-nuclear metal NMR spectroscopy. Paramagnetic NMR as well as (13)C directly detected protonless NMR spectroscopy will also be addressed for application to paramagnetic metalloproteins. Moreover, these techniques offer great potential for studies of other non-metal binding macromolecules.

  18. {sup 6}Li({sup 18}O, {sup 17}O){sup 7}Li reaction and comparison of {sup 6, 7}Li + {sup 16, 17, 18}O potentials

    Energy Technology Data Exchange (ETDEWEB)

    Rudchik, A.T., E-mail: rudchik@kinr.kiev.ua [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Chercas, K.A. [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Kemper, K.W. [Physics Department, Florida State University, Tallahassee, FL 32306-4350 (United States); Rudchik, A.A. [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Kliczewski, S. [H. Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, ul. Radzikowskiego 152, PL-31-342 Cracow (Poland); Koshchy, E.I. [Kharkiv National University, pl. Svobody 4, 61077 Kharkiv (Ukraine); Rusek, K. [National Center for Nuclear Reseaches, ul. Hoża 69, PL-00-681 Warsaw (Poland); Heavy Ion Laboratory of Warsaw University, ul. L. Pasteura 5A, PL-02-093 Warsaw (Poland); Mezhevych, S.Yu.; Ponkratenko, O.A.; Pirnak, Val.M. [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Plujko, V.A. [Taras Shevchenko National University, ul. Volodymyrska 64, 01033 Kyiv (Ukraine); Choiński, J. [Heavy Ion Laboratory of Warsaw University, ul. L. Pasteura 5A, PL-02-093 Warsaw (Poland); Czech, B.; Siudak, R.; Szczurek, A. [H. Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, ul. Radzikowskiego 152, PL-31-342 Cracow (Poland)

    2014-07-15

    Angular distributions of the {sup 6}Li({sup 18}O, {sup 17}O){sup 7}Li reaction were measured at E{sub lab}({sup 18}O)=114 MeV for ground and excited states of the exit channel nuclei for the first time. The data were analyzed within the coupled-reaction-channels method (CRC). The {sup 6}Li + {sup 18}O elastic and inelastic scattering channels as well as simplest one- and two-step reactions were included in the coupled-reaction-channels scheme. The {sup 7}Li + {sup 17}O potential was deduced by fitting CRC calculations to the reaction data. The spectroscopic amplitudes for single nucleon and nuclear cluster configurations were calculated within the translationally invariant shell model. Isotopic differences of the {sup 7}Li + {sup 16, 17, 18}O and {sup 7, 8}Li + {sup 17}O potentials and the reaction mechanisms were studied.

  19. Digital signal processing for a thermal neutron detector using ZnS(Ag):{sup 6}LiF scintillating layers read out with WLS fibers and SiPMs

    Energy Technology Data Exchange (ETDEWEB)

    Mosset, J.-B., E-mail: jean-baptiste.mosset@psi.ch; Stoykov, A.; Greuter, U.; Hildebrandt, M.; Schlumpf, N.

    2016-07-11

    We present a digital signal processing system based on a photon counting approach which we developed for a thermal neutron detector consisting of ZnS(Ag):{sup 6}LiF scintillating layers read out with WLS fibers and SiPMs. Three digital filters have been evaluated: a moving sum, a moving sum after differentiation and a digital CR-RC{sup 4} filter. The performances of the detector with these filters are presented. A full analog signal processing using a CR-RC{sup 4} filter has been emulated digitally. The detector performance obtained with this analog approach is compared with the one obtained with the best performing digital approach. - Highlights: • Application of digital signal processing for a SiPM-based ZnS:6LiF neutron detector. • Optimisation of detector performances with 3 different digital filters. • Comparison with detector performances with a full analog signal processing.

  20. Bulk magnetization and {sup 1}H NMR spectra of magnetically heterogeneous model systems

    Energy Technology Data Exchange (ETDEWEB)

    Levin, E.M., E-mail: levin@iastate.edu [Division of Materials Sciences and Engineering, Ames Laboratory of US DOE (United States); Department of Physics and Astronomy, Iowa State University, Iowa, IA 50011-3020 (United States); Bud' ko, S.L. [Division of Materials Sciences and Engineering, Ames Laboratory of US DOE (United States); Department of Physics and Astronomy, Iowa State University, Iowa, IA 50011-3020 (United States)

    2011-10-15

    Bulk magnetization and {sup 1}H static and magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectra of two magnetically heterogeneous model systems based on laponite (LAP) layered silicate or polystyrene (PS) with low and high proton concentration, respectively, and ferrimagnetic Fe{sub 2}O{sub 3} nano- or micro-particles have been studied. In LAP+Fe{sub 2}O{sub 3}, a major contribution to the NMR signal broadening is due to the dipolar coupling between the magnetic moments of protons and magnetic particles. In PS+Fe{sub 2}O{sub 3}, due to the higher proton concentration in polystyrene and stronger proton-proton dipolar coupling, an additional broadening is observed, i.e. {sup 1}H MAS NMR spectra of magnetically heterogeneous systems are sensitive to both proton-magnetic particles and proton-proton dipolar couplings. An increase of the volume magnetization by {approx}1 emu/cm{sup 3} affects the {sup 1}H NMR signal width in a way that is similar to an increase of the proton concentration by {approx}2x10{sup 22}/cm{sup 3}. {sup 1}H MAS NMR spectra, along with bulk magnetization measurements, allow the accurate determination of the hydrogen concentration in magnetically heterogeneous systems. - Highlights: > {sup 1}H NMR and magnetization allow study of dipolar interactions in magnetically heterogeneous systems. > Both the proton-proton and proton-magnetic particle dipolar interactions affect {sup 1}H NMR spectra. > {sup 1}H NMR and magnetization can be used for the accurate determination of the hydrogen concentration.

  1. UC Merced NMR Instrumentation Acquisition

    Science.gov (United States)

    2015-06-18

    UC Merced NMR Instrumentation Acquisition For the UC Merced NMR Instrumentation Acquisition proposal, a new 400 MHz and an upgraded 500 MHz NMR ...UC Merced NMR Instrumentation Acquisition Report Title For the UC Merced NMR Instrumentation Acquisition proposal, a new 400 MHz and an upgraded 500...MHz NMR have been delivered, installed, and incorporated into research and two lab courses. While no results from these instruments have been

  2. Observation of breakup transfer process for the bound states of {sup 16}O populated from {sup 12}C({sup 6}Li,d) reaction at 20 MeV

    Energy Technology Data Exchange (ETDEWEB)

    Adhikari, S.; Basu, C.; Thompson, I. J.; Sugathan, P.; Jhinghan, A.; Golda, K. S.; Babu, A.; Singh, D.; Ray, S.; Mitra, A. K. [Nuclear Physics Division, Saha Institute of Nuclear Physics, Kolkata-700064 (India); Lawrence Livermore National Laboratory, L-414, Livermore CA 94551 (United States); Inter University Accelerator Centre, New Delhi 110067 (India); Physics Department, Ramkrishna Vivekananda University, Belur, Howrah (India); Nuclear Physics Division, Saha Institute of Nuclear Physics, Kolkata-700064 (India)

    2012-10-20

    The deuteron angular distribution for the {sup 12}C({sup 6}Li,d){sup 16}O* has been measured at 20 MeV populating bound and unbound states of {sup 16}O. Analysis shows a dominance of breakup induced alpha transfer in comparison to a direct alpha transfer process for the bound states. The effect increases as the excitation energy of {sup 16}O decreases, maximizing at the ground state.

  3. Hexameric Capsules Studied by Magic Angle Spinning Solid-State NMR Spectroscopy: Identifying Solvent Molecules in Pyrogallol[4]arene Capsules.

    Science.gov (United States)

    Avram, Liat; Goldbourt, Amir; Cohen, Yoram

    2016-01-18

    Powders of pyrogallol[4]arene hexamers were produced by evaporation from organic solvents and were studied, for the first time, by magic angle spinning solid-state NMR (MAS ssNMR). Evaporation selectively removed non-encapsulated solvent molecules leaving stable hexameric capsules encapsulating solvent molecules. After exposure of the powder to solvent vapors, (1)H/(13)C heteronuclear correlation MAS ssNMR experiments were used to assign the signals of the external and encapsulated solvent molecules. The formed capsules were stable for months and the process of solvent encapsulation was reversible. According to the ssNMR experiments, the encapsulated solvent molecules occupy different sites and those sites differ in their mobility. The presented approach paves the way for studying guest exchange, guest affinity, and gas storage in hexamers of this type in the solid state.

  4. An explanation for the high stability of polycarboxythiophenes in photovoltaic devices—A solid-state NMR dipolar recoupling study

    DEFF Research Database (Denmark)

    Bierring, M.; Nielsen, J.S.; Siu, Ana

    2008-01-01

    observed in photovoltaic devices employing polythiophene substituted with carboxylic-acid moieties under oxygen free conditions. H-1 and C-13 solid-state NMR, IR, and ESR spectroscopy of unmodified and isotopically labeled polythiophenes were studied. Distances between the isotopically labeled carboxylic...... acid carbon atoms were measured by C-13 solid-state magic-angle-spinning (MAS) NMR using symmetry-based double-quantum (2Q) dipolar recoupling. This revealed the presence of C-13-C-13 distances of 3.85 angstrom, which correspond to the C-C distance in hydrogen-bonded carboxylic acid dimers. In spite...... of the presence of carboxylic groups in the polymer as demonstrated by C-13 CP/MAS NMR and IR spectroscopy, the absence of carboxylic protons in solid state H-1 NMR spectra indicate that they are mobile. We link the extraordinary stability of this system to the rigid nature, cross-linking through a hydrogen...

  5. Solid state NMR study calcium phosphate ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Miquel, J.L.; Facchini, L.; Legrand, A.P. (Laboratoire de Physique Quantique, Paris (France). CNRS, URA421, ESPCI); Rey, C. (CNRS, Toulouse (France). ENSC. Laboratoire de Physico-chimie des Solides); Lemaitre, J. (EPF Lausanne (France). Laboratoire de Technologie des Poudres)

    1990-04-01

    High-resolution {sup 31}P and {sup 1}H NMR spectra at 40 and 121 MHz {sup 31}P and 300 MHz {sup 1}H of synthetic and biological samples of calcium phosphates have been obtained by magic angle spinning (MAS) at spinning speeds up to 6.5 kHz, and high power proton decoupling. The samples include crystalline hydroxyapatite, a deficient hydroxyapatite characterized by a Ca/P atomic ratio of 1.5, a poorly crystallized hydroxyapatite, monetite, brushite, octacalcium phosphate, {beta}-tricalcium phosphate and rabbit femoral bone. The interactions between nuclei in unlike structures and the mobility of acid protons are discussed. (author). 11 refs.; 2 figs.; 1 tab.

  6. Proton-Based Ultrafast Magic Angle Spinning Solid-State NMR Spectroscopy.

    Science.gov (United States)

    Zhang, Rongchun; Mroue, Kamal H; Ramamoorthy, Ayyalusamy

    2017-04-18

    Protons are vastly abundant in a wide range of exciting macromolecules and thus can be a powerful probe to investigate the structure and dynamics at atomic resolution using solid-state NMR (ssNMR) spectroscopy. Unfortunately, the high signal sensitivity, afforded by the high natural-abundance and high gyromagnetic ratio of protons, is greatly compromised by severe line broadening due to the very strong (1)H-(1)H dipolar couplings. As a result, protons are rarely used, in spite of the desperate need for enhancing the sensitivity of ssNMR to study a variety of systems that are not amenable for high resolution investigation using other techniques including X-ray crystallography, cryo-electron microscopy, and solution NMR spectroscopy. Thanks to the remarkable improvement in proton spectral resolution afforded by the significant advances in magic-angle-spinning (MAS) probe technology, (1)H ssNMR spectroscopy has recently attracted considerable attention in the structural and dynamics studies of various molecular systems. However, it still remains a challenge to obtain narrow (1)H spectral lines, especially from proteins, without resorting to deuteration. In this Account, we review recent proton-based ssNMR strategies that have been developed in our laboratory to further improve proton spectral resolution without resorting to chemical deuteration for the purposes of gaining atomistic-level insights into molecular structures of various crystalline solid systems, using small molecules and peptides as illustrative examples. The proton spectral resolution enhancement afforded by the ultrafast MAS frequencies up to 120 kHz is initially discussed, followed by a description of an ensemble of multidimensional NMR pulse sequences, all based on proton detection, that have been developed to obtain in-depth information from dipolar couplings and chemical shift anisotropy (CSA). Simple single channel multidimensional proton NMR experiments could be performed to probe the proximity

  7. Stabilization of the angiotensin-(1-7) receptor Mas through interaction with PSD95.

    Science.gov (United States)

    Bian, Weihua; Sun, Licui; Yang, Longyan; Li, Ji-Feng; Hu, Jia; Zheng, Shuai; Guo, Ruihan; Feng, Duiping; Ma, Qian; Shi, Xiaocui; Xiong, Ying; Yang, Xiaomei; Song, Ran; Xu, Jianguo; Wang, Songlin; He, Junqi

    2013-08-01

    The functions and signalling mechanisms of the Ang-(1-7) [angiotensin-(1-7)] receptor Mas have been studied extensively. However, less attention has been paid to the intracellular regulation of Mas protein. In the present study, PSD95 (postsynaptic density 95), a novel binding protein of Mas receptor, was identified, and their association was characterized further. Mas specifically interacts with PDZ1-2, but not the PDZ3, domain of PSD95 via Mas-CT (Mas C-terminus), and the last four amino acids [ETVV (Glu-Thr-Val-Val)] of Mas-CT were determined to be essential for this interaction, as shown by GST pull-down, co-immunoprecipitation and confocal co-localization experiments. Gain-of-function and loss-of-function studies indicated that PSD95 enhanced Mas protein expression by increasing the stabilization of the receptor. Mas degradation was robustly inhibited by the proteasome inhibitor MG132 in time- and dose-dependent manners, and the expression of PSD95 impaired Mas ubiquitination, indicating that the PSD95-Mas association inhibits Mas receptor degradation via the ubiquitin-proteasome proteolytic pathway. These findings reveal a novel mechanism of Mas receptor regulation by which its expression is modulated at the post-translational level by ubiquitination, and clarify the role of PSD95, which binds directly to Mas, blocking the ubiquitination and subsequent degradation of the receptor via the ubiquitin-proteasome proteolytic pathway.

  8. ERP sistēmas ieviešana

    OpenAIRE

    Proskurins, Aleksandrs

    2008-01-01

    Šajā darbā tika apskatīta informācijas sistēmu klasifikācija, uzņēmuma resursu plānošanas sistēmas (ERP) definīcija un tās vieta IS klasifikācijā. Tika apskatīti ERP sistēmu ieviešanas teorētiskie aspekti, izstrādes un pielāgošanas specifika, kā arī tika izanalizēti vairāki ERP sistēmas ieviešanas projekti Latvijas uzņēmumos.

  9. Cross ambiguity functions on the MasPar MP-2

    Energy Technology Data Exchange (ETDEWEB)

    Carlson, D.A.; Pryor, D.V. [Superconducting Research Center, Bowie, MD (United States); Frock, C.K. [and others

    1995-12-01

    In a signal processing environment, cross ambiguity functions are often used to detect when one signal is a time and/or frequency shift of another. They consist of multiple cross-correlations, which can be computed efficiently using complex valued FFTs. This paper discusses the implementation of cross ambiguity functions on the MasPar MP-2, a SIMD processor array. Two different implementations are developed. The first computes each cross ambiguity function serially, using FFT code that parallelizes across the complete set of processors. The second uses the MasPar IORAM to realign the data so that the cross ambiguity functions can be computed in parallel. In this case, multiple FFTs are executed in parallel on subsets of the processors, which lowers the overall amount of communication required.

  10. ERP sistēmas ieviešana

    OpenAIRE

    Proskurins, Aleksandrs

    2008-01-01

    Šajā darbā tika apskatīta informācijas sistēmu klasifikācija, uzņēmuma resursu plānošanas sistēmas (ERP) definīcija un tās vieta IS klasifikācijā. Tika apskatīti ERP sistēmu ieviešanas teorētiskie aspekti, izstrādes un pielāgošanas specifika, kā arī tika izanalizēti vairāki ERP sistēmas ieviešanas projekti Latvijas uzņēmumos.

  11. O-17 NMR studies of some silicate crystals and glasses

    CERN Document Server

    Yildirim, E K

    2000-01-01

    structure. Therefore some of the Sn has to be in three coordinated to oxygen for charge balancing. The sup 1 sup 7 O MAS NMR spectra of a partially crystallised sample showed three distinct sites which are assigned as Sn-O-Sn, Si-O-Sn, and Si-O-Si on the basis of their chemical shift. The C sub Q values obtained from the simulations of these peaks supports this assignment. The sup 2 sup 9 Si MAS NMR of the same sample showed two crystalline and a glassy peaks which are fitted to two crystalline and two glassy sites. The possible composition of this sample was calculated and found to be SiSn sub 8 O sub 1 sub 0. Crystalline and glassy silicates were investigated by means of sup 1 sup 7 O NMR. The dependence of the measured efg on the Si-O-AI bond angle was investigated in some crystalline aluminosilicate sodalites and kalsilite. The results show that C sub Q increases with increasing bond angle while eta decreases with increasing bond angle and they both follow a similar function to that found for the Si-O-Si ...

  12. IN SITU MAGIC ANGLE SPINNING NMR FOR STUDYING GEOLOGICAL CO(2) SEQUESTRATION

    Energy Technology Data Exchange (ETDEWEB)

    Hoyt, David W.; Turcu, Romulus VF; Sears, Jesse A.; Rosso, Kevin M.; Burton, Sarah D.; Kwak, Ja Hun; Felmy, Andrew R.; Hu, Jian Z.

    2011-03-27

    Geological carbon sequestration (GCS) is one of the most promising ways of mitigating atmospheric greenhouse gases (1-3). Mineral carbonation reactions are potentially important to the long-term sealing effectiveness of caprock but remain poorly predictable, particularly in low-water supercritical CO2 (scCO2)-dominated environments where the chemistry has not been adequately explored. In situ probes that provide molecular-level information is desirable for investigating mechanisms and rates of GCS mineral carbonation reactions. MAS-NMR is a powerful tool for obtaining detailed molecular structure and dynamics information of a system regardless whether the system is in a solid, a liquid, a gaseous, or a supercritical state, or a mixture thereof (4,5). However, MAS NMR under scCO2 conditions has never been realized due to the tremendous technical difficulties of achieving and maintaining high pressure within a fast spinning MAS rotor (6,7), where non-metal materials must be used. In this work, we report development of a unique high pressure MAS NMR capability, and its application to mineral carbonation chemistry in scCO2 under geologically relevant temperatures and pressures.

  13. Benford distributions in NMR

    CERN Document Server

    Bhole, Gaurav; Mahesh, T S

    2014-01-01

    Benford's Law is an empirical law which predicts the frequency of significant digits in databases corresponding to various phenomena, natural or artificial. Although counter intuitive at the first sight, it predicts a higher occurrence of digit 1, and decreasing occurrences to other larger digits. Here we report the Benford analysis of various NMR databases and draw several interesting inferences. We observe that, in general, NMR signals follow Benford distribution in time-domain as well as in frequency domain. Our survey included NMR signals of various nuclear species in a wide variety of molecules in different phases, namely liquid, liquid-crystalline, and solid. We also studied the dependence of Benford distribution on NMR parameters such as signal to noise ratio, number of scans, pulse angles, and apodization. In this process we also find that, under certain circumstances, the Benford analysis can distinguish a genuine spectrum from a visually identical simulated spectrum. Further we find that chemical-sh...

  14. Influence of the spinning rate in the HR-MAS pattern of mobile lipids in C6 glioma cells and in artificial oil bodies.

    Science.gov (United States)

    Martín-Sitjar, Juana; Delgado-Goñi, Teresa; Cabañas, Miquel E; Tzen, Jason; Arús, Carles

    2012-12-01

    To evaluate how spinning rate affects mobile lipid (ML) resonances visibility in HR-MAS spectra of C6 glioma cells and artificial oil bodies (AOB), as models of cytosolic lipid droplets. Using C6 cells and AOB of two different sizes, 780 ± 580 and 240 ± 293 nm, as models, we acquired HR-MAS pulse and acquire spectra at different spinning rates between 500 and 15,000 Hz, all at 37 °C. Sample spinning at 15,000 Hz increased by 2.3 and 4.6-fold with respect to 500 Hz spinning the area of resonances corresponding to ML at 0.88 and 1.28 ppm, respectively, for log phase C6 cells. Furthermore, postconfluent C6 cells displayed an increase of 2.5-fold at 0.88 ppm and 4.2-fold at 1.28 ppm. These changes were reversible upon low speed spinning. AOBs did show much lower ML area increases (1.4-1.5-fold) upon high-speed HR-MAS. ML can be reversibly mobilized in C6 glioma cells by high-speed HR-MAS, partially unveiling the NMR "invisible" ML pool. A small part of the ML pool also shows reduced visibility in freely tumbling AOBs.

  15. PERBAIKAN MUTU GENETIK IKAN MAS RAJADANU MELALUI SELEKSI

    Directory of Open Access Journals (Sweden)

    Deni Radona

    2016-11-01

    Full Text Available Ikan mas rajadanu mempunyai karakter cepat tumbuh dan tahan penyakit. Selective breeding merupakan salah satu upaya dalam peningkatan mutu induk dan benih. Penelitian ini bertujuan untuk melihat respons pertumbuhan dan nilai heritabilitas pada ikan mas rajadanu (F-3 yang berpotensi tumbuh lebih cepat dibandingkan dengan generasi sebelumnya (F-2. Pembentukan ikan mas rajadanu F-3 dilakukan dengan metode hierarki (satu jantan membuahi empat betina. Pengujian respons seleksi dilakukan terhadap benih hasil pemijahan induk ikan mas rajadanu F-2 yang terseleksi. Terbentuk sebanyak 25 famili dan dipelihara secara terpisah selama 160 hari pada kolam beton ukuran 1,5 m x 1 m dengan ketinggian air 60 cm. Kolam digunakan sebanyak 25 buah. Respons seleksi dihitung dengan melihat nilai rata-rata pertumbuhan F-3 dibandingkan dengan F-2. Hasil penelitian menunjukan performa ikan mas rajadanu F-3 memiliki nilai respons seleksi (14,20 g; nilai heritabilitas (0,60; pertambahan bobot (41,63 ± 10,51 g; dan pertambahan panjang (9,86 ± 1,43 cm. Rajadanu carp strain have character of fast growing and disease resistant. Selective breeding is one of an attempts can be appllied to improve the broodstock and seed quality genetically. This research was aims to see response of growth and heritability value of F-3 on carp rajadanu that potentially grow faster compared with previous generation (F-2. The F-3 carp rajadanu was designated with hierarchy method (one males fertilize four female. The F-3 was derived from F-2 and formed 25 families. Those families were maintained for 160 days on pond with size of 1.5 m x 1 m and water depth of 60 cm. The response selection was calculated by choosing the best individuals of each based on ADG (averange daily growth. The research result show that the values of response selection was 14.20 g, heritability value of 0.60, weight, and length gain were 41.63 g and 9.86 cm, respectively.

  16. The MicroMAS CubeSat Mission

    Science.gov (United States)

    Cahoy, K.; Blackwell, W. J.; Allen, G.; Bury, M.; Efromson, R.; Galbraith, C.; Hancock, T.; Leslie, V.; Osaretin, I.; Retherford, L.; Scarito, M.; Shields, M.; Toher, D.; Wight, K.; Miller, D.; Marinan, A.; Paek, S.; Peters, E.; Schmidt, F. H.; Alvisio, B.; Wise, E.; Masterson, R.; Franzim Miranda, D.; Crail, C.; Kingsbury, R.; Souffrant, A.; Orrego, L.; Eslinger, G.; Nicholas, A.; Pong, C.

    2012-12-01

    The recently published Midterm Assessment of NASA's Implementation of the Decadal Survey finds that, "The nation's Earth observing system is beginning a rapid decline in capability as long-running missions end and key new missions are delayed, lost, or canceled. The projected loss of observing capability could have significant adverse consequences for science and society." In this presentation, we explore low-cost, mission-flexible, and rapidly deployable spaceborne sensors that can meet stringent performance requirements pervading the NASA Earth Science measurement programs, including especially the recommended NRC Decadal Survey missions. New technologies have enabled a novel approach toward this science observational goal, and in this paper we describe recent technology develop efforts to address the challenges above through the use of CubeSat radiometers. The Micro-sized Microwave Atmospheric Satellite (MicroMAS) is a 3U cubesat (30x10x10 cm, ~4kg) hosting a passive microwave spectrometer operating near the 118.75-GHz oxygen absorption line. The focus of the first MicroMAS mission (hereafter, MicroMAS-1) is to observe convective thunderstorms, tropical cyclones, and hurricanes from a near-equatorial orbit at approximately 500-km altitude. A MicroMAS flight unit is currently being developed in anticipation of a 2014 launch to be provided by NASA. A parabolic reflector is mechanically rotated as the spacecraft orbits the earth, thus directing a cross-track scanned beam with FWHM beamwidth of 2.4-degrees, yielding an approximately 25-km diameter footprint from a nominal altitude of 500 km. Radiometric calibration is carried out using observations of cold space, the earth's limb, and an internal noise diode that is weakly coupled through the RF front-end electronics. A key technology feature is the development of an ultra-compact intermediate frequency processor module for channelization, detection, and A-to-D conversion. The antenna system and RF front

  17. Cellulose Isolation Methodology for NMR Analysis of Cellulose Ultrastructure

    Directory of Open Access Journals (Sweden)

    Art J. Ragauskas

    2011-11-01

    Full Text Available In order to obtain accurate information about the ultrastructure of cellulose from native biomass by 13C cross polarization magic angle spinning (CP/MAS NMR spectroscopy the cellulose component must be isolated due to overlapping resonances from both lignin and hemicellulose. Typically, cellulose isolation has been achieved via holocellulose pulping to remove lignin followed by an acid hydrolysis procedure to remove the hemicellulose components. Using 13C CP/MAS NMR and non-linear line-fitting of the cellulose C4 region, it was observed that the standard acid hydrolysis procedure caused an apparent increase in crystallinity of ~10% or less on the cellulose isolated from Populus holocellulose. We have examined the effect of the cellulose isolation method, particularly the acid treatment time for hemicellulose removal, on cellulose ultrastructural characteristics by studying these effects on cotton, microcrystalline cellulose (MCC and holocellulose pulped Populus. 13C CP/MAS NMR of MCC indicated that holocellulose pulping and acid hydrolysis has little effect on the crystalline ultrastructural components of cellulose. Although any chemical method to isolate cellulose from native biomass will invariably alter substrate characteristics, especially those related to regions accessible to solvents, we found those changes to be minimal and consistent in samples of typical crystallinity and lignin/hemicellulose content. Based on the rate of the hemicellulose removal, as determined by HPLC-carbohydrate analysis and magnitude of cellulose ultrastructural alteration, the most suitable cellulose isolation methodology utilizes a treatment of 2.5 M HCl at 100 °C for a standard residence time between 1.5 and 4 h. However, for the most accurate crystallinity results this residence time should be determined empirically for a particular sample.

  18. MAS及其相关概念%MAS and Correlation Conceptions

    Institute of Scientific and Technical Information of China (English)

    程显毅; 董红斌

    2000-01-01

    The researching of MAS originates from distributed artificial intelligence ,because new theory framework is provided for solving some problems in complex and distributed environment ,MAS is valued increasingly by computer ,automatic control and management science.

  19. Marker-assisted-selection (MAS): A fast track to increase genetic ...

    African Journals Online (AJOL)

    MAS have been widely used for simple inherited traits than for polygenic traits, although there are few success stories in improving quantitative traits through MAS. ... Key words: DNA sequence, gene introgression, genetic maps, germplasm ...

  20. Solid-state NMR characterization of Mowry Formation shales

    Energy Technology Data Exchange (ETDEWEB)

    Miknis, F.P.

    1992-04-01

    Solid-state [sup 13]C and [sup 29]Si NMR measurements were carried out on a series of petroleum source rocks from the Mowry Formation of the Powder River Basin in Wyoming. The objectives of this study wereto use CP/MAS [sup 13]C NMR measurements to monitor changes in the carbon structure of the kerogen that result from depth of burial, and to examine the feasibility of [sup 29]Si NMR for studying the thermal alteration of clay minerals during diagenesis. Carbon and silicon NMR measurements were made on a suite of samples covering a present-day depth interval of 3,000 to 11,500 ft.In general, the NMR results endorsed other geochemical analyses that were performed on the source rocks as part of another study to examine pressure compartmentalization in the Mowry Formation. The carbon aromaticity of the kerogen increased with depth of burial, and at depths greater that approximately 10,000 ft the kerogen showed little capacity to generate additional oil because of the small fraction of residual aliphatic carbon. By combining NMR and Rock-Eval measurements, an estimate of the hydrogen budget was obtained. The calculations indicated that approximately 20% of the kerogen was converted to hydrocarbons, and that sufficient hydrogen was liberated from aromatization and condensation reactions to stabilize the generated products. The [sup 29]Si NMR spectra were characterized by a relatively sharp quartz resonance and a broad resonance from the clay minerals. With increasing depth of burial, the clay resonance became broader and shifted slightly downfield. These changes qualitatively support X-ray analysis that shows progressive alteration of illite to smectite with depth of burial.

  1. Solid-state NMR characterization of Mowry Formation shales

    Energy Technology Data Exchange (ETDEWEB)

    Miknis, F.P.

    1992-04-01

    Solid-state {sup 13}C and {sup 29}Si NMR measurements were carried out on a series of petroleum source rocks from the Mowry Formation of the Powder River Basin in Wyoming. The objectives of this study wereto use CP/MAS {sup 13}C NMR measurements to monitor changes in the carbon structure of the kerogen that result from depth of burial, and to examine the feasibility of {sup 29}Si NMR for studying the thermal alteration of clay minerals during diagenesis. Carbon and silicon NMR measurements were made on a suite of samples covering a present-day depth interval of 3,000 to 11,500 ft.In general, the NMR results endorsed other geochemical analyses that were performed on the source rocks as part of another study to examine pressure compartmentalization in the Mowry Formation. The carbon aromaticity of the kerogen increased with depth of burial, and at depths greater that approximately 10,000 ft the kerogen showed little capacity to generate additional oil because of the small fraction of residual aliphatic carbon. By combining NMR and Rock-Eval measurements, an estimate of the hydrogen budget was obtained. The calculations indicated that approximately 20% of the kerogen was converted to hydrocarbons, and that sufficient hydrogen was liberated from aromatization and condensation reactions to stabilize the generated products. The {sup 29}Si NMR spectra were characterized by a relatively sharp quartz resonance and a broad resonance from the clay minerals. With increasing depth of burial, the clay resonance became broader and shifted slightly downfield. These changes qualitatively support X-ray analysis that shows progressive alteration of illite to smectite with depth of burial.

  2. Mobility and relaxation determinations of lithium in lithium aluminate ceramics using solid-state NMR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Stewart, F.F.; Peterson, E.S. [Idaho National Engineering Lab., Idaho Falls, ID (United States); Stebbins, J.F. [Stanford Univ., CA (United States)] [and others

    1995-02-01

    Lithium aluminate is one of the materials being considered for fusion reactor blankets. When preparing the ceramic, it is important to be able to monitor the microstructures since it is a controlling factor in the rate of tritium release from the blanket. Nuclear magnetic resonance spectroscopy (NMR) has been shown to be a useful tool for the nondestructive analysis of ceramics. Studies detailed in this paper include spectral acquisition, assignment, spin-lattice relaxation time measurements, temperature effects, their correlation to structure, and material purity. The ceramic of interest was lithium aluminate, LiAl{sub 5}O{sub 8}. This material was studied by observation of the NMR active nuclei {sup 6}Li, {sup 7}Li, and {sup 27}Al. For these nuclei, spin-lattice relaxation times (T{sub 1}) were measured and were found to vary considerably, correlating to the presence of paramagnetic impurities within the crystalline lattice. Previous research has shown that the coordination about the aluminum nucleus can be determined using {sup 27}Al NMR spectroscopy. Aluminum-27 NMR spectroscopy was successfully applied, and it provided valuable insight into composition of the ceramic. 20 refs., 4 figs., 3 tabs.

  3. 77 FR 43084 - Multiple Award Schedule (MAS) Program Continuous Open Season-Operational Change

    Science.gov (United States)

    2012-07-23

    ... ADMINISTRATION Multiple Award Schedule (MAS) Program Continuous Open Season- Operational Change AGENCY: Federal... to assess and improve the performance of the Multiple Award Schedule (MAS) contracts operated by GSA. GSA is proposing this operational change to enhance the performance of and modernize the MAS program...

  4. 47 CFR 101.1317 - Competitive bidding procedures for mutually exclusive MAS EA applications.

    Science.gov (United States)

    2010-10-01

    ... exclusive MAS EA applications. 101.1317 Section 101.1317 Telecommunication FEDERAL COMMUNICATIONS COMMISSION... License Requirements § 101.1317 Competitive bidding procedures for mutually exclusive MAS EA applications. Mutually exclusive initial applications for licenses in the portions of the MAS bands licensed on a...

  5. 48 CFR 538.270 - Evaluation of multiple award schedule (MAS) offers.

    Science.gov (United States)

    2010-10-01

    ... award schedule (MAS) offers. 538.270 Section 538.270 Federal Acquisition Regulations System GENERAL... and Administering Federal Supply Schedules 538.270 Evaluation of multiple award schedule (MAS) offers... negotiation objectives and determining price reasonableness, compare the terms and conditions of the MAS...

  6. What drives cross-border M&As in commercial banking?

    NARCIS (Netherlands)

    Galamhussen, Mohamed; Hennart, Jean-Francois; Pinheiro, Carlos Manuel

    2016-01-01

    Using a gravity model, we analyze the determinants of the probability that commercial banks in 89 acquiring countries and 118 target countries will undertake M&As over a 30-year period (1981–2010) and of the value of these M&As. We find that the value of cross-border M&As increases with the size of

  7. High-resolution solid-state NMR spectroscopy of protons with homonuclear dipolar decoupling schemes under magic-angle spinning.

    Science.gov (United States)

    Madhu, P K

    2009-02-01

    High-resolution NMR spectroscopy of (1)H spins in the solid state is normally rendered difficult due to the strong homonuclear (1)H-(1)H dipolar couplings. Even under very high-speed magic-angle spinning (MAS) at ca. 60-70kHz, these couplings are not completely removed. An appropriate radiofrequency pulse scheme is required to average out the homonuclear dipolar interactions in combination with MAS to get high-resolution (1)H NMR spectrum in solid state. Several schemes have been introduced in the recent past with a variety of applications also envisaged. Development of some of these schemes has been made possible with a clear understanding of the underlying spin physics based on bimodal Floquet theory. The utility of these high-resolution pulse schemes in combination with MAS has been demonstrated for spinning speeds of 10-65kHz in a range of (1)H Larmor frequencies from 300 to 800MHz.

  8. Mechanistic insight into formation and changes of nanoparticles in MgF2 sols evidenced by liquid and solid state NMR.

    Science.gov (United States)

    Karg, M; Scholz, G; König, R; Kemnitz, E

    2012-02-28

    The fluorolytic sol-gel reaction of magnesium methoxide with HF in methanol was studied by (19)F, (1)H and (13)C liquid and solid state NMR. In (19)F NMR five different species were identified, three of which belong to magnesium fluoride nanoparticles, i.e. NMR gave access to local structures of solid particles in suspensions. The long-term evolution of (19)F signals was followed and along with (19)F MAS NMR experiments of sols rotating at 13 kHz mechanistic insights into the ageing processes were obtained.

  9. Nacionalismo e indigenismo en el gobierno del MAS

    OpenAIRE

    Mayorga, Fernando; Rodríguez, Benjamín

    2010-01-01

    En los últimos años se ha modificado el mapa político de América latina con resultados electorales que indican una idea genérica de “giro a la izquierda”, imponiendo paulatinamente una taxonomía que distingue gobiernos socialdemócratas y gobiernos populistas. En Bolivia el arribo al gobierno del Movimiento al Socialismo (MAS) en enero de 2006 y la reelección presidencial de Evo Morales, despliega el proceso de una profunda reforma estatal que articula las demandas sociales en torno al naciona...

  10. Reforma integral masía Casa Flac

    OpenAIRE

    Pérez Reyes, Sara

    2014-01-01

    La Masía Casa Flac se encuentra en un entorno rural rodeado de montañas en pleno Pirineo Catalán. Es una edificación compuesta por diferentes casas y pajares construidas en distintas épocas y etapas, para satisfacer las necesidades de sus habitantes a medida que iban desarrollando su actividad agricultora y ganadera. La primera edificación del conjunto data de finales los años 1800 y ha estado expuesta a modificaciones hasta este año, ha tenido pues un mantenimiento mínimo aunq...

  11. MAS-SCM for Auto Sector-The Framework

    Directory of Open Access Journals (Sweden)

    Ritu Sindhu

    2011-07-01

    Full Text Available The purpose of this study is to describe in detail the development status of the innovative Multi -Agent based supply chain management (MAS-SCMAS for auto sector. This study was undertaken in view of the significance of improvement in efficiency of automobile sector and the development of a good multi-agent system framework to achieve that. The factors affecting the efficiency or OEE of the industry and the efficiency properties were identified. It was clearly revealed that the available model do not fulfill the needs in the supply chain management of automobile industry and there is a scope for evolving new model resulting in better efficiency.

  12. Visibility of lipid resonances in HR-MAS spectra of brain biopsies subject to spinning rate variation.

    Science.gov (United States)

    Precht, C; Diserens, G; Oevermann, A; Vermathen, M; Lang, J; Boesch, C; Vermathen, P

    2015-12-01

    Lipid resonances from mobile lipids can be observed by ¹H NMR spectroscopy in multiple tissues and have also been associated with malignancy. In order to use lipid resonances as a marker for disease, a reference standard from a healthy tissue has to be established taking the influence of variable factors like the spinning rate into account. The purpose of our study was to investigate the effect of spinning rate variation on the HR-MAS pattern of lipid resonances in non-neoplastic brain biopsies from different regions and visualize polar and non-polar lipids by fluorescence microscopy using Nile Red staining. ¹H HR-MAS NMR spectroscopy demonstrated higher lipid peak intensities in normal sheep brain pure white matter biopsies compared to mixed white and gray matter biopsies and pure gray matter biopsies. High spinning rates increased the visibility particularly of the methyl resonances at 1.3 and the methylene resonance at 0.89 ppm in white matter biopsies stronger compared to thalamus and brainstem biopsies, and gray matter biopsies. The absence of lipid droplets and presence of a large number of myelin sheaths observed in white matter by Nile Red fluorescence microscopy suggest that the observed lipid resonances originate from the macromolecular pool of lipid protons of the myelin sheath's plasma membranes. When using lipid contents as a marker for disease, the variable behavior of lipid resonances in different neuroanatomical regions of the brain and at variable spinning rates should be considered. The findings may open up interesting possibilities for investigating lipids in myelin sheaths.

  13. Teaching NMR Using Online Textbooks

    Directory of Open Access Journals (Sweden)

    Joseph P. Hornak

    1999-12-01

    Full Text Available Nuclear magnetic resonance (NMR spectroscopy has almost become an essential analytical tool for the chemist. High-resolution one- and multi-dimensional NMR, timedomain NMR, and NMR microscopy are but a few of the NMR techniques at a chemist's disposal to determine chemical structure and dynamics. Consequently, even small chemistry departments are finding it necessary to provide students with NMR training and experience in at least some of these techniques. The hands-on experience is readily provided with access to state-of-the-art commercial spectrometers. Instruction in the principles of NMR is more difficult to achieve as most instructors try to teach NMR using single organic or analytical chemistry book chapters with static figures. This paper describes an online textbook on NMR spectroscopy called The Basics of NMR (http://www.cis.rit.edu/htbooks/nmr/ suitable for use in teaching the principles of NMR spectroscopy. The book utilizes hypertext and animations to present the principles of NMR spectroscopy. The book can be used as a textbook associated with a lecture or as a stand-alone teaching tool. Conference participants are encouraged to review the textbook and evaluate its suitability for us in teaching NMR spectroscopy to undergraduate chemistry majors.

  14. An Improved NMR Study of Liposomes Using 1-Palmitoyl-2-oleoyl-sn-glycero-3-phospatidylcholine as Model

    Directory of Open Access Journals (Sweden)

    AnnaLaura Segre

    2006-05-01

    Full Text Available In this paper we report a comparative characterization of Small UnilamellarVesicles (SUVs, Large Unilamellar Vesicles (LUVs and Multilamellar Vesicles (MLVsprepared from 1-palmitoyl-2-oleoyl-sn-glycero-3-phospatidylcholine (POPC, carried outusing two NMR techniques, namely High Resolution NMR in solution and HighResolution–Magic Angle Spinning (HR-MAS. The size and size distributions of thesevesicles were investigated using the dynamic light scattering technique. An improvedassignment of the 1H-NMR spectrum of MLVs is also reported.

  15. Applications of solid-state Nuclear Magnetic Resonance (NMR) in studies of Portland cements-based materials

    DEFF Research Database (Denmark)

    Skibsted, Jørgen; Andersen, Morten Daugaard; Jakobsen, Hans Jørgen

    2007-01-01

    Solid-state NMR spectroscopy represents an important research tool in the characterization of a range of structural properties for cement-based materials. Different approaches of the technique can be used to obtain information on hydration kinetics, mobile and bound water, porosity, and local...... atomic structures. After a short introduction to these NMR techniques, it is exemplified how magic-angle spinning (MAS) NMR can provide quantitative and structural information about specific phases in anhydrous and hydrated Portland cements with main emphasis on the incorporation of Al3+ ions...

  16. Asynchronous through-bond homonuclear isotropic mixing: application to carbon–carbon transfer in perdeuterated proteins under MAS

    Energy Technology Data Exchange (ETDEWEB)

    Kulminskaya, Natalia; Vasa, Suresh Kumar; Giller, Karin; Becker, Stefan; Linser, Rasmus, E-mail: rali@nmr.mpibpc.mpg.de [Max Planck Institute for Biophysical Chemistry, Department of NMR-based Structural Biology (Germany)

    2015-11-15

    Multiple-bond carbon–carbon homonuclear mixing is a hurdle in extensively deuterated proteins and under fast MAS due to the absence of an effective proton dipolar-coupling network. Such conditions are now commonly employed in solid-state NMR spectroscopy. Here, we introduce an isotropic homonuclear {sup 13}C–{sup 13}C through-bond mixing sequence, MOCCA, for the solid state. Even though applied under MAS, this scheme performs without rotor synchronization and thus does not pose the usual hurdles in terms of power dissipation for fast spinning. We compare its performance with existing homonuclear {sup 13}C–{sup 13}C mixing schemes using a perdeuterated and partially proton-backexchanged protein. Based on the analysis of side chain carbon–carbon correlations, we show that particularly MOCCA with standard 180-degree pulses and delays leading to non-rotor-synchronized spacing performs exceptionally well. This method provides high magnetization transfer efficiency for multiple-bond transfer in the aliphatic region compared with other tested mixing sequences. In addition, we show that this sequence can also be tailor-made for recoupling within a selected spectral region using band-selective pulses.

  17. 31P Solid-state NMR based monitoring of permeation of cell penetrating peptides into skin

    Science.gov (United States)

    Desai, Pinaki R.; Cormier, Ashley R.; Shah, Punit P.; Patlolla, Ram R.; Paravastu, Anant K.; Singh, Mandip

    2013-01-01

    The main objective of the current study was to investigate penetration of cell penetrating peptides (CPPs: TAT, R8, R11 and YKA) through skin intercellular lipids using 31P magic angle spinning (MAS) solid-state NMR. In vitro skin permeation studies were performed on rat skin, sections (0–60, 61–120 and 121–180 µm) were collected and analyzed for 31P NMR signal. The concentration dependent shift of 0, 25, 50, 100 and 200 mg/ml of TAT on skin layers, diffusion of TAT, R8, R11 and YKA in the skin and time dependent permeation of R11 was measured on various skin sections using 31P solid-state NMR. Further, CPPs and CPP-tagged fluorescent dye encapsulate liposomes (FLip) in skin layers were tagged using confocal microscopy. The change in 31P NMR chemical shift was found to depend monotonically on the amount of CPP applied on skin, with saturation behavior above 100 mg/ml CPP concentration. R11 and TAT caused more shift in solid-state NMR peaks compared to other peptides. Furthermore, NMR spectra showed R11 penetration up to 180 µm within 30 min. The results of the solid-state NMR study were in agreement with confocal microscopy studies. Thus, 31P solid-state NMR can be used to track CPP penetration into different skin layers. PMID:23702274

  18. Solid state NMR studies of gels derived from low molecular mass gelators.

    Science.gov (United States)

    Nonappa; Kolehmainen, E

    2016-07-13

    Since its invention more than six decades ago, nuclear magnetic resonance (NMR) spectroscopy has evolved as an inevitable part of chemical as well as structural analysis of small molecules, polymers, biomaterials and hybrid materials. In the solution state, due to the increased viscosity of complex viscoelastic fluids such as gels, liquid crystals and other soft materials, the rate of molecular tumbling is reduced, which in turn affects the chemical shift anisotropy, dipolar and quadrupolar interactions. As a consequence the solution state NMR spectra show broad lines, and therefore, extracting detailed structural information is a challenging task. In this context, solid state (SS) NMR has the ability to distinguish between a minute amount of polymorphic forms, conformational changes, and the number of non-equivalent molecules in an asymmetric unit of a crystal lattice, and to provide both qualitative as well as quantitative analytical data with a short-range order. Therefore, SS NMR has continued to evolve as an indispensable tool for structural analysis and gave birth to a new field called NMR crystallography. Solid state cross polarization (CP) and high resolution (HR) magic angle spinning (MAS) NMR spectroscopy has been used to study weak interactions in polymer gels. However, the application of SS NMR spectroscopy to study gels derived from low molecular weight gelators has been limited until recently. In this review, we will focus on the importance of solid state NMR spectroscopy in understanding and elucidating the structure of supramolecular gels derived from low molecular weight gelators with selected examples.

  19. Solid state NMR studies of gels derived from low molecular mass gelators

    Science.gov (United States)

    Kolehmainen, E.

    2016-01-01

    Since its invention more than six decades ago, nuclear magnetic resonance (NMR) spectroscopy has evolved as an inevitable part of chemical as well as structural analysis of small molecules, polymers, biomaterials and hybrid materials. In the solution state, due to the increased viscosity of complex viscoelastic fluids such as gels, liquid crystals and other soft materials, the rate of molecular tumbling is reduced, which in turn affects the chemical shift anisotropy, dipolar and quadrupolar interactions. As a consequence the solution state NMR spectra show broad lines, and therefore, extracting detailed structural information is a challenging task. In this context, solid state (SS) NMR has the ability to distinguish between a minute amount of polymorphic forms, conformational changes, and the number of non-equivalent molecules in an asymmetric unit of a crystal lattice, and to provide both qualitative as well as quantitative analytical data with a short-range order. Therefore, SS NMR has continued to evolve as an indispensable tool for structural analysis and gave birth to a new field called NMR crystallography. Solid state cross polarization (CP) and high resolution (HR) magic angle spinning (MAS) NMR spectroscopy has been used to study weak interactions in polymer gels. However, the application of SS NMR spectroscopy to study gels derived from low molecular weight gelators has been limited until recently. In this review, we will focus on the importance of solid state NMR spectroscopy in understanding and elucidating the structure of supramolecular gels derived from low molecular weight gelators with selected examples. PMID:27374054

  20. (31)P solid-state NMR based monitoring of permeation of cell penetrating peptides into skin.

    Science.gov (United States)

    Desai, Pinaki R; Cormier, Ashley R; Shah, Punit P; Patlolla, Ram R; Paravastu, Anant K; Singh, Mandip

    2014-02-01

    The main objective of the current study was to investigate penetration of cell penetrating peptides (CPPs: TAT, R8, R11, and YKA) through skin intercellular lipids using (31)P magic angle spinning (MAS) solid-state NMR. In vitro skin permeation studies were performed on rat skin, and sections (0-60, 61-120, and 121-180μm) were collected and analyzed for (31)P NMR signal. The concentration-dependent shift of 0, 25, 50, 100, and 200mg/ml of TAT on skin layers, diffusion of TAT, R8, R11, and YKA in the skin and time dependent permeation of R11 was measured on various skin sections using (31)P solid-state NMR. Further, CPPs and CPP-tagged fluorescent dye encapsulate liposomes (FLip) in skin layers were tagged using confocal microscopy. The change in (31)P NMR chemical shift was found to depend monotonically on the amount of CPP applied on skin, with saturation behavior above 100mg/ml CPP concentration. R11 and TAT caused more shift in solid-state NMR peaks compared to other peptides. Furthermore, NMR spectra showed R11 penetration up to 180μm within 30min. The results of the solid-state NMR study were in agreement with confocal microscopy studies. Thus, (31)P solid-state NMR can be used to track CPP penetration into different skin layers. Copyright © 2013 Elsevier B.V. All rights reserved.

  1. 基于对策论的MAS-BDI主体模型%Modeling MAS-BDI Agent in Game Theory

    Institute of Scientific and Technical Information of China (English)

    吴朝晖; 忻栋; 潘云鹤

    2001-01-01

    BDI Agent will choose the intention, which has minimal penalty and maximal income, to achieve its goal. While in multi-Agent system,it is hard for the Agent to find the best intention,not only because of the lack of information,but also the high complexity ot computation. The factors ,which will affect the Agents' decision-making,are the cooperation state of Agents ,the Agents' reasoning process,etc. In this paper,we introduce a new model of MAS-BDI Agent based on game theory,and propose the intention selection strategy for a single BDI Agent, (cooperated)multi-Agent and(uncooperated)multiAgent.

  2. Adsorption-desorption induced structural changes of Cu-MOF evidenced by solid state NMR and EPR spectroscopy.

    Science.gov (United States)

    Jiang, Yijiao; Huang, Jun; Kasumaj, Besnik; Jeschke, Gunnar; Hunger, Michael; Mallat, Tamas; Baiker, Alfons

    2009-02-18

    Adsorption-desorption induced structural changes of Cu(bpy)(H(2)O)(2)(BF(4)),(bpy) (bpy = 4,4'-bipyridine) [Cu-MOF] have been evidenced by combined NMR and EPR spectroscopy. Upon adsorption of probe molecules even at a few mbar, EPR spectra show that they are activated to form complexes at Cu(II) sites, which results in a change of the Cu-MOF's structure as indicated by a high-field shift of the (11)B MAS NMR. After desorption, both EPR and (11)B MAS NMR spectra evidenced that the structure of the Cu-MOF reversibly shifted to the original state. This observation indicates that MOFs can undergo structural changes during processes where adsorption-desorption steps are involved such as gas storage, separation, and catalysis.

  3. MAS C-Terminal Tail Interacting Proteins Identified by Mass Spectrometry- Based Proteomic Approach.

    Science.gov (United States)

    Tirupula, Kalyan C; Zhang, Dongmei; Osbourne, Appledene; Chatterjee, Arunachal; Desnoyer, Russ; Willard, Belinda; Karnik, Sadashiva S

    2015-01-01

    Propagation of signals from G protein-coupled receptors (GPCRs) in cells is primarily mediated by protein-protein interactions. MAS is a GPCR that was initially discovered as an oncogene and is now known to play an important role in cardiovascular physiology. Current literature suggests that MAS interacts with common heterotrimeric G-proteins, but MAS interaction with proteins which might mediate G protein-independent or atypical signaling is unknown. In this study we hypothesized that MAS C-terminal tail (Ct) is a major determinant of receptor-scaffold protein interactions mediating MAS signaling. Mass-spectrometry based proteomic analysis was used to comprehensively identify the proteins that interact with MAS Ct comprising the PDZ-binding motif (PDZ-BM). We identified both PDZ and non-PDZ proteins from human embryonic kidney cell line, mouse atrial cardiomyocyte cell line and human heart tissue to interact specifically with MAS Ct. For the first time our study provides a panel of PDZ and other proteins that potentially interact with MAS with high significance. A 'cardiac-specific finger print' of MAS interacting PDZ proteins was identified which includes DLG1, MAGI1 and SNTA. Cell based experiments with wild-type and mutant MAS lacking the PDZ-BM validated MAS interaction with PDZ proteins DLG1 and TJP2. Bioinformatics analysis suggested well-known multi-protein scaffold complexes involved in nitric oxide signaling (NOS), cell-cell signaling of neuromuscular junctions, synapses and epithelial cells. Majority of these protein hits were predicted to be part of disease categories comprising cancers and malignant tumors. We propose a 'MAS-signalosome' model to stimulate further research in understanding the molecular mechanism of MAS function. Identifying hierarchy of interactions of 'signalosome' components with MAS will be a necessary step in future to fully understand the physiological and pathological functions of this enigmatic receptor.

  4. NMR, Water and Plants

    NARCIS (Netherlands)

    As, van H.

    1982-01-01

    This Thesis describes the application of a non-destructive pulsed proton NMR method mainly to measure water transport in the xylem vessels of plant stems and in some model systems. The results are equally well applicable to liquid flow in other biological objects than plants, e.g. flow of blood and

  5. Single-sided NMR

    CERN Document Server

    Casanova, Federico; Blümich, Bernhard

    2011-01-01

    Single-Sided NMR describes the design of the first functioning single-sided tomograph, the related measurement methods, and a number of applications. One of the key advantages to this method is the speed at which the images are obtained.

  6. Autonomous driving in NMR.

    Science.gov (United States)

    Perez, Manuel

    2017-01-01

    The automatic analysis of NMR data has been a much-desired endeavour for the last six decades, as it is the case with any other analytical technique. This need for automation has only grown as advances in hardware; pulse sequences and automation have opened new research areas to NMR and increased the throughput of data. Full automatic analysis is a worthy, albeit hard, challenge, but in a world of artificial intelligence, instant communication and big data, it seems that this particular fight is happening with only one technique at a time (let this be NMR, MS, IR, UV or any other), when the reality of most laboratories is that there are several types of analytical instrumentation present. Data aggregation, verification and elucidation by using complementary techniques (e.g. MS and NMR) is a desirable outcome to pursue, although a time-consuming one if performed manually; hence, the use of automation to perform the heavy lifting for users is required to make the approach attractive for scientists. Many of the decisions and workflows that could be implemented under automation will depend on the two-way communication with databases that understand analytical data, because it is desirable not only to query these databases but also to grow them in as much of an automatic manner as possible. How these databases are designed, set up and the data inside classified will determine what workflows can be implemented. Copyright © 2016 John Wiley & Sons, Ltd.

  7. Ca(AlH4)2, CaAlH5, and CaH2+6LiBH4: Calculated dehydrogenation enthalpy, including zero point energy, and the structure of the phonon spectra.

    Science.gov (United States)

    Marashdeh, Ali; Frankcombe, Terry J

    2008-06-21

    The dehydrogenation enthalpies of Ca(AlH(4))(2), CaAlH(5), and CaH(2)+6LiBH(4) have been calculated using density functional theory calculations at the generalized gradient approximation level. Harmonic phonon zero point energy (ZPE) corrections have been included using Parlinski's direct method. The dehydrogenation of Ca(AlH(4))(2) is exothermic, indicating a metastable hydride. Calculations for CaAlH(5) including ZPE effects indicate that it is not stable enough for a hydrogen storage system operating near ambient conditions. The destabilized combination of LiBH(4) with CaH(2) is a promising system after ZPE-corrected enthalpy calculations. The calculations confirm that including ZPE effects in the harmonic approximation for the dehydrogenation of Ca(AlH(4))(2), CaAlH(5), and CaH(2)+6LiBH(4) has a significant effect on the calculated reaction enthalpy. The contribution of ZPE to the dehydrogenation enthalpies of Ca(AlH(4))(2) and CaAlH(5) calculated by the direct method phonon analysis was compared to that calculated by the frozen-phonon method. The crystal structure of CaAlH(5) is presented in the more useful standard setting of P2(1)c symmetry and the phonon density of states of CaAlH(5), significantly different to other common complex metal hydrides, is rationalized.

  8. The use of enriched 6Li and 7Li Lif:Mg,Cu,P glass-rod thermoluminescent dosemeters for linear accelerator out-of-field radiation dose measurements.

    Science.gov (United States)

    Takam, R; Bezak, E; Liu, G; Marcu, L

    2012-06-01

    (6)LiF:Mg,Cu,P and (7)LiF:Mg,Cu,P glass-rod thermoluminescent dosemeters (TLDs) were used for measurements of out-of-field photon and neutron doses produced by Varian iX linear accelerator. Both TLDs were calibrated using 18-MV X-ray beam to investigate their dose-response sensitivity and linearity. CR-39 etch-track detectors (Luxel+, Landauer) were employed to provide neutron dose data to calibrate (6)LiF:Mg,Cu,P TLDs at various distances from the isocentre. With cadmium filters employed, slow neutrons (neutrons. The average in-air photon dose equivalents per monitor unit (MU) ranged from 1.5±0.4 to 215.5±94.6 μSv at 100 and 15 cm from the isocentre, respectively. Based on the cross-calibration factors obtained with CR-39 etch-track detectors, the average in-air fast neutron dose equivalents per MU range from 10.6±3.8 to 59.1±49.9 μSv at 100 and 15 cm from the isocentre, respectively. Contribution of thermal neutrons to total neutron dose equivalent was small: 3.1±7.2 μSv per MU at 15 cm from the isocentre.

  9. 基于6LiF/ZnS(Ag)闪烁体波移光纤读出中子探测器模拟研究%The Monte-Carlo Simulation on Neutron Detector of 6LiF/ZnS(Ag)Scintillator Using Wavelength-Shifting Readout Fibers

    Institute of Scientific and Technical Information of China (English)

    吴冲; 张强; 张鹏; 孙志嘉; 唐彬; 王拓

    2012-01-01

    利用GEANT4构建二维位置灵敏型闪烁体中子探测器模型,并对探测器的关键性能进行了系统的模拟研究.计算结果表明,采用双层闪烁屏与波移光纤作为夹层的“三明治”式结构探测器,其热中子探测效率可以达到49.1%.模拟和实验均表明:探测器具有较好的n/γ抑制能力.γ灵敏度小于10-5;中子位置分辨率随着光纤芯间距和光纤与闪烁屏距离的减小呈现减小趋势,本征空间分辨率最好可以达到X轴0.08 mm,Y轴0.12 mm;光纤与闪烁屏之间采用空气耦合位置分辨率好于硅油耦合.模拟结果与部分实验结果的对比验证显示,探测器具有较好的二维成像能力.%A prototype of position sensitive neutron detector based on 6LiF/ZnS(Ag) scintillator was constructed by GEANT 4 package, and its key properties were studied. The simulation result shows that the thermal neutron detection efficiency could reach 49.1% when the "sandwich structure" of detector was set. Both simulation and experimental result plot its good ability of n/y rejection ration,and the gamma sensitive is less than 10-5. The influences of the coupled material and space between wavelength shift fibers and scintillator,as well as the space between two fibers are considered. The intrinsic spatial resolution is 0. 08 mm for X-axis and 0.12 mm for Y-axis,and the detector has a good 2D imaging capability. The simulation results are compared with that of parts experimental results.

  10. Soils, Pores, and NMR

    Science.gov (United States)

    Pohlmeier, Andreas; Haber-Pohlmeier, Sabina; Haber, Agnes; Sucre, Oscar; Stingaciu, Laura; Stapf, Siegfried; Blümich, Bernhard

    2010-05-01

    Within Cluster A, Partial Project A1, the pore space exploration by means of Nuclear Magnetic Resonance (NMR) plays a central role. NMR is especially convenient since it probes directly the state and dynamics of the substance of interest: water. First, NMR is applied as relaxometry, where the degree of saturation but also the pore geometry controls the NMR signature of natural porous systems. Examples are presented where soil samples from the Selhausen, Merzenhausen (silt loams), and Kaldenkirchen (sandy loam) test sites are investigated by means of Fast Field Cycling Relaxometry at different degrees of saturation. From the change of the relaxation time distributions with decreasing water content and by comparison with conventional water retention curves we conclude that the fraction of immobile water is characterized by T1 samples (Haber-Pohlmeier et al. 2010). Third, relaxometric information forms the basis of understanding magnetic resonance imaging (MRI) results. The general difficulty of imaging in soils are the inherent fast T2 relaxation times due to i) the small pore sizes, ii) presence of paramagnetic ions in the solid matrix, and iii) diffusion in internal gradients. The last point is important, since echo times can not set shorter than about 1ms for imaging purposes. The way out is either the usage of low fields for imaging in soils or special ultra-short pulse sequences, which do not create echoes. In this presentation we will give examples on conventional imaging of macropore fluxes in soil cores (Haber-Pohlmeier et al. 2010), and the combination with relaxometric imaging, as well as the advantages and drawbacks of low-field and ultra-fast pulse imaging. Also first results on the imaging of soil columns measured by SIP in Project A3 are given. Haber-Pohlmeier, S., S. Stapf, et al. (2010). "Waterflow Monitored by Tracer Transport in Natural Porous Media Using MRI." Vadose Zone J.: submitted. Haber-Pohlmeier, S., S. Stapf, et al. (2010). "Relaxation in a

  11. NMR for chemists and biologists

    CERN Document Server

    Carbajo, Rodrigo J

    2013-01-01

    This book offers a concise introduction to the field of nuclear magnetic resonance or NMR. It presents the basic foundations of NMR in a non-mathematical way and provides an overview of both recent and important biological applications of NMR.

  12. NMR magnet technology at MIT

    Energy Technology Data Exchange (ETDEWEB)

    Williams, J.E.C.; Bobrov, E.S.; Iwasa, Y.; Punchard, W.F.B.; Wrenn, J.; Zhukovsky, A. (Massachusetts Inst. of Tech., Cambridge, MA (United States). Francis Bitter National Magnet Lab.)

    1992-01-01

    The design and construction of high field superconducting NMR magnets has much in common with other types of adiabatic superconducting magnets. However, two issues have a particular relevance to NMR magnets. They are field drift and homogeneity. In this paper the control of these factors in the particular context of high field NMR spectrometer magnets is examined.

  13. 13C high resolution solid state NMR spectra of Chinese coals

    Institute of Scientific and Technical Information of China (English)

    陈德玉; 胡建治; 叶朝辉

    1997-01-01

    Several typical exinites in China including alginite, cultinite, suberinite and bituminite are analysed by means of 13C high solution solid state CP MAS TOSS NMR spectra to determine their chemical structures and hydrocarbon potential. Thermal simulation solid products (TSSP) of hydrogen-rich coals arc studied to discuss the generation and expulsion mechanism of coal-generating hydrocarbon. The preliminary results are quite encouraging, containing useful information about genesis of coal-generating oil and gases.

  14. TOKSISITAS LETAL MOLUSKISIDA NIKLOSAMIDA PADA BENIH IKAN MAS (Cyprinus carpio

    Directory of Open Access Journals (Sweden)

    Yosmaniar Yosmaniar

    2009-04-01

    Full Text Available Penggunaan moluskisida untuk menanggulangi hama dalam budidaya tanaman padi yang semakin meningkat berpotensi mencemari lingkungan perairan, karena mengandung residu dari bahan aktifnya. Moluskisida niklosamida (C13H8Cl2N2O4 merupakan bahan aktif pestisida yang digunakan untuk memberantas hama keong mas atau siput murbei (Pomacea sp. di sawah. Dengan demikian, bahan tersebut memiliki potensi untuk mencemari lahan tempat usaha budidaya ikan. Penelitian ini bertujuan untuk mengetahui potensi toksisitas akut niklosamida terhadap benih ikan mas (Cyprinus carpio yang ditunjukkan oleh nilai Median Lethal Concentration (LC50 24, 48, dan 96 jam. Penelitian dilakukan di Instalasi Riset Lingkungan Perikanan Budidaya dan Toksikologi, Cibalagung-Bogor. Menggunakan ikan mas dengan bobot individu 2,47 ± 0,13 g. Moluskisida yang digunakan mengandung bahan aktif niklosamida 250g/L. Wadah pengujian berupa 21 unit akuarium kaca berukuran 40 cm x 20 cm x 20 cm yang dilengkapi aerasi serta saluran pemasukan dan pengeluaran. Jumlah ikan uji setiap wadah 10 ekor dengan peubah yang diukur adalah mortalitas ikan. Selama penelitian ikan tidak diberi makan. Tahapan penelitian terdiri atas penentuan nilai ambang atas-bawah, nilai lethal time dan LC50 -24, 48, 72, dan 96 jam. Data diolah dengan analisis probit program LC50. Hasil penelitian menunjukkan bahwa nilai LC50-24, 48, 72, dan 96 jam terhadap benih ikan mas adalah 0,8012 (0,7140—0,8990; 0,5999 (0,5356—0,6719; 0,4511 (0,4067—0,5004; dan 0,3849 mg/L (0,3684—0,4061. Hal ini menunjukkan niklosamida termasuk pestisida yang memiliki toksisitas sangat tinggi (golongan A. The use of molluscicide in aquatic as well as in terresterial agro ecosystem without properly controlled may produce detrimental effects on freshwater fisheries. Molluscicide utilization for golden apple snail (Pomacea sp. control in rice field has increased. The ingredient potencially has a possibility to pollute aquaculture water. The

  15. Investigating albendazole desmotropes by solid-state NMR spectroscopy.

    Science.gov (United States)

    Chattah, Ana K; Zhang, Rongchun; Mroue, Kamal H; Pfund, Laura Y; Longhi, Marcela R; Ramamoorthy, Ayyalusamy; Garnero, Claudia

    2015-03-02

    Characterization of the molecular structure and physicochemical solid-state properties of the solid forms of pharmaceutical compounds is a key requirement for successful commercialization as potential active ingredients in drug products. These properties can ultimately have a critical effect on the solubility and bioavailability of the final drug product. Here, the desmotropy of Albendazole forms I and II was investigated at the atomic level. Ultrafast magic angle spinning (MAS) solid-state nuclear magnetic resonance (NMR) spectroscopy, together with powder X-ray diffraction, thermal analysis, and Fourier transform infrared spectroscopy, were performed on polycrystalline samples of the two solids in order to fully characterize and distinguish the two forms. High-resolution one-dimensional (1)H, (13)C, and (15)N together with two-dimensional (1)H/(1)H single quantum-single quantum, (1)H/(1)H single quantum-double quantum, and (1)H/(13)C chemical shift correlation solid-state NMR experiments under MAS conditions were extensively used to decipher the intramolecular and intermolecular hydrogen bonding interactions present in both solid forms. These experiments enabled the unequivocal identification of the tautomers of each desmotrope. Our results also revealed that both solid forms may be described as dimeric structures, with different intermolecular hydrogen bonds connecting the tautomers in each dimer.

  16. Food Waste Composting Study from Makanan Ringan Mas

    Science.gov (United States)

    Kadir, A. A.; Ismail, S. N. M.; Jamaludin, S. N.

    2016-07-01

    The poor management of municipal solid waste in Malaysia has worsened over the years especially on food waste. Food waste represents almost 60% of the total municipal solid waste disposed in the landfill. Composting is one of low cost alternative method to dispose the food waste. This study is conducted to compost the food waste generation in Makanan Ringan Mas, which is a medium scale industry in Parit Kuari Darat due to the lack knowledge and exposure of food waste recycling practice. The aim of this study is to identify the physical and chemical parameters of composting food waste from Makanan Ringan Mas. The physical parameters were tested for temperature and pH value and the chemical parameter are Nitrogen, Phosphorus and Potassium. In this study, backyard composting was conducted with 6 reactors. Tapioca peel was used as fermentation liquid and soil and coconut grated were used as the fermentation bed. Backyard composting was conducted with six reactors. The overall results from the study showed that the temperature of the reactors were within the range which are from 30° to 50°C. The result of this study revealed that all the reactors which contain processed food waste tend to produce pH value within the range of 5 to 6 which can be categorized as slightly acidic. Meanwhile, the reactors which contained raw food waste tend to produce pH value within the range of 7 to 8 which can be categorized as neutral. The highest NPK obtained is from Reactor B that process only raw food waste. The average value of Nitrogen is 48540 mg/L, Phosphorus is 410 mg/L and Potassium is 1550 mg/L. From the comparison with common chemical fertilizer, it shows that NPK value from the composting are much lower than NPK of the common chemical fertilizer. However, comparison with NPK of organic fertilizer shown only slightly difference value in NPK.

  17. Two phase morphology limits lithium diffusion in TiO(2)(anatase): a (7)Li MAS NMR study.

    Science.gov (United States)

    Wagemaker, M; van de Krol, R; Kentgens, A P; van Well, A A; Mulder, F M

    2001-11-21

    7Li magic angle spinning solid-state nuclear magnetic resonance is applied to investigate the lithium local environment and lithium ion mobility in tetragonal anatase TiO(2) and orthorhombic lithium titanate Li(0.6)TiO(2). Upon lithium insertion, an increasing fraction of the material changes its crystallographic structure from anatase TiO(2) to lithium titanate Li(0.6)TiO(2). Phase separation occurs, and as a result, the Li-rich lithium titanate phase is coexisting with the Li-poor TiO(2) phase containing only small Li amounts approximately equal to 0.01. In both the anatase and the lithium titanate lattice, Li is found to be hopping over the available sites with activation energies of 0.2 and 0.09 eV, respectively. This leads to rapid microscopic diffusion rates at room temperature (D(micr) = 4.7 x 10(-12) cm(2)s(-1) in anatase and D(micr) = 1.3 x 10(-11) cm(2)s(-1) in lithium titanate). However, macroscopic intercalation data show activation energies of approximately 0.5 eV and smaller diffusion coefficients. We suggest that the diffusion through the phase boundary is determining the activation energy of the overall diffusion and the overall diffusion rate itself. The chemical shift of lithium in anatase is independent of temperature up to approximately 250 K but decreases at higher temperatures, reflecting a change in the 3d conduction electron densities. The Li mobility becomes prominent from this same temperature showing that such electronic effects possibly facilitate the mobility.

  18. Chemical shift tensor determination using magnetically oriented microcrystal array (MOMA): 13C solid-state CP NMR without MAS

    Science.gov (United States)

    Kusumi, R.; Kimura, F.; Song, G.; Kimura, T.

    2012-10-01

    Chemical shift tensors for the carboxyl and methyl carbons of L-alanine crystals were determined using a magnetically oriented microcrystal array (MOMA) prepared from a microcrystalline powder sample of L-alanine. A MOMA is a single-crystal-like composite in which microcrystals are aligned three-dimensionally in a matrix resin. The single-crystal rotation method was applied to the MOMA to determine the principal values and axes of the chemical shift tensors. The result showed good agreement with the literature data for the single crystal of L-alanine. This demonstrates that the present technique is a powerful tool for determining the chemical shift tensor of a crystal from a microcrystal powder sample.

  19. Friedel's salt formation in sulfoaluminate cements: A combined XRD and {sup 27}Al MAS NMR study

    Energy Technology Data Exchange (ETDEWEB)

    Paul, G. [Dipartimento di Scienze ed Innovazione Tecnologica, Università del Piemonte Orientale A. Avogadro, Viale T. Michel 11, 15121 Alessandria (Italy); Boccaleri, E., E-mail: enrico.boccaleri@mfn.unipmn.it [Dipartimento di Scienze ed Innovazione Tecnologica, Università del Piemonte Orientale A. Avogadro, Viale T. Michel 11, 15121 Alessandria (Italy); Buzzi, L.; Canonico, F. [Buzzi Unicem S.p.A., Via L. Buzzi 6, 15033 Casale Monferrato (Italy); Gastaldi, D., E-mail: dgastaldi@buzziunicem.it [Buzzi Unicem S.p.A., Via L. Buzzi 6, 15033 Casale Monferrato (Italy)

    2015-01-15

    Four different binders based on calcium sulfoaluminate cements have been submitted to accelerated chlorination through ionic exchange on hydrated pastes, in order to investigate their ability to chemically bind chloride ions that might reduce chloride penetration. The composition of hydrated cements before and after the treatment was evaluated by means of an X-Ray Diffraction–{sup 27}Al Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy combined study, allowing to take into account even partially amorphous phases and to make quantitative assumption on the relative abundance of the different aluminium-containing phases. It was found that low SO{sub 3} Sulfoaluminate–Portland ternary systems are the most effective in binding chloride ions and the active role played by different members of the AFm family in chloride uptake was confirmed. Moreover, a peculiar behavior related to the formation of Friedel's salt in different pH conditions was also established for the different cements.

  20. Generation and characterization of alkali metal clusters in Y-FAU zeolites. An ESR and MAS NMR spectroscopic study

    Science.gov (United States)

    Hannus, István; Béres, Attila; Nagy, János B.; Halász, János; Kiricsi, Imre

    1997-06-01

    Charged and neutral metal clusters of various compositions and sizes can be prepared by controlling the alkali metal content by the decomposition of alkali azides and the composition of the host zeolite by ion-exchange. ESR signals show that electron transfer from alkali metal atoms to alkali metal cations does occur, but in a direction opposite to that predicted by the gas-phase thermochemistry. Alkali metal clusters proved to be very active basic catalytic centers.

  1. Multiple non-coding exons and alternative splicing in the mouse Mas protooncogene.

    Science.gov (United States)

    Alenina, Natalia; Böhme, Ilka; Bader, Michael; Walther, Thomas

    2015-09-01

    The Mas protooncogene encodes a G protein-coupled receptor with the common seven transmembrane domains, expressed mainly in the testis and brain. We provided evidence that Mas is a functional angiotensin-(1-7) receptor and can interact with the angiotensin II type 1 (AT1) receptor. The gene is transcriptionally regulated during development in the brain and testis, but its structure was unresolved. In this study we used 5'- and 3'-RACE, RT-PCR, and RNase-protection assays to elucidate the complete Mas gene structure and organization. We identified 12 exons in the mouse Mas gene with 11 in the 5' untranslated mRNA, which can be alternatively spliced. We also showed that Mas transcription can start from 4 tissue-specific promoters, whereby testis-specific Mas mRNA is transcribed from two upstream promoters, and the expression of Mas in the brain starts from two downstream promoters. Alternative splicing and multiple promoter usage result in at least 12 Mas transcripts in which different 5' untranslated regions are fused to a common coding sequence. Moreover, termination of Mas mRNA is regulated by two different polyadenylation signals. The gene spans approximately 27 kb, and the longest detected mRNA contains 2,451 bp. Thus, our results characterize the Mas protooncogene as the gene with the most complex gene structure of all described members of the gene family coding for G protein-coupled receptors. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Chronic allergic pulmonary inflammation is aggravated in angiotensin-(1-7) Mas receptor knockout mice.

    Science.gov (United States)

    Magalhães, Giselle S; Rodrigues-Machado, Maria Glória; Motta-Santos, Daisy; Alenina, Natalia; Bader, Michael; Santos, Robson A; Barcelos, Lucíola S; Campagnole-Santos, Maria José

    2016-12-01

    The angiotensin-(1-7) [ANG-(1-7)]/Mas receptor pathway is currently recognized as a counterbalancing mechanism of the renin-angiotensin system in different pathophysiological conditions. We have previously described that treatment with ANG-(1-7) attenuates lung inflammation and remodeling in an experimental model of asthma. In the present study, we investigated whether lack of the Mas receptor could alter the inflammatory response in a model of chronic allergic lung inflammation induced by ovalbumin (OVA). Mas receptor wild-type (MasWT) and knockout (MasKO) mice were subjected to four doses of OVA (20 μg/mice ip) with a 14-day interval. At the 21st day, nebulization with OVA (1%) was started, three times per week until the 46th day. Control groups received saline (0.9% ip) and were nebulized with saline (0.9%). MasWT-OVA developed a modest inflammatory response and minor pulmonary remodeling to OVA challenge. Strikingly, MasKO-OVA presented a significant increase in inflammatory cell infiltrate, increase in extracellular matrix deposition, increase in thickening of the alveolar parenchyma, increase in thickening of the smooth muscle layer of the pulmonary arterioles, increase in proinflammatory cytokine and chemokine levels in the lungs, characteristic of chronic asthma. Additionally, MasKO-OVA presented an increase in ERK1/2 phosphorylation compared with MasWT-OVA. Furthermore, MasKO-OVA showed a worse performance in a test of maximum physical exercise compared with MasWT-OVA. Our study shows that effects triggered by the Mas receptor are important to attenuate the inflammatory and remodeling processes in a model of allergic lung inflammation in mice. Our data indicate that impairment of the ANG-(1-7)/Mas receptor pathway may lead to worsening of the pathophysiological changes of asthma. Copyright © 2016 the American Physiological Society.

  3. Reverse Induced Fit-Driven MAS-Downstream Transduction: Looking for Metabotropic Agonists.

    Science.gov (United States)

    Pernomian, Larissa; Gomes, Mayara Santos; de Paula da Silva, Carlos Henrique Tomich; Campos, Joaquin

    2017-09-11

    The protective effects assigned to MAS receptors activation have spurred a great interest in the development of MAS agonists for clinical purposes. However, the current bases that drive the design of these ligands preclude important concepts recently addressed for MAS activation. Emerging data confirmed that physiological concentrations of peptide MAS agonists induce an atypical signaling that does not reach the metabotropic efficacy of constitutive MAS activation. The canonical activation of MAS-coupled G proteins is only achieved by supraphysiological concentrations of peptide MAS agonists or physiological concentrations of chemically modified analogues. These pleiotropic differences are because of two overlapped but non-identical ligand binding domains (LBD): one non-metabotropic site that recognizes peptide agonists and one metabotropic domain that recognizes modified analogues. Accordingly, it is feasible that supraphysiological concentrations of peptide MAS agonists undergo to chemical modifications that make them suitable for binding to the metabotropic LBD. Recent advances on Receptor Theory confirmed that G protein-coupled receptor (GPCR) oligomerization enhances pharmacological parameters coupled to metabotropic signaling from GPCR ligands, including MAS agonists. For instance, the formation of GPCR-signalosome complex (higher order heteroligomers of GPCR involved in signaling crosstalk) makes the transduction of agonists a more adaptive signal. Considering the recent identification of MAS-signalosome, we postulate the reverse induced fit hypothesis in which MAS-signalosome would trigger chemical modifications required for agonists bind to the metabotropic MAS/LBD. In view of this hypothesis, we cover rational perspectives that consider this information for the development of novel metabotropic MAS agonists provided with constitutive efficacy at physiological concentrations. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  4. 13C and 15N CP/MAS, 1H-15N SCT CP/MAS and FTIR spectroscopy as tools for qualitative detection of the presence of zwitterionic and non-ionic forms of ansa-macrolide 3-formylrifamycin SV and its derivatives in solid state.

    Science.gov (United States)

    Przybylski, Piotr; Pyta, Krystian; Klich, Katarzyna; Schilf, Wojciech; Kamieński, Bohdan

    2014-01-01

    (13)C, (15)N CP/MAS, including (1)H-(13)C and (1)H-(15)N short contact time CP/MAS experiments, and FTIR methods were applied for detailed structural characterization of ansa-macrolides as 3-formylrifamycin SV (1) and its derivatives (2-6) in crystal and in powder forms. Although HPLC chromatograms for 2/CH3 OH and 2/CH3 CCl3 were the same for rifampicin crystals dissolved in respective solvents, the UV-vis data recorded for them were different in 300-375 nm region. Detailed solid state (13)C and (15)N CP/MAS NMR and FTIR studies revealed that rifampicin (2), in contrast to 3-formylrifamycin SV (1) and its amino derivatives (3-6), can occur in pure non-ionic or zwitterionic forms in crystal and in pure these forms or a mixture of them in a powder. Multinuclear CP/MAS and FTIR studies demonstrated also that 3-6 derivatives were present exclusively in pure zwitterionic forms, both in powder and in crystal. On the basis of the solid state NMR and FTIR studies, two conformers of 3-formylrifamycin SV were detected in powder form due to the different orientations of carbonyl group of amide moiety. The PM6 molecular modeling at the semi-empirical level of theory, allowed visualization the most energetically favorable non-ionic and zwitterionic forms of 1-6 antibiotics, strongly stabilized via intramolecular H-bonds. FTIR studies indicated that the originally adopted forms of these type antibiotics in crystal or in powder are stable in standard laboratory conditions in time. The results presented point to the fact that because of a possible presence of two forms of rifampicin (compound 2), quantification of the content of this antibiotic in relevant pharmaceuticals needs caution. Copyright © 2013 John Wiley & Sons, Ltd.

  5. 29Si,27Al Magic—Angle—Spinning Nuclear Magnetic Resonance(MAS NMR) Studies of Kaolinite and Its Thermal Transformation Products

    Institute of Scientific and Technical Information of China (English)

    何宏平; 胡澄; 等

    1995-01-01

    27Al,29Si MAS NMR studies of kaolinite and its thermal transformation products show that in the kaolinite-mullite reaction series there is an extensive segregation of Al2O3 and SiO2 and the reaction of Al2O3 with SiO2 to form mullite is the main path of mullite formation.At about 850°C,the peak intensity of Al(V) reaches its maximum and with the further rise of temperature the Al(V)signal completely disappears.At about 950°C,γ-Al2O3 accounts for about 71%of the material phases containing Al atoms.In the series there is no obvious presence of Al-Si spinel.The 27Al and 29Si MAS NMR spectra show that there is an obvious difference between the temperature points for Al-O2(OH)4 octahedral sheet collapsing and Si-O4 tetrahedral sheet breaking down.

  6. Probing the nanostructure, interfacial interaction, and dynamics of chitosan-based nanoparticles by multiscale solid-state NMR.

    Science.gov (United States)

    Wang, Fenfen; Zhang, Rongchun; Wu, Qiang; Chen, Tiehong; Sun, Pingchuan; Shi, An-Chang

    2014-12-10

    Chitosan-based nanoparticles (NPs) are widely used in drug and gene delivery, therapy, and medical imaging, but a molecular-level understanding of the internal morphology and nanostructure size, interface, and dynamics, which is critical for building fundamental knowledge for the precise design and efficient biological application of the NPs, remains a great challenge. Therefore, the availability of a multiscale (0.1-100 nm) and nondestructive analytical technique for examining such NPs is of great importance for nanotechnology. Herein, we present a new multiscale solid-state NMR approach to achieve this goal for the investigation of chitosan-poly(N-3-acrylamidophenylboronic acid) NPs. First, a recently developed (13)C multiple cross-polarization magic-angle spinning (MAS) method enabled fast quantitative determination of the NPs' composition and detection of conformational changes in chitosan. Then, using an improved (1)H spin-diffusion method with (13)C detection and theoretical simulations, the internal morphology and nanostructure size were quantitatively determined. The interfacial coordinated interaction between chitosan and phenylboronic acid was revealed by one-dimensional MAS and two-dimensional (2D) triple-quantum MAS (11)B NMR. Finally, dynamic-editing (13)C MAS and 2D (13)C-(1)H wide-line separation experiments provided details regarding the componential dynamics of the NPs in the solid and swollen states. On the basis of these NMR results, a model of the unique nanostructure, interfacial interaction, and componential dynamics of the NPs was proposed.

  7. Direct determination of phosphate sugars in biological material by (1)H high-resolution magic-angle-spinning NMR spectroscopy.

    Science.gov (United States)

    Diserens, Gaëlle; Vermathen, Martina; Gjuroski, Ilche; Eggimann, Sandra; Precht, Christina; Boesch, Chris; Vermathen, Peter

    2016-08-01

    The study aim was to unambiguously assign nucleotide sugars, mainly UDP-X that are known to be important in glycosylation processes as sugar donors, and glucose-phosphates that are important intermediate metabolites for storage and transfer of energy directly in spectra of intact cells, as well as in skeletal muscle biopsies by (1)H high-resolution magic-angle-spinning (HR-MAS) NMR. The results demonstrate that sugar phosphates can be determined quickly and non-destructively in cells and biopsies by HR-MAS, which may prove valuable considering the importance of phosphate sugars in cell metabolism for nucleic acid synthesis. As proof of principle, an example of phosphate-sugar reaction and degradation kinetics after unfreezing the sample is shown for a cardiac muscle, suggesting the possibility to follow by HR-MAS NMR some metabolic pathways. Graphical abstract Glucose-phosphate sugars (Glc-1P and Glc-6P) detected in muscle by 1H HR-MAS NMR.

  8. NMR of unfolded proteins

    Indian Academy of Sciences (India)

    Amarnath Chtterjee; Ashutosh Kumar; Jeetender Chugh; Sudha Srivastava; Neel S Bhavesh; Ramakrishna V Hosur

    2005-01-01

    In the post-genomic era, as more and more genome sequences are becoming known and hectic efforts are underway to decode the information content in them, it is becoming increasingly evident that flexibility in proteins plays a crucial role in many of the biological functions. Many proteins have intrinsic disorder either wholly or in specific regions. It appears that this disorder may be important for regulatory functions of the proteins, on the one hand, and may help in directing the folding process to reach the compact native state, on the other. Nuclear magnetic resonance (NMR) has over the last two decades emerged as the sole, most powerful technique to help characterize these disordered protein systems. In this review, we first discuss the significance of disorder in proteins and then describe the recent developments in NMR methods for their characterization. A brief description of the results obtained on several disordered proteins is presented at the end.

  9. Evidence for Heterodimerization and Functional Interaction of the Angiotensin Type 2 Receptor and the Receptor MAS

    DEFF Research Database (Denmark)

    Leonhardt, Julia; Steckelings, Ulrike Muscha

    2017-01-01

    The angiotensin type 2 receptor (AT2R) and the receptor MAS are receptors of the protective arm of the renin-angiotensin system. They mediate strikingly similar actions. Moreover, in various studies, AT2R antagonists blocked the effects of MAS agonists and vice versa. Such cross-inhibition may...... indicate heterodimerization of these receptors. Therefore, this study investigated the molecular and functional interplay between MAS and the AT2R. Molecular interactions were assessed by fluorescence resonance energy transfer and by cross correlation spectroscopy in human embryonic kidney-293 cells...... transfected with vectors encoding fluorophore-tagged MAS or AT2R. Functional interaction of AT2R and MAS was studied in astrocytes with CX3C chemokine receptor-1 messenger RNA expression as readout. Coexpression of fluorophore-tagged AT2R and MAS resulted in a fluorescence resonance energy transfer efficiency...

  10. MAS based coordinated scheduling of storage capacities in a virtual microgrid

    DEFF Research Database (Denmark)

    Brehm, Robert; Top, Søren; Mátéfi-Tempfli, Stefan

    A distributed decentralized multi-agent system (MAS) for coordinated scheduling of charge and discharge intervals for storage capacities in a utility grid integrated microgrid is presented. As basis for the MAS based energy management system (EMS) serves a scheduling algorithm based on a distribu......A distributed decentralized multi-agent system (MAS) for coordinated scheduling of charge and discharge intervals for storage capacities in a utility grid integrated microgrid is presented. As basis for the MAS based energy management system (EMS) serves a scheduling algorithm based...... on a distributed optimization algorithm to minimize power flow from/to a virtual microgrid over a transformer substation. A cooperative low-level MAS scheme, which is based on the consensus algorithm is introduced. It is shown that using a cooperative MAS, load profile flattening (peak-shaving) for the utility...... be used, for example by a Distribution System Operator (DSO) to control grid load profiles of virtual microgrids....

  11. NMR studies of metalloproteins

    OpenAIRE

    Li, H; H. Sun

    2011-01-01

    Metalloproteins represent a large share of the proteomes, with the intrinsic metal ions providing catalytic, regulatory, and structural roles critical to protein functions. Structural characterization of metalloproteins and identification of metal coordination features including numbers and types of ligands and metal-ligand geometry, and mapping the structural and dynamic changes upon metal binding are significant for understanding biological functions of metalloproteins. NMR spectroscopy has...

  12. Evidence for Heterodimerization and Functional Interaction of the Angiotensin Type 2 Receptor and the Receptor MAS.

    Science.gov (United States)

    Leonhardt, Julia; Villela, Daniel C; Teichmann, Anke; Münter, Lisa-Marie; Mayer, Magnus C; Mardahl, Maibritt; Kirsch, Sebastian; Namsolleck, Pawel; Lucht, Kristin; Benz, Verena; Alenina, Natalia; Daniell, Nicholas; Horiuchi, Masatsugu; Iwai, Masaru; Multhaup, Gerhard; Schülein, Ralf; Bader, Michael; Santos, Robson A; Unger, Thomas; Steckelings, Ulrike Muscha

    2017-06-01

    The angiotensin type 2 receptor (AT2R) and the receptor MAS are receptors of the protective arm of the renin-angiotensin system. They mediate strikingly similar actions. Moreover, in various studies, AT2R antagonists blocked the effects of MAS agonists and vice versa. Such cross-inhibition may indicate heterodimerization of these receptors. Therefore, this study investigated the molecular and functional interplay between MAS and the AT2R. Molecular interactions were assessed by fluorescence resonance energy transfer and by cross correlation spectroscopy in human embryonic kidney-293 cells transfected with vectors encoding fluorophore-tagged MAS or AT2R. Functional interaction of AT2R and MAS was studied in astrocytes with CX3C chemokine receptor-1 messenger RNA expression as readout. Coexpression of fluorophore-tagged AT2R and MAS resulted in a fluorescence resonance energy transfer efficiency of 10.8 ± 0.8%, indicating that AT2R and MAS are capable to form heterodimers. Heterodimerization was verified by competition experiments using untagged AT2R and MAS. Specificity of dimerization of AT2R and MAS was supported by lack of dimerization with the transient receptor potential cation channel, subfamily C-member 6. Dimerization of the AT2R was abolished when it was mutated at cysteine residue 35. AT2R and MAS stimulation with the respective agonists, Compound 21 or angiotensin-(1-7), significantly induced CX3C chemokine receptor-1 messenger RNA expression. Effects of each agonist were blocked by an AT2R antagonist (PD123319) and also by a MAS antagonist (A-779). Knockout of a single of these receptors made astrocytes unresponsive for both agonists. Our results suggest that MAS and the AT2R form heterodimers and that-at least in astrocytes-both receptors functionally depend on each other. © 2017 American Heart Association, Inc.

  13. MOS-2: A Two-Dimension Space for Positioning MAS Organizational Models

    OpenAIRE

    Abbas, Hosny; Shaheen, Samir

    2015-01-01

    The increased complexity and dynamism of present and future Multi-Agent Systems (MAS) enforce the need for considering both of their static (design-time) and the dynamic (run-time) aspects. A type of balance between the two aspects can definitely give better results related to system stability and adaptivity. MAS organization is the research area that is concerned with these issues and it is currently a very active and interesting research area. Designing a MAS with an initial organization an...

  14. COMPOZER-based longitudinal cross-polarization via dipolar coupling under MAS.

    Science.gov (United States)

    Kamihara, Takayuki; Murakami, Miwa; Noda, Yasuto; Takeda, Kazuyuki; Takegoshi, K

    2014-08-01

    We propose a cross polarization (CP) sequence effective under magic-angle spinning (MAS) which is tolerant to RF field inhomogeneity and Hartmann-Hahn mismatch. Its key feature is that spin locking is not used, as CP occurs among the longitudinal (Z) magnetizations modulated by the combination of two pulses with the opposite phases. We show that, by changing the phases of the pulse pairs synchronized with MAS, the flip-flop term of the dipolar interaction is restored under MAS.

  15. The study of 12C(α,γ astrophysical reaction using 12C(6Li,d and 12C(7Li,t reaction at 20 MeV and in the framework of the potential model

    Directory of Open Access Journals (Sweden)

    Adhikari S.

    2015-01-01

    Full Text Available The triton angular distribution in the 12C(7Li,t16O reaction has been measured at 20 MeV incident energy. Comparison of the data with Finite Range DWBA and CDCC-CRC calculations show that breakup coupling effects are prominent in the transfer to the ground state. This observation is similar to that in the 12C(6Li,d reaction at the same incident energy. The alpha spectroscopic factor of the 16O ground state is determined (Sα=0.25 from a comparison of the measured angular distribution with respect to the CDCC-CRC calculations. The E2 S-factor of the 12C(α,γ reaction at 300 keV in the framework of a potential model is determined to be about 118 keV-barn.

  16. Fast magic-angle sample spinning solid-state NMR at 60-100kHz for natural abundance samples.

    Science.gov (United States)

    Nishiyama, Yusuke

    2016-09-01

    In spite of tremendous progress made in pulse sequence designs and sophisticated hardware developments, methods to improve sensitivity and resolution in solid-state NMR (ssNMR) are still emerging. The rate at which sample is spun at magic angle determines the extent to which sensitivity and resolution of NMR spectra are improved. To this end, the prime objective of this article is to give a comprehensive theoretical and experimental framework of fast magic angle spinning (MAS) technique. The engineering design of fast MAS rotors based on spinning rate, sample volume, and sensitivity is presented in detail. Besides, the benefits of fast MAS citing the recent progress in methodology, especially for natural abundance samples are also highlighted. The effect of the MAS rate on (1)H resolution, which is a key to the success of the (1)H inverse detection methods, is described by a simple mathematical factor named as the homogeneity factor k. A comparison between various (1)H inverse detection methods is also presented. Moreover, methods to reduce the number of spinning sidebands (SSBs) for the systems with huge anisotropies in combination with (1)H inverse detection at fast MAS are discussed.

  17. Structural studies on meiosis-activating sterols and structurally related compounds : potential ligands of the FF-MAS receptor

    NARCIS (Netherlands)

    Boer, D.R.

    2001-01-01

    Meiosis Activating Sterols (MAS) are key regulatory factors in the meiotic cell cycle. Two compounds in this family, Follicular Fluid-MAS (FF-MAS or 4,4-dimethyl-5a-cholest-8,14,24-triene-3b-ol) and Testicular-MAS (T-MAS or 4,4-dimethyl-5a-cholest-8,14-diene-3b-ol), have been isolated and

  18. MAS-mediated antioxidant effects restore the functionality of angiotensin converting enzyme 2-angiotensin-(1-7)-MAS axis in diabetic rat carotid.

    Science.gov (United States)

    Pernomian, Larissa; Gomes, Mayara Santos; Restini, Carolina Baraldi Araujo; de Oliveira, Ana Maria

    2014-01-01

    We hypothesized that endothelial AT1-activated NAD(P)H oxidase-driven generation of reactive oxygen species during type I-diabetes impairs carotid ACE2-angiotensin-(1-7)-Mas axis functionality, which accounts for the impaired carotid flow in diabetic rats. We also hypothesized that angiotensin-(1-7) chronic treatment of diabetic rats restores carotid ACE2-angiotensin-(1-7)-Mas axis functionality and carotid flow. Relaxant curves for angiotensin II or angiotensin-(1-7) were obtained in carotid from streptozotocin-induced diabetic rats. Superoxide or hydrogen peroxide levels were measured by flow cytometry in carotid endothelial cells. Carotid flow was also determined. We found that endothelial AT1-activated NAD(P)H oxidase-driven generation of superoxide and hydrogen peroxide in diabetic rat carotid impairs ACE2-angiotensin-(1-7)-Mas axis functionality, which reduces carotid flow. In this mechanism, hydrogen peroxide derived from superoxide dismutation inhibits ACE2 activity in generating angiotensin-(1-7) seemingly by activating I(Cl,SWELL0, while superoxide inhibits the nitrergic Mas-mediated vasorelaxation evoked by angiotensin-(1-7). Angiotensin-(1-7) treatment of diabetic rats restored carotid ACE2-angiotensin-(1-7)-Mas axis functionality by triggering a positive feedback played by endothelial Mas receptors, that blunts endothelial AT1-activated NAD(P)H oxidase-driven generation of reactive oxygen species. Mas-mediated antioxidant effects also restored diabetic rat carotid flow, pointing to the contribution of ACE2-angiotensin-(1-7)-Mas axis in maintaining carotid flow.

  19. Solid State NMR Studies of Energy Conversion and Storage Materials

    Science.gov (United States)

    Jankuru Hennadige, Sohan Roshel De Silva

    NMR (Nuclear magnetic resonance) spectroscopy is utilized to study energy conversion and storage materials. Different types of NMR techniques including Magic Angle Spinning, Cross-polarization and relaxation measurement experiments were employed. Four different projects are discussed in this dissertation. First, three types of CFx battery materials were investigated. Electrochemical studies have demonstrated different electrochemical performances by one type, delivering superior performance over the other two. 13C and 19F MAS NMR techniques are employed to identify the atomic/molecular structural factors that might account for differences in electrochemical performance among different types. Next as the second project, layered polymer dielectrics were investigated by NMR. Previous studies have shown that thin film capacitors are improved by using alternate layers of two polymers with complementary properties: one with a high breakdown strength and one with high dielectric constant as opposed to monolithic layers. 13C to 1H cross-polarization techniques were used to investigate any inter-layer properties that may cause the increase in the dielectric strength. The third project was to study two types of thermoelectric materials. These samples were made of heavily doped phosphorous and boron in silicon by two different methods: ball-milled and annealed. These samples were investigated by NMR to determine the degree of disorder and obtain insight into the doping efficiency. The last ongoing project is on a lithium-ion battery system. The nature of passivating layers or the solid electrolyte interphase (SEI) formed on the electrodes surface is important because of the direct correlation between the SEI and the battery life time/durability. Multinuclear (7Li, 19F, 31P) techniques are employed to identify the composition of the SEI formation of both positive and negative electrodes.

  20. Multi-Robot Remote Interaction with FS-MAS

    Directory of Open Access Journals (Sweden)

    Yunliang Jiang

    2013-02-01

    Full Text Available The need to reduce bandwidth, improve productivity, autonomy and the scalability in multi‐robot teleoperation has been recognized for a long time. In this article we propose a novel finite state machine mobile agent based on the network interaction service model, namely FS‐MAS. This model consists of three finite state machines, namely the Finite State Mobile Agent (FS‐Agent, which is the basic service module. The Service Content Finite State Machine (Content‐FS, using the XML language to define workflow, to describe service content and service computation process. The Mobile Agent computation model Finite State Machine (MACM‐FS, used to describe the service implementation. Finally, we apply this service model to the multi‐robot system, the initial realization completing complex tasks in the form of multi‐robot scheduling. This demonstrates that the robot has greatly improved intelligence, and provides a wide solution space for critical issues such as task division, rational and efficient use of resource and multi‐robot collaboration.

  1. Powder-XRD and (14) N magic angle-spinning solid-state NMR spectroscopy of some metal nitrides.

    Science.gov (United States)

    Kempgens, Pierre; Britton, Jonathan

    2016-05-01

    Some metal nitrides (TiN, ZrN, InN, GaN, Ca3 N2 , Mg3 N2 , and Ge3 N4 ) have been studied by powder X-ray diffraction (XRD) and (14) N magic angle-spinning (MAS) solid-state NMR spectroscopy. For Ca3 N2 , Mg3 N2 , and Ge3 N4 , no (14) N NMR signal was observed. Low speed (νr  = 2 kHz for TiN, ZrN, and GaN; νr  = 1 kHz for InN) and 'high speed' (νr  = 15 kHz for TiN; νr  = 5 kHz for ZrN; νr  = 10 kHz for InN and GaN) MAS NMR experiments were performed. For TiN, ZrN, InN, and GaN, powder-XRD was used to identify the phases present in each sample. The number of peaks observed for each sample in their (14) N MAS solid-state NMR spectrum matches perfectly well with the number of nitrogen-containing phases identified by powder-XRD. The (14) N MAS solid-state NMR spectra are symmetric and dominated by the quadrupolar interaction. The envelopes of the spinning sidebands manifold are Lorentzian, and it is concluded that there is a distribution of the quadrupolar coupling constants Qcc 's arising from structural defects in the compounds studied.

  2. NMR and Nqr Study of Atomic Order in Alkali Borate Glasses.

    Science.gov (United States)

    Gravina, Samuel John

    A modified Robinson oscillator circuit was built for the detection of nuclear quadrupole resonance (NQR) in the 200 to 10,000 kHz region. The circuit demonstrates near ideal performance with the detected noise limited only by the sample temperature. The use of computer controlled data acquisition and a carefully designed sample probe allows for the use of an integrating time constant of up to 6 hours. This spectrometer has been used to detect ^{10}B and ^{11 }B NQR in lithium and sodium borate glasses and crystals. In pure boron oxide glass two distinct boron sites are found. By comparing this experiment with previous NMR and Raman spectroscopy studies, one of the sites, which comprises 85% of the total boron, can be attributed to boron atoms in boroxol rings. As sodium is added to the glass the abundance of boroxol rings decreases. At 20 mol% sodium oxide less than 2% of the boron atoms are found in boroxol rings. The dipole-dipole interaction between lithium cations and four-coordinated boron atoms (B_4 units) has been measured. It is found that every B_4 unit has one lithium cation next to it at an average distance of 2.82 A. A comparison with lithium borate crystals shows that diborate groups do not occur in significant quantities. Both high field and low field NMR studies of the boron quadrupole interaction in a B_4 unit also show that diborate groups are not found in the glass. A ^{23}Na and ^6Li NMR MASS study of lithium and sodium borate glasses shows that ^{23 }Na chemical shifts can distinguish sodium cations bound to non-bridging oxygens from sodium cations bound to bridging oxygens. The chemical shifts measured in lithium-sodium borate glasses are identical to those measured in lithium borate or sodium borate glasses, indicating similar alkali-oxygen coordination. A significant narrowing of the ^6Li NMR spectrum in a mixed alkali glass can be understood as a decrease in the entropy of the lithium cations. This result is consistent with the weak

  3. Solid-state NMR spectra of lipid-anchored proteins under magic angle spinning.

    Science.gov (United States)

    Nomura, Kaoru; Harada, Erisa; Sugase, Kenji; Shimamoto, Keiko

    2014-03-01

    Solid-state NMR is a promising tool for elucidating membrane-related biological phenomena. We achieved the measurement of high-resolution solid-state NMR spectra for a lipid-anchored protein embedded in lipid bilayers under magic angle spinning (MAS). To date, solid-state NMR measurements of lipid-anchored proteins have not been accomplished due to the difficulty in supplying sufficient amount of stable isotope labeled samples in the overexpression of lipid-anchored proteins requiring complex posttranslational modification. We designed a pseudo lipid-anchored protein in which the protein component was expressed in E. coli and attached to a chemically synthesized lipid-anchor mimic. Using two types of membranes, liposomes and bicelles, we demonstrated different types of insertion procedures for lipid-anchored protein into membranes. In the liposome sample, we were able to observe the cross-polarization and the (13)C-(13)C chemical shift correlation spectra under MAS, indicating that the liposome sample can be used to analyze molecular interactions using dipolar-based NMR experiments. In contrast, the bicelle sample showed sufficient quality of spectra through scalar-based experiments. The relaxation times and protein-membrane interaction were capable of being analyzed in the bicelle sample. These results demonstrated the applicability of two types of sample system to elucidate the roles of lipid-anchors in regulating diverse biological phenomena.

  4. Receptor MAS protects mice against hypothermia and mortality induced by endotoxemia.

    Science.gov (United States)

    Souza, Laura L; Duchene, Johan; Todiras, Mihail; Azevedo, Luciano C P; Costa-Neto, Claudio M; Alenina, Natalia; Santos, Robson A; Bader, Michael

    2014-04-01

    The renin-angiotensin (Ang) system is involved in maintaining cardiovascular function by regulating blood pressure and electrolyte homeostasis. More recently, alternative pathways within the renin-angiotensin system have been described, such as the ACE-2/Ang-(1-7)/Mas axis, with opposite effects to the ones of the ACE/Ang-II/AT1 axis. Correspondingly, our previous work reported that Ang-(1-7) via its receptor Mas inhibits the mRNA expression of the proinflammatory cytokines interleukin 6 (IL-6) and tumor necrosis factor-α increased by lipopolysaccharide (LPS) in mouse peritoneal macrophages. These data led us to investigate the functional role of the Ang-(1-7)/Mas axis in an in vivo LPS model. In this work, we present evidence that Ang-(1-7) via Mas significantly reduced the LPS-increased production of circulating cytokines, such as IL-6, IL-12, and CXCL-1. This inhibitory effect was mediated by Mas because it was not detectable in Mas-deficient (Mas) mice. Accordingly, IL-6, CXCL-1, and CXCL-2 levels were higher after LPS treatment in the absence of Mas. Mas mice were less resistant to LPS-induced endotoxemia, their survival rate being 50% compared with 95% in wild-type mice. Telemetric analyses showed that Mas mice presented more pronounced LPS-induced hypothermia with a 3°C lower body temperature compared with wild-type mice. Altogether, our findings suggest that Ang-(1-7) and Mas inhibit LPS-induced cytokine production and hypothermia and thereby protect mice from the fatal consequences of endotoxemia.

  5. Mas receptor deficiency exacerbates lipopolysaccharide-induced cerebral and systemic inflammation in mice.

    Science.gov (United States)

    Oliveira-Lima, Onésia C; Pinto, Mauro C X; Duchene, Johan; Qadri, Fatimunnisa; Souza, Laura L; Alenina, Natalia; Bader, Michael; Santos, Robson A S; Carvalho-Tavares, Juliana

    2015-12-01

    Beyond the classical actions of the renin-angiotensin system on the regulation of cardiovascular homeostasis, several studies have shown its involvement in acute and chronic inflammation. The G protein-coupled receptor Mas is a functional binding site for the angiotensin-(1-7); however, its role in the immune system has not been fully elucidated. In this study, we evaluated the effect of genetic deletion of Mas receptor in lipopolysaccharide (LPS)-induced systemic and cerebral inflammation in mice. Inflammatory response was triggered in Mas deficient (Mas(-/-)) and C57BL/6 wild-type (WT) mice (8-12 weeks-old) by intraperitoneal injection of LPS (5 mg/kg). Mas(-/-) mice presented more intense hypothermia compared to WT mice 24 h after LPS injection. Systemically, the bone marrow of Mas(-/-) mice contained a lower number of neutrophils and monocytes 3 h and 24 h after LPS injection, respectively. The plasma levels of inflammatory mediators KC, MCP-1 and IL-10 were higher in Mas(-/-) mice 24 h after LPS injection in comparison to WT. In the brain, Mas(-/-) animals had a significant increase in the number of adherent leukocytes to the brain microvasculature compared to WT mice, as well as, increased number of monocytes and neutrophils recruited to the pia-mater. The elevated number of adherent leukocytes on brain microvasculature in Mas(-/-) mice was associated with increased expression of CD11b - the alpha-subunit of the Mac-1 integrin - in bone marrow neutrophils 3h after LPS injection, and with increased brain levels of chemoattractants KC, MIP-2 and MCP-1, 24 h later. In conclusion, we demonstrated that Mas receptor deficiency results in exacerbated inflammation in LPS-challenged mice, which suggest a potential role for the Mas receptor as a regulator of systemic and brain inflammatory response induced by LPS. Copyright © 2015 Elsevier GmbH. All rights reserved.

  6. Probing lipid-cholesterol interactions in DOPC/eSM/Chol and DOPC/DPPC/Chol model lipid rafts with DSC and (13)C solid-state NMR.

    Science.gov (United States)

    Fritzsching, Keith J; Kim, Jihyun; Holland, Gregory P

    2013-08-01

    The interaction between cholesterol (Chol) and phospholipids in bilayers was investigated for the ternary model lipid rafts, DOPC/eSM/Chol and DOPC/DPPC/Chol, with differential scanning calorimetry (DSC) and (13)C cross polarization magic angle spinning (CP-MAS) solid-state NMR. The enthalpy and transition temperature (Tm) of the Lα liquid crystalline phase transition from DSC was used to probe the thermodynamics of the different lipids in the two systems as a function of Chol content. The main chain (13)C (CH2)n resonance is resolved in the (13)C CP-MAS NMR spectra for the unsaturated (DOPC) and saturated (eSM or DPPC) chain lipid in the ternary lipid raft mixtures. The (13)C chemical shift of this resonance can be used to detect differences in chain ordering and overall interactions with Chol for the different lipid constituents in the ternary systems. The combination of DSC and (13)C CP-MAS NMR results indicate that there is a preferential interaction between SM and Chol below Tm for the DOPC/eSM/Chol system when the Chol content is ≤20mol%. In contrast, no preferential interaction between Chol and DPPC is observed in the DOPC/DPPC/Chol system above or below Tm. Finally, (13)C CP-MAS NMR resolves two Chol environments in the DOPC/eSM/Chol system below Tm at Chol contents >20mol% while, a single Chol environment is observed for DOPC/DPPC/Chol at all compositions.

  7. Transformer-coupled NMR probe

    Science.gov (United States)

    Utsuzawa, Shin; Mandal, Soumyajit; Song, Yi-Qiao

    2012-03-01

    In this study, we propose an NMR probe circuit that uses a transformer with a ferromagnetic core for impedance matching. The ferromagnetic core provides a strong but confined coupling that result in efficient energy transfer between the sample coil and NMR spectrometer, while not disturbing the B1 field generated by the sample coil. We built a transformer-coupled NMR probe and found that it offers comparable performance (loss NQR.

  8. Magic Angle Spinning NMR Metabolomics

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Jian Z.

    2016-05-31

    Nuclear Magnetic Resonance (NMR) spectroscopy is a non-destructive, quantitative, reproducible, untargeted and unbiased method that requires no or minimal sample preparation, and is one of the leading analytical tools for metabonomics research [1-3]. The easy quantification and the no need of prior knowledge about compounds present in a sample associated with NMR are advantageous over other techniques [1,4]. 1H NMR is especially attractive because protons are present in virtually all metabolites and its NMR sensitivity is high, enabling the simultaneous identification and monitoring of a wide range of low molecular weight metabolites.

  9. NMR characterization of native liquid spider dragline silk from Nephila edulis.

    Science.gov (United States)

    Hronska, M; van Beek, J D; Williamson, P T F; Vollrath, Fritz; Meier, Beat H

    2004-01-01

    Solid spider dragline silk is well-known for its mechanical properties. Nonetheless a detailed picture of the spinning process is lacking. Here we report NMR studies on the liquid silk within the wide sac of the major ampullate (m.a.) gland from the spider Nephila edulis. The resolution in the NMR spectra is shown to be significantly improved by the application of magic-angle spinning (MAS). From the narrow width of the resonance lines and the chemical shifts observed, it is concluded that the silk protein within the wide sac of the m.a. gland is dynamically disordered throughout the molecule in the sense that each amino acid of a given type senses an identical environment, on average. The NMR data obtained are consistent with an isotropic liquid phase.

  10. Role of the receptor Mas in macrophage-mediated inflammation in vivo.

    Science.gov (United States)

    Hammer, Anna; Yang, Guang; Friedrich, Juliane; Kovacs, Agnes; Lee, De-Hyung; Grave, Katharina; Jörg, Stefanie; Alenina, Natalia; Grosch, Janina; Winkler, Jürgen; Gold, Ralf; Bader, Michael; Manzel, Arndt; Rump, Lars C; Müller, Dominik N; Linker, Ralf A; Stegbauer, Johannes

    2016-12-06

    Recently, an alternative renin-angiotensin system pathway has been described, which involves binding of angiotensin-(1-7) to its receptor Mas. The Mas axis may counterbalance angiotensin-II-mediated proinflammatory effects, likely by affecting macrophage function. Here we investigate the role of Mas in murine models of autoimmune neuroinflammation and atherosclerosis, which both involve macrophage-driven pathomechanisms. Mas signaling affected macrophage polarization, migration, and macrophage-mediated T-cell activation. Mas deficiency exacerbated the course of experimental autoimmune encephalomyelitis and increased macrophage infiltration as well as proinflammatory gene expression in the spleen and spinal cord. Furthermore, Mas deficiency promoted atherosclerosis by affecting macrophage infiltration and migration and led to increased oxidative stress as well as impaired endothelial function in ApoE-deficient mice. In summary, we identified the Mas axis as an important factor in macrophage function during inflammation of the central nervous and vascular system in vivo. Modulating the Mas axis may constitute an interesting therapeutic target in multiple sclerosis and/or atherosclerosis.

  11. Hydronephrosis alters cardiac ACE2 and Mas receptor expression in mice.

    Science.gov (United States)

    Zhang, Yanling; Ma, Lulu; Wu, Junyan; Chen, Tingting

    2015-06-01

    Hydronephrosis is characterized by substantial loss of tubules and affects renin secretion in the kidney. However, whether alterations of angiotensin-converting enzyme (ACE), ACE2 and Mas receptor in the heart are observed in hydronephrosis is unknown. Thus, we assessed these components in hydronephrotic mice treated with AT1 receptor blockade and ACE inhibitor. Hydronephrosis was induced by left ureteral ligation in Balb/C mice except sham-operated animals. The levels of cardiac ACE, ACE2 and Mas receptor were measured after treatment of losartan or enalapril. Hydronephrosis led to an increase of ACE level and a decrease of ACE2 and Mas receptor in the heart. Losartan decreased cardiac ACE level, but ACE2 and Mas receptor levels significantly increased in hydronephrotic mice (p Mas receptor in the heart. Plasma renin activity (PRA) and Ang II decreased in hydronephrotic mice, but significantly increased after treatment with losartan or enalapril. Hydronephrosis increased cardiac ACE and suppressed ACE2 and Mas receptor levels. AT1 blockade caused sustained activation of cardiac ACE2 and Mas receptor, but ACE inhibitor had the limitation of such activation of Mas receptor in hydronephrotic animals. © The Author(s) 2015.

  12. ACE2/ANG-(1-7)/Mas pathway in the brain: the axis of good

    National Research Council Canada - National Science Library

    Xu, Ping; Sriramula, Srinivas; Lazartigues, Eric

    2011-01-01

    ...). Among them, angiotensin converting enzyme-2 (ACE2) and the Mas receptor have forced a reevaluation of the original cascade and led to the emergence of a new arm of the RAS: the ACE2/ANG-(1-7)/Mas axis...

  13. Psychometric Comparison of the Motivation Assessment Scale (MAS) and the Questions about Behavioral Function (QABF)

    Science.gov (United States)

    Koritsas, S.; Iacono, T.

    2013-01-01

    Background: The Motivation Assessment Scale (MAS) and the Questions About Behavioral Function (QABF) are frequently used to assess the learned function of challenging behaviour in people with intellectual disability (ID). The aim was to explore and compare the psychometric properties of the MAS and the QABF. Method: Seventy adults with ID and…

  14. The utility of MAS5 expression summary and detection call algorithms

    Directory of Open Access Journals (Sweden)

    Wilson Claire L

    2007-07-01

    Full Text Available Abstract Background Used alone, the MAS5.0 algorithm for generating expression summaries has been criticized for high False Positive rates resulting from exaggerated variance at low intensities. Results Here we show, with replicated cell line data, that, when used alongside detection calls, MAS5 can be both selective and sensitive. A set of differentially expressed transcripts were identified that were found to be changing by MAS5, but unchanging by RMA and GCRMA. Subsequent analysis by real time PCR confirmed these changes. In addition, with the Latin square datasets often used to assess expression summary algorithms, filtered MAS5.0 was found to have performance approaching that of its peers. Conclusion When used alongside detection calls, MAS5 is a sensitive and selective algorithm for identifying differentially expressed genes.

  15. Mas receptor contributes to pregnancy-induced cardiac remodeling.

    Science.gov (United States)

    Carmos-Silva, Cintia; Almeida, Jônathas Fernandes Queiroz de; Macedo, Larissa Matuda; Melo, Marcos Barrouin B; Pedrino, Gustavo Rodrigues; Santos, Fernanda Fernanda Cristina Alcantara; Biancardi, Manoel Francisco; Santos, Robson Augusto Souza Dos Augusto Souza; Carvalho, Adryano Augustto; Mendes, Elizabeth Pereira; Colugnati, Diego Basile; Mazaro-Costa, Renata; Castro, Carlos Henrique de

    2016-09-13

    Previous studies have demonstrated a protective effect of the Ang-(1-7)/Mas receptor axis on pathological cardiac hypertrophy. Also, the involvement of Mas receptor in the exercise-induced cardiac hypertrophy has been suggested. However, the role of the Ang-(1-7)/Mas receptor on pregnancy-induced cardiac remodeling remains unknown. The objective of this study was to evaluate the participation of the Mas receptor in the development of the cardiac hypertrophy and fibrosis induced by gestation. Female Wistar rats were shared in 3 groups: control , pregnant , and pregnant treated with Mas receptor antagonist A-779 . Wild type (WT) and Mas-knockout mice (KO) were distributed in non-pregnant  and pregnant  groups. Systolic blood pressure (SBP) was measured by tail-cuff plethysmography. The medial part of the left ventricle (LV) was collected for histological analysis. Echocardiographic analysis was used to evaluate the cardiac function. SBP was not changed by pregnancy or A-779 treatment in the Wistar rats. Pharmacological blockade or genetic deletion of Mas receptor attenuates the pregnancy-induced myocyte hypertrophy. The treatment with A-779 or genetic deletion of the Mas receptor increased the collagen III deposition in LV from pregnant animals without changing the fibroblast proliferation. KO mice presented a lower ejection fraction, fraction shortening, stroke volume and higher end systolic volume compared to WT. Interestingly, the pregnancy restored these parameters. In conclusion, these data show that while Mas receptor blockade or deletion decreases physiological hypertrophy of pregnancy, it is associated with more extracellular matrix deposition. These alterations are associated with improvement of the cardiac function through Mas-independent mechanism. ©2016 The Author(s).

  16. Angiotensin-(1-7)/Mas axis modulates fear memory and extinction in mice.

    Science.gov (United States)

    Lazaroni, Thiago Luiz do Nascimento; Bastos, Cristiane Perácio; Moraes, Márcio Flávio Dutra; Santos, Robson Souza; Pereira, Grace Schenatto

    2016-01-01

    Inappropriate defense-alerting reaction to fear is a common feature of neuropsychiatric diseases. Therefore, impairments in brain circuits, as well as in molecular pathways underlying the neurovegetative adjustments to fear may play an essential role on developing neuropsychiatric disorders. Here we tested the hypothesis that interfering with angiotensin-(1-7) [Ang-(1-7)]/Mas receptor axis homeostasis, which appears to be essential to arterial pressure control, would affect fear memory and extinction. Mas knockout (MasKO) mice, in FVB/N background, showed normal cued fear memory and extinction, but increased freezing in response to context. Next, as FVB/N has poor performance in contextual fear memory, we tested MasKO in mixed 129xC57BL/6 background. MasKO mice behaved similarly to wild-type (WT), but memory extinction was slower in contextual fear conditioning to a weak protocol (1CS/US). In addition, delayed extinction in MasKO mice was even more pronounced after a stronger protocol (3CS/US). We showed previously that Angiotensin II receptor AT1 antagonist, losantan, rescued object recognition memory deficit in MasKO mice. Here, losartan was also effective. Memory extinction was accelerated in MasKO mice after treatment with losartan. In conclusion, we showed for the first time that Ang-(1-7)/Mas axis may modulate fear memory extinction. Furthermore, we suggest MasKO mice as an animal model to study post-traumatic stress disorder (PTSD). Copyright © 2015 Elsevier Inc. All rights reserved.

  17. Exploring abiotic stress on asynchronous protein metabolism in single kernels of wheat studied by NMR spectroscopy and chemometrics

    DEFF Research Database (Denmark)

    Winning, H.; Viereck, N.; Wollenweber, B.

    2009-01-01

    at terminal spikelet, during grain-filling or at both stages. Principal component trajectories of the total protein content and the protein fractions of flour as well as the H-1 NMR spectra of single wheat kernels, wheat flour, and wheat methanol extracts were analysed to elucidate the metabolic development...... during grain-filling. The results from both the H-1 NMR spectra of methanol extracts and the H-1 HR-MAS NMR of single kernels showed that a single drought event during the generative stage had as strong an influence on protein metabolism as two consecutive events of drought. By contrast, a drought event...... indicating that protein metabolism is influenced by multiple drought events, the H-1 NMR spectra of the methanol extracts of flour from mature grains revealed that the amount of fumaric acid is particularly sensitive to water deficits....

  18. High-resolution 1H NMR spectroscopy of fish muscle, eggs and small whole fish via Hadamard-encoded intermolecular multiple-quantum coherence.

    Directory of Open Access Journals (Sweden)

    Honghao Cai

    Full Text Available BACKGROUND AND PURPOSE: Nuclear magnetic resonance (NMR spectroscopy has become an important technique for tissue studies. Since tissues are in semisolid-state, their high-resolution (HR spectra cannot be obtained by conventional NMR spectroscopy. Because of this restriction, extraction and high-resolution magic angle spinning (HR MAS are widely applied for HR NMR spectra of tissues. However, both of the methods are subject to limitations. In this study, the feasibility of HR (1H NMR spectroscopy based on intermolecular multiple-quantum coherence (iMQC technique is explored using fish muscle, fish eggs, and a whole fish as examples. MATERIALS AND METHODS: Intact salmon muscle tissues, intact eggs from shishamo smelt and a whole fish (Siamese algae eater are studied by using conventional 1D one-pulse sequence, Hadamard-encoded iMQC sequence, and HR MAS. RESULTS: When we use the conventional 1D one-pulse sequence, hardly any useful spectral information can be obtained due to the severe field inhomogeneity. By contrast, HR NMR spectra can be obtained in a short period of time by using the Hadamard-encoded iMQC method without shimming. Most signals from fatty acids and small metabolites can be observed. Compared to HR MAS, the iMQC method is non-invasive, but the resolution and the sensitivity of resulting spectra are not as high as those of HR MAS spectra. CONCLUSION: Due to the immunity to field inhomogeneity, the iMQC technique can be a proper supplement to HR MAS, and it provides an alternative for the investigation in cases with field distortions and with samples unsuitable for spinning. The acquisition time of the proposed method is greatly reduced by introduction of the Hadamard-encoded technique, in comparison with that of conventional iMQC method.

  19. Studies of Secondary Melanoma on C57BL/6J Mouse Liver Using 1H NMR Metabolomics

    Energy Technology Data Exchange (ETDEWEB)

    Feng, Ju; Isern, Nancy G.; Burton, Sarah D.; Hu, Jian Z.

    2013-10-31

    NMR metabolomics, consisting of solid state high resolution (hr) magic angle spinning (MAS) 1H NMR (1H hr-MAS), liquid state high resolution 1H-NMR, and principal components analysis (PCA) has been used to study secondary metastatic B16-F10 melanoma in C57BL/6J mouse liver . The melanoma group can be differentiated from its control group by PCA analysis of the absolute concentrations or by the absolute peak intensities of metabolites from either 1H hr-MAS NMR data on intact liver tissues or liquid state 1H-NMR spectra on liver tissue extracts. In particular, we found that the absolute concentrations of alanine, glutamate, creatine, creatinine, fumarate and cholesterol are elevated in the melanoma group as compared to controls, while the absolute concentrations of succinate, glycine, glucose, and the family of linear lipids including long chain fatty acids, total choline and acylglycerol are decreased. The ratio of glycerophosphocholine to phosphocholine is increased by about 1.5 fold in the melanoma group, while the absolute concentration of total choline is actually lower in melanoma mice. These results suggest the following picture in secondary melanoma metastasis: Linear lipid levels are decreased by beta oxidation in the melanoma group, which contributes to an increase in the synthesis of cholesterol, and also provides an energy source input for TCA cycle. These findings suggest a link between lipid oxidation, the TCA cycle and the hypoxia-inducible factors (HIF) signal pathway in tumor metastases. Thus this study indicates that the metabolic profile derived from NMR analysis can provide a valuable bio-signature of malignancy and cell hypoxia in metastatic melanoma.

  20. Single-crystal X-ray diffraction and NMR crystallography of a 1:1 cocrystal of dithianon and pyrimethanil.

    Science.gov (United States)

    Pöppler, Ann Christin; Corlett, Emily K; Pearce, Harriet; Seymour, Mark P; Reid, Matthew; Montgomery, Mark G; Brown, Steven P

    2017-03-01

    A single-crystal X-ray diffraction structure of a 1:1 cocrystal of two fungicides, namely dithianon (DI) and pyrimethanil (PM), is reported [systematic name: 5,10-dioxo-5H,10H-naphtho[2,3-b][1,4]dithiine-2,3-dicarbonitrile-4,6-dimethyl-N-phenylpyrimidin-2-amine (1/1), C14H4N2O2S2·C12H13N2]. Following an NMR crystallography approach, experimental solid-state magic angle spinning (MAS) NMR spectra are presented together with GIPAW (gauge-including projector augmented wave) calculations of NMR chemical shieldings. Specifically, experimental (1)H and (13)C chemical shifts are determined from two-dimensional (1)H-(13)C MAS NMR correlation spectra recorded with short and longer contact times so as to probe one-bond C-H connectivities and longer-range C...H proximities, whereas H...H proximities are identified in a (1)H double-quantum (DQ) MAS NMR spectrum. The performing of separate GIPAW calculations for the full periodic crystal structure and for isolated molecules allows the determination of the change in chemical shift upon going from an isolated molecule to the full crystal structure. For the (1)H NMR chemical shifts, changes of 3.6 and 2.0 ppm correspond to intermolecular N-H...O and C-H...O hydrogen bonding, while changes of -2.7 and -1.5 ppm are due to ring current effects associated with C-H...π interactions. Even though there is a close intermolecular S...O distance of 3.10 Å, it is of note that the molecule-to-crystal chemical shifts for the involved sulfur or oxygen nuclei are small.